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Sample records for characterization crystal structure

  1. SYNTHESIS, CHARACTERIZATION AND CRYSTAL STRUCTURES ...

    African Journals Online (AJOL)

    B. S. Chandravanshi

    ABSTRACT. Reaction of [VO(acac)2] (acac = acetylacetonate) with ... Single crystal X-ray structural studies indicate that the hydrazone ligands coordinate to ..... Molecular structure of complex (1) at 30% probability displacement. Figure 4.

  2. SYNTHESIS, CHARACTERIZATION AND CRYSTAL STRUCTURE ...

    African Journals Online (AJOL)

    Preferred Customer

    Reaction of [MoO2(acac)2] (where acac = acetylacetonate) with N'-(2-hydroxy-4- ... Single crystal X-ray structural studies indicate that the hydrazone ligand coordinates .... Molecular structure of the complex at 30% probability displacement.

  3. SYNTHESIS, CHARACTERIZATION, AND CRYSTAL STRUCTURE ...

    African Journals Online (AJOL)

    a

    KEY WORDS: Barium, Crystal structure, 2,6-Pyridinedicarboxylic acid .... The rational design of novel metal-organic frameworks has attracted great ..... Bond, A.D.; Jones, W. Supramolecular Organization and Materials Design, Jones, W.; Rao,.

  4. Synthesis, characterization and crystal structure of a ...

    African Journals Online (AJOL)

    The Mo atom in the complex is in octahedral coordination. Thermal stability of the complex has also been studied. KEY WORDS: Molybdenum complex, Hydrazone ligand, Crystal structure, X-ray diffraction, Thermal property. Bull. Chem. Soc. Ethiop. 2014, 28(3), 409-414. DOI: http://dx.doi.org/10.4314/bcse.v28i3.10 ...

  5. Crystal structure, characterization and magnetic properties of a 1D ...

    Indian Academy of Sciences (India)

    Crystal structure, characterization and magnetic properties of a 1D copper(II) polymer incorporating a Schiff base with carboxylate side arm. SHYAMAPADA SHIT MADHUSUDAN NANDY CORRADO RIZZOLI CÉDRIC DESPLANCHES SAMIRAN MITRA. Regular Article Volume 128 Issue 6 June 2016 pp 913-920 ...

  6. SYNTHESIS, CHARACTERIZATION AND CRYSTAL STRUCTURE OF BIS-(2-HYDROXYBENZALDEHYDEDIAMINOGUANIZONE

    Directory of Open Access Journals (Sweden)

    Diana Dragancea, Vladimir B. Arion, Sergiu Shova

    2008-12-01

    Full Text Available The new ligand, bis(2-hydroxybenzaldehydediaminoguanizone (1 has been synthesized and characterized by elemental analysis, IR and 1H NMR spectroscopies. The crystal structure of the compound was determined by X-ray diffraction. The ligand C15H15N5O2·C2H5OH crystallizes in the monoclinic space group P21/c with unit cell parameters a = 8.9102(3, b = 10.0357(3, c = 19.7618(6 Å, β = 98.385(2°, Z = 4, V = 1748.21(9 Å3, R1 = 0.040. The amino form of the ligand adopts a planar conformation stabilized by two intramolecular hydrogen bonds of the type O–H···N, in which the H atoms of the central amino group are directed to the lone-pair regions of the azomethine nitrogen atoms.

  7. Structural and morphological characterization of fullerite crystals prepared from the vapor phase

    International Nuclear Information System (INIS)

    Haluska, M.; Fejdi, P.; Vybornov, M.; Kuzmany, H.

    1993-01-01

    Crystal structure, habits and surface structures of fullerite crystals prepared from vapor phase were characterized by X-ray analysis, interfacial angle measurements and optical and scanning electron microscopy (SEM). The study of selected C 60 crystals confirmed the fcc structure at room temperature. The crystal habit is determined by two types of morphological faces, namely {100} and {111}. SEM was used for the observation of thermal etched surfaces. (orig.)

  8. Characterization and crystal structures of new Schiff base macrocyclic compounds

    Czech Academy of Sciences Publication Activity Database

    Khalaji, A.D.; Ghoran, S.H.; Pojarová, Michaela; Dušek, Michal

    2015-01-01

    Roč. 56, č. 7 (2015), s. 1410-1414 ISSN 0022-4766 R&D Projects: GA ČR(CZ) GA14-03276S Institutional support: RVO:68378271 Keywords : synthesis * macrocyclic Schiff base * single crystal structure analysis * spectroscopy Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.536, year: 2015

  9. Synthesis and structural characterization of CsNiP crystal

    Indian Academy of Sciences (India)

    Unknown

    The crystals obtained by this method were of good quality exhibiting ... type framework structure having Cs atoms inside it (figures. 3 and 4). This helps for .... Gopalakrishna G S, Prasad J S and Lokanath N K 2001 Proc. joint 4th and 6th ICSTR ...

  10. Topological Characterization of Carbon Graphite and Crystal Cubic Carbon Structures.

    Science.gov (United States)

    Siddiqui, Wei Gao Muhammad Kamran; Naeem, Muhammad; Rehman, Najma Abdul

    2017-09-07

    Graph theory is used for modeling, designing, analysis and understanding chemical structures or chemical networks and their properties. The molecular graph is a graph consisting of atoms called vertices and the chemical bond between atoms called edges. In this article, we study the chemical graphs of carbon graphite and crystal structure of cubic carbon. Moreover, we compute and give closed formulas of degree based additive topological indices, namely hyper-Zagreb index, first multiple and second multiple Zagreb indices, and first and second Zagreb polynomials.

  11. Studies on growth, crystal structure and characterization of novel organic nicotinium trifluoroacetate single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Dhanaraj, P.V. [Centre for Crystal Growth, SSN College of Engineering, Kalavakkam 603 110 (India); Rajesh, N.P., E-mail: rajeshnp@hotmail.com [Centre for Crystal Growth, SSN College of Engineering, Kalavakkam 603 110 (India); Sundar, J. Kalyana; Natarajan, S. [Department of Physics, Madurai Kamaraj University, Madurai 625 021 (India); Vinitha, G. [Department of Physics, Crescent Engineering College, Chennai 600 048 (India)

    2011-09-15

    Highlights: {yields} Good quality crystals of nicotinium trifluoroacetate in monoclinic system were grown for first time. {yields} Nicotinium trifluoroacetate crystal exhibits third order nonlinear optical properties. {yields} The optical spectrum of nicotinium trifluoroacetate crystal reveals the wide transmission in the entire range with cutoff wavelength at 286 nm. {yields} Nicotinium trifluoroacetate is a low dielectric constant material. - Abstract: An organic material, nicotinium trifluoroacetate (NTF) was synthesized and single crystals in monoclinic system were grown from aqueous solution for the first time. Its solubility and metastable zone width were estimated. The crystal structure of NTF was analyzed to reveal the molecular arrangements and the formation of hydrogen bonds in the crystal. High-resolution X-ray diffraction rocking curve measurements were performed to analyze the structural perfection of the grown crystals. Functional groups in NTF were identified by Fourier transform infrared spectral analysis. Thermal behaviour and stability of NTF were studied by thermogravimetric and differential thermal analysis and differential scanning calorimetry. Mechanical and dielectric properties of NTF crystals were analyzed. Optical studies reveal that NTF crystals are transparent in the wavelength range 286-1100 nm. The third order nonlinear optical parameters of NTF were derived by the Z-scan technique.

  12. Electrical and Structural Characterization of Web Dendrite Crystals

    Science.gov (United States)

    Schwuttke, G. H.; Koliwad, K.; Dumas, K. A.

    1985-01-01

    Minority carrier lifetime distributions in silicon web dendrites are measured. Emphasis is placed on measuring areal homogeneity of lifetime, show its dependency on structural defects, and its unique change during hot processing. The internal gettering action of defect layers present in web crystals and their relation to minority carrier lifetime distributions is discussed. Minority carrier lifetime maps of web dendrites obtained before and after high temperature heat treatment are compared to similar maps obtained from 100 mm diameter Czochralski silicon wafers. Such maps indicate similar or superior areal homogeneity of minority carrier lifetime in webs.

  13. Facile synthesis and structure characterization of hexagonal tungsten bronzes crystals

    Science.gov (United States)

    Lee, Jiann-Shing; Liu, Hao-Chuan; Peng, Gao-De; Tseng, Yawteng

    2017-05-01

    A facile molten-salt route was used to synthesize hexagonal Cs0.33WO3, Rb0.33WO3 and K0.30WO3 crystals. The three isostructural compounds were successfully prepared from the reaction of MxWO3 powders (M = Cs, Rb, K) in the CsCl/NaCl, RbCl/NaCl and KCl/NaCl fluxes, respectively. The structure determination and refinement, based on single-crystal X-ray diffraction data, are in agreement with previous works, possessing space group P63/mcm. The a and c parameters vary non-linearly with increasing radii of the M+ cations (rM) that is coordinated to twelve oxygen atoms. Both the volumes of unit-cell and WO6 octahedra vary linearly with rM, which become smaller from Cs0.33WO3 to K0.30WO3. The distortion of WO6 octahedra as well as isotropic displacement parameters increases from Cs0.33WO3 to K0.30WO3. The geometry of the WO6 octahedron becomes more regular with increasing rM. These structural trends arise from the effective size of the M+ cation.

  14. Mechanosynthesis, crystal structure and magnetic characterization of neodymium orthoferrite

    Energy Technology Data Exchange (ETDEWEB)

    Serna, Pedro Vera; Campos, Cecilio Garcia [Division de Ingenierias, Universidad Politecnica de Tecamac (UPTECAMAC), Tecamac de Felipe Villanueva, Estado de Mexico (Mexico); De Jesus, Felix Sanchez; Miro, Ana Maria Bolarin [Area Academica de Ciencias de la Tierra y Materiales, Universidad Autonoma del Estado de Hidalgo (UAEH), Mineral de la Reforma, Hidalgo (Mexico); Loran, Jose Antonio Juanico [Division de Ingenieria Industrial Nanotecnologia, Universidad Politecnica del Valle de Mexico (UPVM), Tultitlan, Estado de Mexico (Mexico); Longwell, Jeffrey, E-mail: pedrovera.upt@gmail.com [Department of Languages and Linguistics, New Mexico State University (NMSU), Las Cruces, NM (United States)

    2016-03-15

    Neodymium orthoferrite NdFeO{sub 3} was obtained at room temperature by mechanosynthesis with a stoichiometric ratio of Nd2O{sub 3} and Fe{sub 2}O{sub 3} powders, whereas the traditional synthesis requires a temperature of approximately 1000 °C. The crystal structure was analyzed by X-ray diffraction analysis using Cu radiation and a LynxEye XE detector, whose strong fluorescence filtering enabled a high signal intensity. The analysis indicated that the obtained crystallites were nano-sized. The particle morphology was observed by scanning electron microscopy, and the magnetic saturation was tested by vibrating sample magnetometry. The synthesis of NdFeO{sub 3} was detected after a few hours of milling, indicating that the milling imparted mechanical energy to the system. (author)

  15. Crystallization and Characterization of Galdieria sulphuraria RUBISCO in Two Crystal Forms: Structural Phase Transition Observed in P21 Crystal Form

    Directory of Open Access Journals (Sweden)

    Boguslaw Stec

    2007-10-01

    Full Text Available We have isolated ribulose-1,5-bisphosphate-carboxylase/oxygenase (RUBISCOfrom the red algae Galdieria Sulphuraria. The protein crystallized in two different crystalforms, the I422 crystal form being obtained from high salt and the P21 crystal form beingobtained from lower concentration of salt and PEG. We report here the crystallization,preliminary stages of structure determination and the detection of the structural phasetransition in the P21 crystal form of G. sulphuraria RUBISCO. This red algae enzymebelongs to the hexadecameric class (L8S8 with an approximate molecular weight 0.6MDa.The phase transition in G. sulphuraria RUBISCO leads from two hexadecamers to a singlehexadecamer per asymmetric unit. The preservation of diffraction power in a phasetransition for such a large macromolecule is rare.

  16. Structural and functional characterization of HPHT diamond crystals used in photoconductive devices

    Energy Technology Data Exchange (ETDEWEB)

    Pace, E.; Pini, A. [Florence Univ. (Italy). Ist. di Astronomia; Vinattieri, A.; Bogani, F.; Santoro, M.; Messina, G.; Santangelo, S.; Sato, Y.

    2000-09-01

    Diamond films are extensively studied for applications as functional material for UV photoconductors. CVD-grown polycrystalline diamond films show very interesting performances, but their complete exploitation is actually limited by a slow time response if compared to other materials, by a relatively high concentration of structural defects, impurities and grain boundaries, which may affect the collection length of photogenerated charges. High-quality single crystal diamonds could solve some of these problems. The absence of grain boundaries can produce longer collection lengths. The nitrogen and impurity contents can be reduced and then large type-IIa diamond single-crystals can be obtained. In this work, a detailed structural and functional characterization of type Ib HPHT diamond crystals has been carried out and the results have been compared to similar characterizations of CVD films to evaluate the different behavior, taking also into account that these high pressure high temperature (HPHT) diamond crystals contain several tens ppm of nitrogen. (orig.)

  17. Synthesis and structural characterization of bulk Sb2Te3 single crystal

    Science.gov (United States)

    Sultana, Rabia; Gahtori, Bhasker; Meena, R. S.; Awana, V. P. S.

    2018-05-01

    We report the growth and characterization of bulk Sb2Te3 single crystal synthesized by the self flux method via solid state reaction route from high temperature melt (850˚C) and slow cooling (2˚C/hour) of constituent elements. The single crystal X-ray diffraction pattern showed the 00l alignment and the high crystalline nature of the resultant sample. The rietveld fitted room temperature powder XRD revealed the phase purity and rhombohedral structure of the synthesized crystal. The formation and analysis of unit cell structure further verified the rhombohedral structure composed of three quintuple layers stacked one over the other. The SEM image showed the layered directional growth of the synthesized crystal carried out using the ZEISS-EVOMA-10 scanning electron microscope The electrical resistivity measurement was carried out using the conventional four-probe method on a quantum design Physical Property Measurement System (PPMS). The temperature dependent electrical resistivity plot for studied Sb2Te3 single crystal depicts metallic behaviour in the absence of any applied magnetic field. The synthesis as well as the structural characterization of as grown Sb2Te3 single crystal is reported and discussed in the present letter.

  18. A facile approach towards synthesis, characterization, single crystal structure, and DFT study of 5-bromosalicylalcohol

    Energy Technology Data Exchange (ETDEWEB)

    Rastogi, Rupali, E-mail: rastogirupali@ymail.com [ITM University, Department of Chemistry (India); Tarannum, Nazia [Ch. Charan Singh University, Department of Chemistry (India); Butcher, R. J. [Howard University, Chemistry Department (United States)

    2016-03-15

    5-Bromosalicylalcohol was prepared by the interaction of NaBH{sub 4} and 5-bromosalicylaldehyde. The use of sodium borohydride makes the reaction easy, facile, economic and does not require any toxic catalyst. The compound is characterized by FTIR, {sup 1}H NMR, {sup 13}C NMR, TEM and ESI-mass spectra. Crystal structure is determined by single crystal X-ray analysis. Quantum mechanical calculations of geometries, energies and thermodynamic parameters are carried out using density functional theory (DFT/B3LYP) method with 6-311G(d,p) basis set. The optimized geometrical parameters obtained by B3LYP method show good agreement with experimental data.

  19. Solid dispersions of Myricetin with enhanced solubility: Formulation, characterization and crystal structure of stability-impeding Myricetin monohydrate crystals

    Science.gov (United States)

    Mureşan-Pop, M.; Pop, M. M.; Borodi, G.; Todea, M.; Nagy-Simon, T.; Simon, S.

    2017-08-01

    Three solid dispersion forms of Myricetin combined with the Polyvinylpyrrolidone were successfully prepared by spray drying method, and characterized by X-ray powder diffraction, thermal analysis, infrared spectroscopy and optical microscopy. Zeta potential measurements provided indications on solid dispersions stability in aqueous suspension related to their storage at elevated temperature and relative humidity, which depends on the Myricetin load. By increase of Myricetin load, the stability of the solid dispersion is impeded due to growth of Myricetin monohydrate crystals. The amorphous dispersions with 10% and 50% Myricetin load are stable and, compared to pure Myricetin, their aqueous solubility is enhanced by a factor of 47 and 13, respectively. The dispersion with 80% Myricetin load is unstable on storage, and this behavior acts in conjunction with the development of Myricetin monohydrate crystals. Single-crystal X-ray diffraction results obtained for Myricetin monohydrate reveal a structure of an infinite 2D network of hydrogen-bonded molecules involving all six hydroxyl groups of Myricetin. The water molecules are positioned in between the infinite chains, and contribute via H-bonds to robust crystal packing. The calculated needle-like morphology of monohydrate form is in agreement with the optical microscopy results. The study shows that the solid amorphous dispersions with up to 50% Myricetin load are a viable option for achieving substantial solubility improvement of Myricetin, and supports their potential use in pharmaceutical applications.

  20. Structural, vibrational and thermal characterization of phase transformation in L-histidinium bromide monohydrate single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Moura, G.M. [Universidade Federal do Maranhão, CCSST, Imperatriz, MA, 65900-410 (Brazil); Universidade Federal do Sul e Sudeste do Pará, ICEN, Marabá, PA 68505-080 (Brazil); Carvalho, J.O. [Universidade Federal do Maranhão, CCSST, Imperatriz, MA, 65900-410 (Brazil); Instituto Federal do Tocantins, Araguaína, TO, 77.826-170 (Brazil); Silva, M.C.D.; Façanha Filho, P.F. [Universidade Federal do Maranhão, CCSST, Imperatriz, MA, 65900-410 (Brazil); Santos, A.O. dos, E-mail: adenilson1@gmail.com [Universidade Federal do Maranhão, CCSST, Imperatriz, MA, 65900-410 (Brazil)

    2015-09-01

    L-Histidinium bromide monohydrate (LHBr) single crystal is a nonlinear optical material. In this work the high temperature phase transformation and the thermal stability of single crystals of LHBr was investigated by X-ray diffraction, thermogravimetric analysis, differential thermal analysis, differential scanning calorimetry and Raman spectroscopy. The results showed the LHBr phase transformation of orthorhombic (P2{sub 1}2{sub 1}2{sub 1}) to monoclinic system (P 1 2 1) at 120 °C, with the lattice parameters a = 12.162(1) Å, b = 16.821(2) Å, c = 19.477(2) Å and β = 108.56(2)°. These techniques are complementary and confirm the structural phase transformation due to loss water of crystallization. - Highlights: • -histidinium bromide single crystal was grown by slow evaporation technique. • X-ray diffraction characterize the high-temperature phase transformation. • The structural phase transformation occur due to loss of water of crystallization. • The LHBr thermal expansion coefficients exhibit an anisotropic behavior.

  1. Growth, structural and magnetic characterization of Al-substituted barium hexaferrite single crystals

    International Nuclear Information System (INIS)

    Vinnik, D.A.; Zherebtsov, D.A.; Mashkovtseva, L.S.; Nemrava, S.; Bischoff, M.; Perov, N.S.; Semisalova, A.S.; Krivtsov, I.V.; Isaenko, L.I.; Mikhailov, G.G.; Niewa, R.

    2014-01-01

    Highlights: • Growth of large Al-substituted crystals BaFe 12−x Al x O 19. • Al-content controllable by flux composition. • Crystallographic site preference of Al unraveled. • Magnetic characterization depending on Al-content. - Abstract: Large single crystals of aluminum-substituted M-type barium hexaferrite BaFe 12−x Al x O 19 were obtained from carbonate flux. The Al content in the crystals can be controlled via the Al content of the flux up to x = 1.1 according to single crystal X-ray structure refinements. Al shows a distinct preference to substitute Fe on crystallographic sites with high coordination numbers by oxygen atoms, whereas no significant amounts of Al can be found on a tetrahedrally coordinated site. An increasing amount of the aluminum dopant results in a monotonous reduction of the Curie temperature from 440 to 415 °C and the saturation magnetization at room temperature from 68 to 57 emu/g for single crystal and from 61 to 53 emu/g for powder samples

  2. The synthesis, characterization, crystal structure and theoretical calculations of a new meso-BOBIPY substituted phthalonitrile

    International Nuclear Information System (INIS)

    Sen, Pinar; Yildiz, S. Zeki; Atalay, Yusuf; Dege, Necmi; Demirtas, Günes

    2014-01-01

    A novel 4-(2-meso-BOBIPY-phenoxy)phthalonitrile (6) derivative has been synthesized starting from BF 3 –OEt 2 complex and 4-(2-meso-dipyrromethene-phenoxy)phthalonitrile (5) which was prepared by the oxidation of 4-(2-meso-dipyrromethane-phenoxy)phthalonitrile (4). The final product exhibit noticeable spectroscopic properties which were examined by its absorption and fluorescence emission spectra. The original compounds prepared in the reaction pathway were characterized by the combination of FT-IR, 1 H and 13 C NMR, UV–vis, MS and HRMS spectral data. The final product (6) was obtained as single crystal which crystallized in the triclinic space group P-1 with a=7.9411 (6) Å, b=9.0150 (6) Å, c=14.419 (1) Å, α=74.917 (5)°, β=86.824 (6)°, γ=84.109 (5)° and Z=2. The crystal structure has intermolecular C–H···F–B and C–H···N interactions. These interactions construct bifurcated hydrogen bonds in the crystal structure. In this study, It has been calculated; molecular structure, vibrational frequencies, 1 H and 13 C NMR chemical shifts and HOMO and LUMO energies of the title compound by using B3LYP method with 6–311++G(dp) basis set, and the electronic spectral characterization was investigated for the target product, as well. - Highlights: • A novel 4-(2-meso-BOBIPY-phenoxy)phthalonitrile derivative has been synthesized. • The title product exhibit noticeable spectroscopic properties which were examined by its absorption and fluorescence emission spectra. • The final product (6) was obtained as single crystal which crystallized in the triclinic space group. • Molecular structure, vibrational frequencies, 1 H and 13 C NMR chemical shifts and HOMO and LUMO energies of the title compound were calculated theoretically. • The electronic spectral characterization was investigated, as well. • The title compound is also open to prepare further BODIPY substituted oligomeric molecules via on it

  3. Synthesis, crystal structure, characterizations and magnetic study of a novel two-dimensional iron fluoride

    Science.gov (United States)

    Bouketaya, Sabrine; Smida, Mouna; Abdelbaky, Mohammed S. M.; Dammak, Mohamed; García-Granda, Santiago

    2018-06-01

    A new hybrid compound formulated as [Fe3F8(H2O)2](Am2TAZ)2 (Am2TAZ= 3,5-diamino-1,2,4-triazole) was prepared under hydrothermal conditions. The crystal structure was solved by single-crystal X-ray diffraction and the bulk was characterized by thermal analyses (TG-MS), vibrational spectroscopy (FTIR, Raman), Ultraviolet-visible spectroscopy (UV-Vis), and scanning electron microscopy (SEM-EDX). It crystallizes in the triclinic system space group P 1 ̅ with unit cell parameters a= 7.100(2) Å, b= 7.658(2) Å, c= 8.321(2) Å, α = 107.330(20)°, β = 111.842(18)°, γ = 93.049(17)°, Z = 1 and V= 394.01(17) Å3. The studied X-ray crystal structure shows the two oxidation states for iron atoms (Fe2+, Fe3+) and generates a 2D inorganic network, built up of inorganic layers constructed from infinite inorganic chains running along a axis. In fact, these chains are connected via (Fe3+(3)F6) octahedral. OW-H…F and N-H…F hydrogen bonds, making up the whole 3D network, are strongly linked in the layers. Magnetization measurements were performed, exhibiting the paramagnetic feature of the studied compound above 150 K.

  4. Structural characterization of H plasma-doped ZnO single crystals by positron annihilation spectroscopies

    Energy Technology Data Exchange (ETDEWEB)

    Anwand, Wolfgang; Brauer, Gerhard; Cowan, Thomas E. [Institut fuer Strahlenphysik, Forschungszentrum Dresden-Rossendorf, P.O. Box 510 119, 01314 Dresden (Germany); Grambole, Dieter; Skorupa, Wolfgang [Institut fuer Ionenstrahlphysik und Materialforschung, Forschungszentrum Dresden-Rossendorf, P.O. Box 510 119, 01314 Dresden (Germany); Cizek, Jakub; Kuriplach, Jan; Prochazka, Ivan [Department of Low Temperature Physics, Charles University, V Holesovickach 2, 18000 Prague (Czech Republic); Egger, Werner; Sperr, Peter [Institut fuer Angewandte Physik und Messtechnik, Fakultaet fuer Luft- und Raumfahrttechnik, Universitaet der Bundeswehr, Heisenbergweg 39, 85579 Neubiberg (Germany)

    2010-11-15

    Nominally undoped, hydrothermally grown ZnO single crystals have been investigated before and after exposure to remote H plasma. Structural characterizations have been made by various positron annihilation spectroscopies (continuous and pulsed slow positron beams, conventional lifetime). The content of bound hydrogen (H-b) before and after the remote H plasma treatment at the polished side of the crystals was determined at depths of 100 and 600 nm, respectively, using nuclear reaction analysis. At a depth of 100 nm, H-b increased from (11.8{+-}2.5) to (48.7{+-}7.6) x 10{sup 19} cm{sup -3} after remote H plasma treatment, whereas at 600 nm no change in H-b was observed. (Copyright copyright 2010 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  5. Crystal structure and characterization of a novel L-serine ammonia-lyase from Rhizomucor miehei

    Energy Technology Data Exchange (ETDEWEB)

    Qin, Zhen [College of Food Science and Nutritional Engineering, Beijing Advanced Innovation Center of Food Nutrition and Human Health, China Agricultural University, Beijing 100083 (China); Yan, Qiaojuan [College of Engineering, China Agricultural University, Beijing 100083 (China); Ma, Qingjun [Key Laboratory of Experimental Marine Biology, Institute of Oceanology, Chinese Academy of Sciences, Qingdao 266071 (China); Jiang, Zhengqiang, E-mail: zhqjiang@cau.edu.cn [College of Food Science and Nutritional Engineering, Beijing Advanced Innovation Center of Food Nutrition and Human Health, China Agricultural University, Beijing 100083 (China)

    2015-10-23

    L-serine ammonia-lyase, as a member of the β-family of pyridoxal-5′-phosphate (PLP) dependent enzymes, catalyzes the conversion of L-serine (L-threonine) to pyruvate (α-ketobutyrate) and ammonia. The crystal structure of L-serine ammonia-lyase from Rhizomucor miehei (RmSDH) was solved at 1.76 Å resolution by X-ray diffraction method. The overall structure of RmSDH had the characteristic β-family PLP dependent enzyme fold. It consisted of two distinct domains, both of which show the typical open twisted α/β structure. A PLP cofactor was located in the crevice between the two domains, which was attached to Lys52 by a Schiff-base linkage. Unique residue substitutions (Gly78, Pro79, Ser146, Ser147 and Thr312) were discovered at the catalytic site of RmSDH by comparison of structures of RmSDH and other reported eukaryotic L-serine ammonia-lyases. Optimal pH and temperature of the purified RmSDH were 7.5 and 40 °C, respectively. It was stable in the pH range of 7.0–9.0 and at temperatures below 40 °C. This is the first crystal structure of a fungal L-serine ammonia-lyase. It will be useful to study the catalytic mechanism of β-elimination enzymes and will provide a basis for further enzyme engineering. - Highlights: • The crystal structure of a fungal L-serine ammonia-lyase (RmSDH) was solved. • Five unique residue substitutions are found at the catalytic site of RmSDH. • RmSDH was expressed in Pichia. pastoris and biochemically characterized. • RmSDH has potential application in splitting D/L-serine.

  6. Reversible Single-Crystal-to-Single-Crystal Structural Transformation in a Mixed-Ligand 2D Layered Metal-Organic Framework: Structural Characterization and Sorption Study

    Directory of Open Access Journals (Sweden)

    Chih-Chieh Wang

    2017-12-01

    Full Text Available A 3D supramolecular network, [Cd(bipy(C4O4(H2O2]·3H2O (1 (bipy = 4,4′-bipyridine and C4O42− = dianion of H2C4O4, constructed by mixed-ligand two-dimensional (2D metal-organic frameworks (MOFs has been reported and structurally determined by the single-crystal X-ray diffraction method and characterized by other physicochemical methods. In 1, the C4O42− and bipy both act as bridging ligands connecting the Cd(II ions to form a 2D layered MOF, which are then extended to a 3D supramolecular network via the mutually parallel and interpenetrating arrangements among the 2D-layered MOFs. Compound 1 shows a two-step dehydration process with weight losses of 11.0% and 7.3%, corresponding to the weight-loss of three guest and two coordinated water molecules, respectively, and exhibits an interesting reversible single-crystal-to-single-crystal (SCSC structural transformation upon de-hydration and re-hydration for guest water molecules. The SCSC structural transformation have been demonstrated and monitored by single-crystal and X-ray powder diffraction, and thermogravimetic analysis studies.

  7. Physiochemical Characterization of Iodine (V Oxide Part II: Morphology and Crystal Structure of Particulate Films

    Directory of Open Access Journals (Sweden)

    Brian K. Little

    2015-11-01

    Full Text Available In this study, the production of particulate films of iodine (V oxides is investigated. The influence that sonication and solvation of suspended particles in various alcohol/ketone/ester solvents have on the physical structure of spin or drop cast films is examined in detail with electron microscopy, powder x-ray diffraction, and UV-visible absorption spectroscopy. Results indicate that sonicating iodine oxides in alcohol mixtures containing trace amounts of water decreases deposited particle sizes and produces a more uniform film morphology. UV-visible spectra of the pre-cast suspensions reveal that for some solvents, the iodine oxide oxidizes the solvent, producing I2 and lowering the pH of the suspension. Characterizing the crystals within the cast films reveal their composition to be primarily HI3O8, their orientations to exhibit a preferential orientation, and their growth to be primarily along the ac-plane of the crystal, enhanced at higher spin rates. Spin-coating at lower spin rates produces laminate-like particulate films versus higher density, one-piece films of stacked particles produced by drop casting. The particle morphology in these films consists of a combination of rods, plates, cubes, and rhombohedra structure.

  8. Synthesis, characterization, crystal structure and quantum chemical investigations of three novel coumarin-benzenesulfonohydrazide derivatives

    Science.gov (United States)

    Chethan Prathap, K. N.; Lokanath, N. K.

    2018-04-01

    Coumarin derivatives are an important class of heterocyclic compounds due to their physical and biological properties. Coumarin derivatives have been identified with many significant electro-optical properties and biological activities. Three novel coumarin derivatives containing benzene sulfonohydrazide group were synthesized by condensation reaction. The synthesized compounds were characterized by various spectroscopic techniques (Mass, 1H/13C NMR and FTIR). Thermal and optical properties were investigated by thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and UV-Vis spectroscopic studies. Finally their structures were confirmed by single crystal X-ray diffraction (XRD) studies. The three compounds exhibit diverse intermolecular interactions, as observed by the crystal packing and Hirshfeld surface analysis. Further, their structures were optimized by density functional theory (DFT) calculations using B3LYP hybrid functionals with 6-311G+(d,p) level basis set. The Mulliken charge, molecular electrostatic potential (MEP), frontier molecular orbitals (HOMO-LUMO) were investigated. The experimentally determined parameters were compared with those calculated theoretically and they complement each other with a very good correlation. The transitions among the molecular orbitals were investigated using time-dependent density functional theory (TD-DFT) and the electronic absorption spectra obtained showed very good agreement with the experimentally measured UV-Vis spectra. Furthermore, non-linear optical (NLO) properties were investigated by calculating polarizabilities and hyperpolarizabilities. All three compounds exhibit significantly high hyperpolarizabilities compared to the reference material urea, which makes them potential candidates for NLO applications.

  9. Purification, crystal structure determination and functional characterization of type III antifreeze proteins from the European eelpout Zoarces viviparus

    DEFF Research Database (Denmark)

    Wilkens, Casper; Poulsen, Jens-Christian Navarro; Ramløv, Hans

    2014-01-01

    Antifreeze proteins (AFPs) are essential components of many organisms adaptation to cold temperatures. Fish type III AFPs are divided into two groups, SP isoforms being much less active than QAE1 isoforms. Two type III AFPs from Zoarces viviparus, a QAE1 (ZvAFP13) and an SP (ZvAFP6) isoform......, are here characterized and their crystal structures determined. We conclude that the higher activity of the QAE1 isoforms cannot be attributed to single residues, but rather a combination of structural effects. Furthermore both ZvAFP6 and ZvAFP13 crystal structures have water molecules around T18...... equivalent to the tetrahedral-like waters previously identified in a neutron crystal structure. Interestingly, ZvAFP6 forms dimers in the crystal, with a significant dimer interface. The presence of ZvAFP6 dimers was confirmed in solution by native electrophoresis and gel filtration. To our knowledge...

  10. Structural Characterization of Doped GaSb Single Crystals by X-ray Topography

    Energy Technology Data Exchange (ETDEWEB)

    Honnicke, M.G.; Mazzaro, I.; Manica, J.; Benine, E.; M da Costa, E.; Dedavid, B. A.; Cusatis, C.; Huang, X. R.

    2009-09-13

    We characterized GaSb single crystals containing different dopants (Al, Cd and Te), grown by the Czochralski method, by x-ray topography and high angular resolution x-ray diffraction. Lang topography revealed dislocations parallel and perpendicular to the crystal's surface. Double-crystal GaSb 333 x-ray topography shows dislocations and vertical stripes than can be associated with circular growth bands. We compared our high-angular resolution x-ray diffraction measurements (rocking curves) with the findings predicted by the dynamical theory of x-ray diffraction. These measurements show that our GaSb single crystals have a relative variation in the lattice parameter ({Delta}d/d) on the order of 10{sup -5}. This means that they can be used as electronic devices (detectors, for example) and as x-ray monochromators.

  11. Synthesis, characterization and crystal structure of N,N'-Bis(2,3-Dimethoxybenzylidene)-1,2-Diaminoethane

    Czech Academy of Sciences Publication Activity Database

    Khalaji, A.D.; Fejfarová, Karla; Dušek, Michal; Bijanzadeh, H.R.

    2011-01-01

    Roč. 41, č. 12 (2011), 1955-1960 ISSN 1074-1542 Institutional research plan: CEZ:AV0Z10100521 Keywords : Shiff bases * X-ray diffraction * Jana2006 * crystal structure * characterization Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.566, year: 2011

  12. Organic compounds containing methoxy and cyanoacrylic acid: Synthesis, characterization, crystal structures, and theoretical studies

    Energy Technology Data Exchange (ETDEWEB)

    Khalaji, A. D., E-mail: alidkhalaji@yahoo.com [Golestan University, Department of Chemistry, Faculty of Science (Iran, Islamic Republic of); Maddahi, E. [Iran University of Science & Technology, Ms.C Educated, Department of Chemistry (Iran, Islamic Republic of); Dusek, M.; Fejfarova, K. [Institute of Physics of the ASCR, v.v.i. (Czech Republic); Chow, T. J. [Academia Sinica, Institute of Chemistry (China)

    2015-12-15

    Metal-free organic compounds 24-SC ((E)-2-cyano-3-(2,4-dimethoxyphenyl)acrylic acid) and 34-SC ((E)-2-cyano-3-(3,4-dimethoxyphenyl)acrylic acid), containing methoxy groups as a donor and the acrylic acid as an acceptor were synthesized and characterized by CHN, FT-IR, UV-Vis, {sup 1}H-NMR and single crystal X-ray diffraction and used as photosensitizers for the application of dye-sensitized solar cells (DSSC). The sensitizing characteristics of them were evaluated. Both compounds contain the natural molecule, its anionic form and the piperidinium cation and they differ by number of these molecules in the asymmetric unit. To get further insight into the effect of molecular structure on the performance of DSSC, their geometry and energies of HOMO and LUMO were optimized by density functional theory calculation at the B3LYP/6-31G(d) level with Gaussian 03. Overall conversion efficiencies of 0.78 under full sunlight irradiation are obtained for DSSCs based on the new metal-free organic dyes 24-SC and 34-SC.

  13. The purification, crystallization and preliminary structural characterization of human MAWDBP, a member of the phenazine biosynthesis-like protein family

    International Nuclear Information System (INIS)

    Herde, Petra; Blankenfeldt, Wulf

    2006-01-01

    The purification, crystallization and preliminary structural characterization of human MAWD-binding protein (MAWDBP) are described. MAWDBP is the only representative of the phenazine biosynthesis-like protein family in the human genome. Its expression is elevated in several disease processes, including insulin resistance, folate deficiency and hypotension, and it may also be involved in carcinogenesis. The exact molecular function of MAWDBP is unknown. Native and seleno-l-methionine-labelled MAWDBP were expressed in Escherichia coli and crystallized at room temperature from precipitants containing 10 mM KF, 14%(w/v) PEG 3350 and 0.1 M sodium citrate pH 5.4. Crystals belong to space group H32, with unit-cell parameters a = b = 187, c = 241 Å, indicative of three to five monomers per asymmetric unit. Crystals were cryoprotected with 15%(v/v) glycerol and data have been collected to 2.7 Å resolution

  14. The purification, crystallization and preliminary structural characterization of human MAWDBP, a member of the phenazine biosynthesis-like protein family

    Energy Technology Data Exchange (ETDEWEB)

    Herde, Petra; Blankenfeldt, Wulf, E-mail: wulf.blankenfeldt@mpi-dortmund.mpg.de [Max-Planck-Institute of Molecular Physiology, Otto-Hahn-Strasse 11, 44227 Dortmund (Germany)

    2006-06-01

    The purification, crystallization and preliminary structural characterization of human MAWD-binding protein (MAWDBP) are described. MAWDBP is the only representative of the phenazine biosynthesis-like protein family in the human genome. Its expression is elevated in several disease processes, including insulin resistance, folate deficiency and hypotension, and it may also be involved in carcinogenesis. The exact molecular function of MAWDBP is unknown. Native and seleno-l-methionine-labelled MAWDBP were expressed in Escherichia coli and crystallized at room temperature from precipitants containing 10 mM KF, 14%(w/v) PEG 3350 and 0.1 M sodium citrate pH 5.4. Crystals belong to space group H32, with unit-cell parameters a = b = 187, c = 241 Å, indicative of three to five monomers per asymmetric unit. Crystals were cryoprotected with 15%(v/v) glycerol and data have been collected to 2.7 Å resolution.

  15. Synthesis, characterization and crystal structures of new organic compounds containing cyanoacrylic acid

    Czech Academy of Sciences Publication Activity Database

    Khalaji, A.D.; Mogheiseh, M.; Eigner, Václav; Dušek, Michal; Chow, T.J.; Maddahi, E.

    2015-01-01

    Roč. 1098, Oct (2015), s. 318-323 ISSN 0022-2860 R&D Projects: GA ČR(CZ) GA14-03276S Institutional support: RVO:68378271 Keywords : organic compounds * cyanoacrylic acid * single-crystal structure analysis * dye-sensitized solar cells * density functional theory Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.780, year: 2015

  16. Synthesis, characterization, crystal structures, QSAR study and antibacterial activities of organotin bisphosphoramidates

    Czech Academy of Sciences Publication Activity Database

    Gholivand, K.; Valmoozi, A.A.E.; Gholami, A.; Dušek, Michal; Eigner, Václav; Abolghasemi, S.

    2016-01-01

    Roč. 806, Mar (2016), s. 33-44 ISSN 0022-328X R&D Projects: GA ČR GA15-12653S Institutional support: RVO:68378271 Keywords : bisphosphoramidate * organotin compounds * crystal structure * antibacterial activity * QSAR Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 2.184, year: 2016

  17. Synthesis, crystal structure, spectroscopic characterization and nonlinear optical properties of Co(II)- picolinate complex

    Energy Technology Data Exchange (ETDEWEB)

    Tamer, Ömer, E-mail: omertamer@sakarya.edu.tr; Avcı, Davut; Atalay, Yusuf

    2015-11-15

    A cobalt(II) complex of picolinate was synthesized, and its structure was fully characterized by the applying of X-ray diffraction method as well as FT-IR, FT-Raman and UV–vis spectroscopies. In order to both support the experimental results and convert study to more advanced level, density functional theory calculations were performed by using B3LYP level. Single crystal X-ray structural analysis shows that cobalt(II) ion was located to the center of distorted octahedral geometry. The C=O, C=C and C=N stretching vibrations were found as highly active and strong peaks, inducing the molecular charge transfer within Co(II) complex. The small energy gap between frontier molecular orbital energies was another indicator of molecular charge transfer interactions within Co(II) complex. The nonlinear optical properties of Co(II) complex were investigated at DFT/B3LYP level, and the hypepolarizability parameter was found to be decreased due to the presence of inversion symmetry. The natural bond orbital (NBO) analysis was performed to investigate molecular stability, hyperconjugative interactions, intramolecular charge transfer (ICT) and bond strength for Co(II) complex. Finally, molecular electrostatic potential (MEP) and spin density distributions for Co(II) complex were evaluated. - Highlights: • Co(II) complex of picolinate was prepared. • Its FT-IR, FT-Raman and UV–vis spectra were measured. • DFT calculations were performed to support experimental results. • Small HOMO-LUMO energy gap is an indicator of molecular charge transfer. • Spin density localized on Co(II) as well as O and N atoms.

  18. Crystal structure and functional characterization of SF216 from Shigella flexneri.

    Science.gov (United States)

    Kim, Ha-Neul; Seok, Seung-Hyeon; Lee, Yoo-Sup; Won, Hyung-Sik; Seo, Min-Duk

    2017-11-01

    Shigella flexneri is a Gram-negative anaerobic bacterium that causes highly infectious bacterial dysentery in humans. Here, we solved the crystal structure of SF216, a hypothetical protein from the S. flexneri 5a strain M90T, at 1.7 Å resolution. The crystal structure of SF216 represents a homotrimer stabilized by intersubunit interactions and ion-mediated electrostatic interactions. Each subunit consists of three β-strands and five α-helices with the β-β-β-α-α-α-α-α topology. Based on the structural information, we also demonstrate that SF216 shows weak ribonuclease activity by a fluorescence quenching assay. Furthermore, we identify potential druggable pockets (putative hot spots) on the surface of the SF216 structure by computational mapping. © 2017 Federation of European Biochemical Societies.

  19. Synthesis, characterization and x-ray crystal structure of a dimethyltin (IV) dichloride complex of 2-acetylpyridine benzophenone azine

    International Nuclear Information System (INIS)

    Mustaffa Shamsuddin; Md Abu Affan; Ramli Atan

    1998-01-01

    Dimethyltin dichloride react with 2-ac ethylpyridine benzophenone azine (apba) in refluxing dry hexane to give (SnMe 2 Cl 2 (apba)) where the azine ligand acts as a bidentate N-N chelating ligand. The complex has been characterized by IR spectroscopy, 1 H and 13 C NMR spectroscopic data and elemental analyses. The crystal structure of the dimethyltin(IV) derivative has also been determined. Crystals are monoclinic with space group P2(1)/n with cell dimensions: a = 10.1819(3) Armstrong, b = 18.3113(5) Armstrong, c = 12.6451(4) Armstrong

  20. New organic single crystal of (benzylthio)acetic acid: Synthesis, crystal structure, spectroscopic (ATR-FTIR, 1H and 13C NMR) and thermal characterization

    Science.gov (United States)

    Sienkiewicz-Gromiuk, Justyna; Tarasiuk, Bogdan; Mazur, Liliana

    2016-04-01

    (Benzylthio)acetic acid (Hbta) was synthesized with 78% yield from benzyl chloride and thiourea as substrates. Well-shaped crystals of Hbta were grown by slow solvent evaporation technique from pure methanol. The compound was investigated by single-crystal X-ray and powder diffraction techniques and was also characterized by other analytical methods, like ATR-FTIR, 1H and 13C NMR and TG/DSC. The acid molecule adopts bent conformation in the solid state. The crystal structure of Hbta is stabilized by numerous intermolecular interactions, including O-H···O, C-H···O, C-H···S and C-H···π contacts. Thermal decomposition of the obtained material takes place above 150 °C.

  1. Structural characterization of bulk GaN crystals grown under high hydrostatic pressure

    Science.gov (United States)

    Liliental-Weber, Zuzanna; Kisielowski, C.; Ruvimov, S.; Chen, Y.; Washburn, J.; Grzegory, I.; Bockowski, M.; Jun, J.; Porowski, S.

    1996-09-01

    This paper describes TEM characterization of bulk GaN crystals grown at 1500-1800Kin the form of plates from a solution of atomic nitrogen in liquid gallium under high nitrogen pressure (up to 20 kbars). The x-ray rocking curves for these crystals were in the range of 20-30 arc-sec. The plate thickness along the c axis was about 100 times smaller than the nonpolar growth directions. A substantial difference in material quality was observed on the opposite sides of the plates normal to the c direction. On one side the surface was atomically flat, while on the other side the surface was rough, with pyramidal features up to 100 nm high. The polarity of the crystals was determined using convergent-beam electron diffraction. The results showed that, regarding the long bond between Ga and N along the c-axis, Ga atoms were found to be closer to the flat side of the crystal, while N atoms were found to be closer to the rough side. Near the rough side, within 1/10 to 1/4 of the plate thickness, there was a high density of planar defects (stacking faults and dislocation loops decorated by Ga/void precipitates). A model explaining the defect formation is proposed.

  2. Bis[(2,3,4-Trimethoxy-Benzylidenepropylideneamino)Phenyl] Ether: Synthesis, characterization and crystal structure

    Czech Academy of Sciences Publication Activity Database

    Khalaji, A.D.; Fejfarová, Karla; Dušek, Michal

    2012-01-01

    Roč. 42, č. 3 (2012), s. 263-266 ISSN 1074-1542 Grant - others:AV ČR(CZ) AP0701 Program:Akademická prémie - Praemium Academiae Institutional research plan: CEZ:AV0Z10100521 Keywords : Shiff bases * crystal structure * X-ray diffraction * Jana2006 Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.513, year: 2012

  3. Crystal structure and characterization of the novel NH+⋯N hydrogen bonded polar crystal [NH2(CH2)4NH][BF4

    International Nuclear Information System (INIS)

    Wojtaś, M.; Gagor, A.; Czupiński, O.; Medycki, W.; Jakubas, R.

    2012-01-01

    Dielectric properties and phase transitions of the piperazinium tetrafluoroborate ([NH 2 (CH 2 ) 4 NH][BF 4 ], abbreviated as PFB) crystal are related to the one-dimensional arrangement of the cations linked by the bistable NH + ⋯N hydrogen bonds and molecular motions of the [BF 4 ] − units. The crystal structure of [NH 2 (CH 2 ) 4 NH][BF 4 ] is monoclinic at room temperature with the polar space group Pn. The polar/acentric properties of the room temperature phase IV have been confirmed by the piezoelectric and pyroelectric measurements. DSC measurements show that the compound undergoes three first-order structural phase transitions: at 421/411 K (heating/cooling), at 386/372 K and at 364/349 K. 1 H and 19 F NMR measurements indicate the reorientational motions of [BF 4 ] − anions and piperazinium(+) cations as well as the proton motion in the hydrogen-bonded chains of piperazine along the [001] direction. Over the phase I the isotropic reorientational motions or even self-diffusion of the cations and anions are expected. The conductivity measurements in the vicinity of the II–I PT indicate a superionic phase over the phase I. - Graphical abstract: It must be emphasized that the titled compound represents the first organic–inorganic simple salt containing the single-protonated piperazinium cation which was studied by means of the wide variety of experimental techniques. A survey of Cambridge Structural Database (CSD version 5.32 (November 2010) and updates (May 2011)) for structure containing the piperazinium cations yields 248 compounds with the doubly protonated piperazinium(2+) cations and only eight compounds with the singly protonated piperazinium(+) cations. Among these structures only one is the hybrid organic–inorganic material. This is piperazinium nitrate characterized structurally. The crystal packing of [NH 2 (CH 2 ) 4 NH][BF 4 ], phase IV. The dashed lines stand for the hydrogen bonds. The hydrogen bonds to BF4 groups are not included for

  4. Biophysical characterization and crystal structure of the Feline Immunodeficiency Virus p15 matrix protein.

    Science.gov (United States)

    Serrière, Jennifer; Robert, Xavier; Perez, Magali; Gouet, Patrice; Guillon, Christophe

    2013-06-24

    Feline Immunodeficiency Virus (FIV) is a viral pathogen that infects domestic cats and wild felids. During the viral replication cycle, the FIV p15 matrix protein oligomerizes to form a closed matrix that underlies the lipidic envelope of the virion. Because of its crucial role in the early and late stages of viral morphogenesis, especially in viral assembly, FIV p15 is an interesting target in the development of potential new therapeutic strategies. Our biochemical study of FIV p15 revealed that it forms a stable dimer in solution under acidic conditions and at high concentration, unlike other retroviral matrix proteins. We determined the crystal structure of full-length FIV p15 to 2 Å resolution and observed a helical organization of the protein, typical for retroviral matrix proteins. A hydrophobic pocket that could accommodate a myristoyl group was identified, and the C-terminal end of FIV p15, which is mainly unstructured, was visible in electron density maps. As FIV p15 crystallizes in acidic conditions but with one monomer in the asymmetric unit, we searched for the presence of a biological dimer in the crystal. No biological assembly was detected by the PISA server, but the three most buried crystallographic interfaces have interesting features: the first one displays a highly conserved tryptophan acting as a binding platform, the second one is located along a 2-fold symmetry axis and the third one resembles the dimeric interface of EIAV p15. Because the C-terminal end of p15 is involved in two of these three interfaces, we investigated the structure and assembly of a C-terminal-truncated form of p15 lacking 14 residues. The truncated FIV p15 dimerizes in solution at a lower concentration and crystallizes with two molecules in the asymmetric unit. The EIAV-like dimeric interface is the only one to be retained in the new crystal form. The dimeric form of FIV p15 in solution and its extended C-terminal end are characteristic among lentiviral matrix proteins

  5. First crystal structures of pharmaceutical ibrutinib: systematic solvate screening and characterization

    Czech Academy of Sciences Publication Activity Database

    Zvoníček, V.; Skořepová, E.; Dušek, Michal; Babor, M.; Zvatora, P.; Šoós, M.

    2017-01-01

    Roč. 17, č. 6 (2017), s. 3116-3127 ISSN 1528-7483 R&D Projects: GA MŠk LO1603; GA ČR GA17-23196S EU Projects: European Commission(XE) CZ.2.16/3.1.00/24510 Institutional support: RVO:68378271 Keywords : Ibrutinib solvates * anticancer drug * Raman spectroscopy * powder X-ray diffraction * crystal structure Subject RIV: BM - Solid Matter Physics ; Magnetism OBOR OECD: Condensed matter physics (including formerly solid state physics, supercond.) Impact factor: 4.055, year: 2016

  6. Spectral characterization and crystal structure of 2-amino-N′-[(1Z-1-(4-chlorophenylethylidene]-benzohydrazide

    Directory of Open Access Journals (Sweden)

    Mohammad Arfan

    2016-01-01

    Full Text Available The crystal structure of 2-amino-N′-[(1Z-1-(4-chlorophenylethylidene]benzohydrazide (I is determined by X-ray diffraction at room temperature. The structure of I also was characterized by elemental analysis, mass, FT-IR and NMR spectroscopic techniques. The compound crystallizes in triclinic system, and space group is P1¯. Unit-cell dimensions are the following: a = 7.05380(10 Å, b = 7.65490(10 Å, c = 13.7094(4 Å, V = 694.01(2 Å3, Z = 2. The title compound is nearly planar and has intermolecular N–H⋯O hydrogen bonding. According to the spectral data, I exhibits an amide-iminol tautomerism.

  7. Synthesis, characterization, crystal structure and theoretical study of a compound with benzodiazole ring: antimicrobial activity and DNA binding.

    Science.gov (United States)

    Latha, P; Kodisundaram, P; Sundararajan, M L; Jeyakumar, T

    2014-08-14

    2-(Thiophen-2-yl)-1-((thiophen-2-yl)methyl)-1H-1,3-benzodiazole (HL) is synthesized and characterized by elemental analysis, UV-Vis, FT-IR, (1)H, (13)C NMR, mass spectra, scanning electron microscope (SEM) and single crystal X-ray diffraction. The crystal structure is stabilized by intermolecular CH⋯N and CH⋯π interactions. The molecular structure is also optimized at the B3LYP/6-31G level using density functional theory (DFT). The structural parameters from the theory are nearer to those of crystal, the calculated total energy of coordination is -1522.814a.u. The energy of HOMO-LUMO and the energy gap are -0.20718, -0.04314, 0.16404a.u, respectively. All data obtained from the spectral studies support the structural properties of the compound HL. The benzimidazole ring is essentially planar. The in vitro biological screening effects of the synthesized compound is tested against four bacterial and four fungal strains by well diffusion method. Antioxidant property and DNA binding behaviour of the compound has been investigated using spectrophotometric method. Copyright © 2014 Elsevier B.V. All rights reserved.

  8. Zinc(II) halide complexes with 2-methoxyaniline ligand: Synthesis, characterization, thermal analyses, crystal structure determination and luminescent properties

    Science.gov (United States)

    Amani, Vahid

    2018-03-01

    Three new mononuclear zinc(II) complexes, [Zn(2-MeO-C6H4NH2)2X2] (X is Cl in 1, Br in 2 and I in 3), were prepared from the reactions of ZnX2 with 2-methoxyaniline (2-MeO-C6H4NH2) ligand in methanol. Suitable crystals of these complexes were obtained for X-ray diffraction measurements by slow evaporation of methanol solution at room temperature. The three complexes were thoroughly characterized by thermogravimetric analysis, elemental analysis (CHNO), spectral methods (IR, UV-Vis, 13C{1H}NMR, 1H NMR and luminescence), and single crystal X-ray diffraction. The X-ray structural analysis indicated that in the structures of these complexes, the zinc(II) cation is four-coordinated in a distorted tetrahedral configuration by two N atoms from two 2-methoxyanyline ligands and two halide anions. Also, in these complexes intermolecular interactions, for example Nsbnd H⋯X hydrogen bonds (in 1-3), Csbnd H⋯X hydrogen bonds (in 3), Csbnd H⋯π interactions (in 1 and 2) and π⋯π interactions (in 3), are effective in the stabilization of the crystal structures. In addition, the luminescence spectra of all complexes in methanolic solution show that the intensity of their emission bands is stronger than that for free 2-methoxyaniline ligand.

  9. Synthesis, characterization, and crystal structures of diruthenium complexes containing bridging salicylato ligands

    Energy Technology Data Exchange (ETDEWEB)

    Jiang, Mingxuan; Yau, Chun Huan; Hu, Yuxin; Tan, Yong Leng Kelvin [Hwa Chong Institution (Singapore); Li, Yingzhou; Ganguly, Rakesh; Leong, Weng Kee [Division of Chemistry and Biological Chemistry, School of Physical and Mathematical Sciences, Nanyang Technological University (Singapore)

    2017-08-03

    The thermal reaction of Ru{sub 3}(CO){sub 12} (1) with salicylic acid, in the presence of triphenylphosphine, pyridine, or dimethylsulfoxide, afforded the dinuclear complexes Ru{sub 2}(CO){sub 4}(μ-O{sub 2}CC{sub 6}H{sub 4}OH){sub 2}L{sub 2} (2) [L = PPh{sub 3} (2a). C{sub 5}H{sub 5}N (2b); (CH{sub 3}){sub 2}SO (2c)]. Complex 2b was further reacted with the aromatic dimmines 2,2'-dipyridine or 1,10-phenanthroline to give the cationic diruthenium complexes [Ru{sub 2}(CO){sub 2}(μ-CO){sub 2}(μ-O{sub 2}CC{sub 6}H{sub 4}OH)(N intersection N){sub 2}]{sup +} (3) [(N intersection N) = 2,2'-dipyridine (3a); 1,10-phenanthroline (3b)], which were isolated as their tetraphenylborate salts. All five novel complexes were characterized spectroscopically and analytically. For 2a-2b and 3a-3b, single-crystal X-ray diffraction studies were also carried out. (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  10. Febuxostat-Minoxidil Salt Solvates: Crystal Structures, Characterization, Interconversion and Solubility Performance

    Directory of Open Access Journals (Sweden)

    Li-Yang Li

    2018-02-01

    Full Text Available Three febuxostat-minoxidil salt solvates with acetone (ACE, tetrahydrofuran (THF and isopropanol (IPA are synthesized by solvent-assisted grinding and characterized by infrared (IR, nuclear magnetic resonance (1H-NMR, single crystal and powder X-ray diffraction (PXRD, thermogravimetry (TG and differential scanning calorimetry (DSC. These febuxostat-minoxidil salt solvates feature isostructural with the same stoichiometries (1:1:1 molecule ratio. The proton transfers from the carboxylic group of febuxostat (FEB to imino N atom of minoxidil (MIN, which forms the motif with combined R 2 2 (9 R 4 2 (8 R 2 2 (9 graph set in the three solvates. The solvents occupy the different positions related to the motif, which results in the apparent differences in PXRD patterns before/after desolvation although they are isostructures. The FEB-MIN·THF was more thermostable than FEB-MIN·ACE and FEB-MIN·IPA relative to solvent removal from DSC patterns, which is different from the results from the solvent-exchange experiments in chemical kinetics. All three salt solvates exhibit increased equilibrium solubility compared to FEB in aqueous medium.

  11. Synthesis and structural characterization of Na 2 MnP 2 O 7 crystal

    Indian Academy of Sciences (India)

    Na2MnP2O7 crystals were synthesized by hydrothermal technique. Crystals obtained are in the form of single crystals of rhombohedral morphology with lattice parameters as follows: triclinic, 1 ¯ , = 0.71069 Å, = 6.657(3) Å, = 6.714(6) Å, = 6.518(4) Å, = 112.31(6)°, = 92.14(4)°, = 83.89(5)°, = 268.0(3) Å3, ...

  12. Neutral-helium-atom diffraction from a micron-scale periodic structure: Photonic-crystal-membrane characterization

    Science.gov (United States)

    Nesse, Torstein; Eder, Sabrina D.; Kaltenbacher, Thomas; Grepstad, Jon Olav; Simonsen, Ingve; Holst, Bodil

    2017-06-01

    Surface scattering of neutral helium beams created by supersonic expansion is an established technique for measuring structural and dynamical properties of surfaces on the atomic scale. Helium beams have also been used in Fraunhofer and Fresnel diffraction experiments. Due to the short wavelength of the atom beams of typically 0.1 nm or less, Fraunhofer diffraction experiments in transmission have so far been limited to grating structures with a period (pitch) of up to 200 nm. However, larger periods are of interest for several applications, for example, for the characterization of photonic-crystal-membrane structures, where the period is typically in the micron to high submicron range. Here we present helium atom diffraction measurements of a photonic-crystal-membrane structure with a two-dimensional square lattice of 100 ×100 circular holes. The nominal period and the hole radius were 490 and 100 nm, respectively. To our knowledge this is the largest period that has been measured with helium diffraction. The helium diffraction measurements are interpreted using a model based on the helium beam characteristics. It is demonstrated how to successfully extract values from the experimental data for the average period of the grating, the hole diameter, and the width of the virtual source used to model the helium beam.

  13. Nanoscale characterization of local structures and defects in photonic crystals using synchrotron-based transmission soft X-ray microscopy

    Science.gov (United States)

    Nho, Hyun Woo; Kalegowda, Yogesh; Shin, Hyun-Joon; Yoon, Tae Hyun

    2016-01-01

    For the structural characterization of the polystyrene (PS)-based photonic crystals (PCs), fast and direct imaging capabilities of full field transmission X-ray microscopy (TXM) were demonstrated at soft X-ray energy. PS-based PCs were prepared on an O2-plasma treated Si3N4 window and their local structures and defects were investigated using this label-free TXM technique with an image acquisition speed of ~10 sec/frame and marginal radiation damage. Micro-domains of face-centered cubic (FCC (111)) and hexagonal close-packed (HCP (0001)) structures were dominantly found in PS-based PCs, while point and line defects, FCC (100), and 12-fold symmetry structures were also identified as minor components. Additionally, in situ observation capability for hydrated samples and 3D tomographic reconstruction of TXM images were also demonstrated. This soft X-ray full field TXM technique with faster image acquisition speed, in situ observation, and 3D tomography capability can be complementally used with the other X-ray microscopic techniques (i.e., scanning transmission X-ray microscopy, STXM) as well as conventional characterization methods (e.g., electron microscopic and optical/fluorescence microscopic techniques) for clearer structure identification of self-assembled PCs and better understanding of the relationship between their structures and resultant optical properties. PMID:27087141

  14. Crystal Structure and Biochemical Characterization of a Mycobacterium smegmatis AAA-Type Nucleoside Triphosphatase Phosphohydrolase (Msm0858).

    Science.gov (United States)

    Unciuleac, Mihaela-Carmen; Smith, Paul C; Shuman, Stewart

    2016-05-15

    AAA proteins (ATPases associated with various cellular activities) use the energy of ATP hydrolysis to drive conformational changes in diverse macromolecular targets. Here, we report the biochemical characterization and 2.5-Å crystal structure of a Mycobacterium smegmatis AAA protein Msm0858, the ortholog of Mycobacterium tuberculosis Rv0435c. Msm0858 is a magnesium-dependent ATPase and is active with all nucleoside triphosphates (NTPs) and deoxynucleoside triphosphates (dNTPs) as substrates. The Msm0858 structure comprises (i) an N-terminal domain (amino acids [aa] 17 to 201) composed of two β-barrel modules and (ii) two AAA domains, D1 (aa 212 to 473) and D2 (aa 476 to 744), each of which has ADP in the active site. Msm0858-ADP is a monomer in solution and in crystallized form. Msm0858 domains are structurally homologous to the corresponding modules of mammalian p97. However, the position of the N-domain modules relative to the AAA domains in the Msm0858-ADP tertiary structure is different and would impede the formation of a p97-like hexameric quaternary structure. Mutational analysis of the A-box and B-box motifs indicated that the D1 and D2 AAA domains are both capable of ATP hydrolysis. Simultaneous mutations of the D1 and D2 active-site motifs were required to abolish ATPase activity. ATPase activity was effaced by mutation of the putative D2 arginine finger, suggesting that Msm0858 might oligomerize during the ATPase reaction cycle. A truncated variant Msm0858 (aa 212 to 745) that lacks the N domain was characterized as a catalytically active homodimer. Recent studies have underscored the importance of AAA proteins (ATPases associated with various cellular activities) in the physiology of mycobacteria. This study reports the ATPase activity and crystal structure of a previously uncharacterized mycobacterial AAA protein, Msm0858. Msm0858 consists of an N-terminal β-barrel domain and two AAA domains, each with ADP bound in the active site. Msm0858 is a

  15. Crystal Structure and Spectroscopic Characterization of K8(VO)2O(SO4)6:

    DEFF Research Database (Denmark)

    Rasmussen, Søren Birk; Rasmussen, Rikke Christina; Fehrmann, Rasmus

    2003-01-01

    Red and yellow dichroistic crystals of a vanadium(V) compound, potassium (mu-oxo, di-mu-suifato)bis(oxodisulfato-vanadate), K-8(VO)(2)O(SO4)(6), have been obtained from the ternary catalytic model melt system K2S2O7-K2SO4-V2O5. By slow cooling of the melt from 420 to 355 degreesC, crystal growth...

  16. Syntheses, spectroscopic characterization, crystal structure and natural rubber vulcanization activity of new disulfides derived from sulfonyldithiocarbimates

    Science.gov (United States)

    Alves, Leandro de Carvalho; Rubinger, Mayura Marques Magalhães; Tavares, Eder do Couto; Janczak, Jan; Pacheco, Elen Beatriz Acordi Vasques; Visconte, Leila Lea Yuan; Oliveira, Marcelo Ribeiro Leite

    2013-09-01

    The compounds (Bu4N)2[(4-RC6H4SO2NCS2)2] [Bu4N = tetrabutylammonium cation; R = H (1), F (2), Cl (3) and Br (4)] and (Ph4P)2[(4-RC6H4SO2NCS2)2]ṡH2O [Ph4P = tetraphenylphosphonium cation and R = I (5)] were synthesized by the reaction of the potassium dithiocarbimates (4-RC6H4SO2NCS2K2ṡ2H2O) with I2 and Bu4NBr or Ph4PCl. The IR data were consistent with the formation of the dithiocarbimatodisulfides anions. The NMR spectra showed the expected signals for the cations and anions in a 2:1 proportion. The structures of compounds 1-5 were determined by the single crystal X-ray diffraction. The compounds 2, 3 and 4 are isostructural and crystallise in the centrosymmetric space group C2/c of the monoclinic system. Compound 1 crystallises in the monoclinic system in the space group of P21/n and the compound 5 crystallises in the centrosymmetric space group P-1 of the triclinic system. The complex anions of compounds 2, 3 and 4 exhibit similar conformations having twofold symmetry, while in 1 and 5 the anions exhibit C1 symmetry. The activity of the new compounds in the vulcanization of the natural rubber was evaluated and compared to the commercial accelerators ZDMC, TBBS and TMTD. These studies confirm that the sulfonyldithiocarbimato disulfides anions are new vulcanization accelerators, being slower than the commercial accelerators, but producing a greater degree of crosslinking, and scorch time values compatible with good processing safety for industrial applications. The mechanical properties, stress and tear resistances were determined and compared to those obtained with the commercial accelerators.

  17. Mononuclear mercury(II) complexes containing bipyridine derivatives and thiocyanate ligands: Synthesis, characterization, crystal structure determination, and luminescent properties

    Science.gov (United States)

    Amani, Vahid; Alizadeh, Robabeh; Alavije, Hanieh Soleimani; Heydari, Samira Fadaei; Abafat, Marzieh

    2017-08-01

    A series of mercury(II) complexes, [Hg(Nsbnd N)(SCN)2] (Nsbnd N is 4,4‧-dimethyl-2,2‧-bipyridine in 1, 5,5‧-dimethyl-2,2‧-bipyridine in 2, 6,6‧-dimethyl-2,2‧-bipyridine in 3 and 6-methyl-2,2‧-bipyridine in 4), were prepared from the reactions of Hg(SCN)2 with mentioned ligands in methanol. Suitable crystals of these complexes were obtained for X-ray diffraction measurement by methanol diffusion into a DMSO solution. The four complexes were thoroughly characterized by spectral methods (IR, UV-Vis, 13C{1H}NMR, 1H NMR and luminescence), elemental analysis (CHNS) and single crystal X-ray diffraction. The X-ray structural analysis indicated that in the structures of these complexes, the mercury(II) cation is four-coordinated in a distorted tetrahedral configuration by two S atoms from two thiocyanate anions and two N atoms from one chelating 2,2‧-bipyridine derivative ligand. Also, in these complexes intermolecular interactions, for example Csbnd H⋯N hydrogen bonds (in 1-4), Csbnd H⋯S hydrogen bonds (in 1, 2 and 4), π … π interactions (in 2-4), Hg⋯N interactions (in 2) and S⋯S interactions (in 4), are effective in the stabilization of the crystal structures and the formation of the 3D supramolecular complexes. Furthermore, the luminescence spectra of the title complexes show that the intensity of their emission bands are stronger than the emission bands for the free bipyridine derivative ligands.

  18. Synthesis, Crystal Structural Characterization and Biological Properties of Thiosemicarbazones of Schiff Bases Derived from 4-Acyl-2-pyrazoline-5-one

    Directory of Open Access Journals (Sweden)

    Arjunsinh Rana

    2011-01-01

    Full Text Available A novel synthesis, single crystal and biological activity of 4-acylthiosemicarbazone-3-methyl-1-(4`-methylphenyl-2-pyrazolin-5-one by condensation of 4-acyl-3-methyl-1-(4`-methylphenyl-2-pyrazolin-5-one with thiosemicarbazide was carried out. The compounds were characterized on the basis of elemental analysis, IR, 1H NMR, Mass, DSC and 13C NMR spectral data. The compounds were tested for their antibacterial activity against various gram +ve and -ve bacteria. The results were compared with the marketed drugs. The crystal structure was determined by single x-ray diffraction. 4-Acetyl thiosemicarbazone-3-methyl-1-(4`-methylphenyl-2-pyrazolin-5-one(AcPTMP-ths crystallizes in the monoclinic system, space group P21/n with a=6.0828(7Å, b=29.547(4Å, c=7.9101(15Å, α=90°, γ=95.602(15°, γ=90°, V=1414.9(4 Å3, Z=4, Dc=1.429 mg/m3 and 4-Propionylthiosemicarbazone-3-methyl-1-(4`-methylphenyl-2-pyrazolin-5-one (PropPTMP-ths crystallizes in the monoclinic system, space group P21/c with a=13.5622(10Å, b=13.3671(12Å, c=22.151(2Å, α=90°, β=93.13(7°, γ=90°, V=4010.1(6 Å3, Z=8, Dc=1.310 mg/m3. The compounds were screened for antibacterial properties and exhibited potential activity.

  19. Thorium/uranium mixed oxide nano-crystals: Synthesis, structural characterization and magnetic properties

    International Nuclear Information System (INIS)

    Hudry, Damien; Griveau, Jean-Christophe; Apostolidis, Christos; Colineau, Eric; Rasmussen, Gert; Walter, Olaf; Wang, Di; Venkata Sai Kiran Chakravadhaluna; Courtois, Eglantine; Kubel, Christian

    2014-01-01

    One of the primary aims of the actinide community within nano-science is to develop a good understanding similar to what is currently the case for stable elements. As a consequence, efficient, reliable and versatile synthesis techniques dedicated to the formation of new actinide-based nano-objects (e.g., nano-crystals) are necessary. Hence, a 'library' dedicated to the preparation of various actinide based nano-scale building blocks is currently being developed. Nano-scale building blocks with tunable sizes, shapes and compositions are of prime importance. So far, the non-aqueous synthesis method in highly coordinating organic media is the only approach which has demonstrated the capability to provide size and shape control of actinide-based nano-crystals (both for thorium and uranium, and recently extended to neptunium and plutonium). In this paper, we demonstrate that the non-aqueous approach is also well adapted to control the chemical composition of the nano-crystals obtained when mixing two different actinides. Indeed, the controlled hot co-injection of thorium acetylacetonate and uranyl acetate (together with additional capping agents) into benzyl ether can be used to synthesize thorium/uranium mixed oxide nano-crystals covering the full compositional spectrum. Additionally, we found that both size and shape are modified as a function of the thorium/uranium ratio. Finally, the magnetic properties of the different thorium/uranium mixed oxide nano-crystals were investigated. Contrary to several reports, we did not observe any ferromagnetic behavior. As a consequence, ferromagnetism cannot be described as a universal feature of nano-crystals of non-magnetic oxides as recently claimed in the literature. (authors)

  20. Optical and structural characterization of KBr crystals doped cadmium bromide (CdBr2)

    International Nuclear Information System (INIS)

    Bensouici, A.; Plaza, J.L.; Dieguez, E.; Halimi, O.; Guerbous, L.; Sebais, M.

    2010-01-01

    In this paper we demonstrate the presence of CdBr 2 and cadmium aggregates in KBr matrix during Czochralski growth of KBr crystals. The chemical decomposition of CdBr 2 due to high temperature of crystallisation and reformation of cadmium bromide seems to be responsible for this effect.

  1. Optical and structural characterization of KBr crystals doped cadmium bromide (CdBr{sub 2})

    Energy Technology Data Exchange (ETDEWEB)

    Bensouici, A., E-mail: bensouicia@yahoo.f [Laboratory of Crystallography (Saint Lucia), Department of Physics, Mentouri-Constantine University, Constantine (Algeria); Plaza, J.L., E-mail: joseluis.plaza@uam.e [Crystal Growth Laboratory (CGL), Departamento de Fisica de Materiales, Universidad Autonoma de Madrid, Madrid (Spain); Dieguez, E. [Crystal Growth Laboratory (CGL), Departamento de Fisica de Materiales, Universidad Autonoma de Madrid, Madrid (Spain); Halimi, O. [Laboratory of Crystallography (Saint Lucia), Department of Physics, Mentouri-Constantine University, Constantine (Algeria); Guerbous, L. [Centre de recherche nucleaire d' Alger (CRNA), Alger 16000 (Algeria); Sebais, M. [Laboratory of Crystallography (Saint Lucia), Department of Physics, Mentouri-Constantine University, Constantine (Algeria)

    2010-04-15

    In this paper we demonstrate the presence of CdBr{sub 2} and cadmium aggregates in KBr matrix during Czochralski growth of KBr crystals. The chemical decomposition of CdBr{sub 2} due to high temperature of crystallisation and reformation of cadmium bromide seems to be responsible for this effect.

  2. The nitro-reduced metabolite of nimesulide: Crystal structure, spectroscopic characterization, ESI-QTOF mass spectrometric analysis and antibacterial evaluation

    Science.gov (United States)

    Nunes, Julia H. B.; Nakahata, Douglas H.; Lustri, Wilton R.; Corbi, Pedro P.; de Paiva, Raphael E. F.

    2018-04-01

    Here we present a synthetic procedure, spectroscopic characterization and single-crystal X-ray structure for the nitro-reduced metabolite of the anti-inflammatory drug nimesulide, hereby referred to as NMS-NH2. The nitro-reduced metabolite was synthesized using the Béchamp reduction (iron powder under acidic media), leading to the conversion of the nitrobenzene group of nimesulide to an aniline. Mass spectrometry, infrared and nuclear magnetic resonance spectroscopies data are also provided for NMS-NH2, and discussed in comparison to nimesulide. NMS-NH2 was also evaluated in terms of its antibacterial activities, considering that the free sbnd NH2 group could allow the compound to act as a dihydropteroate synthase inhibitor. NMS-NH2 had a modest antibacterial activity against P. aeruginosa (5.0 mg mL-1), which was not observed for NMS.

  3. Synthesis, characterization and crystal structure of a 2-(diethylaminomethylindole ligated dimethylaluminium complex

    Directory of Open Access Journals (Sweden)

    Logan E. Shephard

    2015-10-01

    Full Text Available The title compound, [Al(CH32(C13H17N2] (systematic name; {2-[(diethylaminomethyl]indol-1-yl-κ2N,N′}dimethylaluminium, was prepared by methane elimination from the reaction of 2-(diethylaminomethylindole and trimethylaluminium. The complex crystallizes readily from a concentrated toluene solution in high yield. The asymmetric unit contains two crystallographically independent molecules. Each molecule has a four-coordinate aluminium atom that has pseudo-tetrahedral geometry. C—H...π interactions link the independent molecules into chains extending along the b-axis direction.

  4. Solid state characterization and crystal structure from X-ray powder diffraction of two polymorphic forms of ranitidine base.

    Science.gov (United States)

    de Armas, Héctor Novoa; Peeters, Oswald M; Blaton, Norbert; Van Gyseghem, Elke; Martens, Johan; Van Haele, Gerrit; Van Den Mooter, Guy

    2009-01-01

    Ranitidine hydrochloride (RAN-HCl), a known anti-ulcer drug, is the product of reaction between HCl and ranitidine base (RAN-B). RAN-HCl has been extensively studied; however this is not the case of the RAN-B. The solid state characterization of RAN-B polymorphs has been carried out using different analytical techniques (microscopy, thermal analysis, Fourier transform infrared spectrometry in the attenuated total reflection mode, (13)C-CPMAS-NMR spectroscopy and X-ray powder diffraction). The crystal structures of RAN-B form I and form II have been determined using conventional X-ray powder diffraction in combination with simulated annealing and whole profile pattern matching, and refined using rigid-body Rietveld refinement. RAN-B form I is a monoclinic polymorph with cell parameters: a = 7.317(2), b = 9.021(2), c = 25.098(6) A, beta = 95.690(1) degrees and space group P2(1)/c. The form II is orthorhombic: a = 31.252(4), b = 13.052(2), c = 8.0892(11) A with space group Pbca. In RAN-B polymorphs, the nitro group is involved in a strong intramolecular hydrogen bond responsible for the existence of a Z configuration in the enamine portion of the molecules. A tail to tail packing motif can be denoted via intermolecular hydrogen bonds. The crystal structures of RAN-B forms are compared to those of RAN-HCl polymorphs. RAN-B polymorphs are monotropic polymorphic pairs. (c) 2008 Wiley-Liss, Inc. and the American Pharmacists Association

  5. Syntheses, characterizations and crystal structures of three new organically templated or organically bonded zinc selenates

    International Nuclear Information System (INIS)

    Feng Meiling; Mao Jianggao; Song Junling

    2004-01-01

    Three new organically templated or organically bonded zinc selenates, namely, {H 2 bipy}Zn(SeO 4 ) 2 (H 2 O) 2 1 (bipy=4,4'-bipyridine), {H 2 pip}{Zn(SeO 4 ) 2 (H 2 O) 4 }·2H 2 O 2 (pip=piprazine), and Zn(SeO 4 )(phen)(H 2 O) 2 3 (phen=1,10-phenanthroline) have been synthesized by hydrothermal reactions. The structure of compound 1 features a 1D chain composed of [Zn(SeO 4 ) 2 (H 2 O) 2 ] 2- anions. Compound 2 has a 2D layer structure built from {Zn(SeO 4 ) 2 (H 2 O) 4 } 2- anions that are cross-linked by doubly protonated piperazine cations via N-H···O hydrogen bonds. The structure of compound 3 contains a 1D chain of Zn(SeO 4 )(phen)(H 2 O) 2 , such chains are further interlinked by hydrogen bonds and π···π interactions to form a layer. The different roles the templates played have also been discussed

  6. Phenotype characterization of embryoid body structures generated by a crystal comet effect tail in an intercellular cancer collision scenario

    Directory of Open Access Journals (Sweden)

    Diaz JA

    2012-01-01

    Full Text Available Jairo A Diaz, Mauricio F MurilloDepartment of Pathology, Hospital Departmental Villavicencio, Hospital Departmental Granada, Medicine School, University Cooperative of Colombia, Villavicencio, Meta, ColombiaAbstract: Cancer is, by definition, the uncontrolled growth of autonomous cells that eventually destroy adjacent tissues and generate architectural disorder. However, this concept cannot be totally true. In three well documented studies, we have demonstrated that cancer tissues produce order zones that evolve over time and generate embryoid body structures in a space-time interval. The authors decided to revise the macroscopic and microscopic material in well-developed malignant tumors in which embryoid bodies were identified to determine the phenotype characterization that serves as a guideline for easy recognition. The factors responsible for this morphogenesis are physical, bioelectric, and magnetic susceptibilities produced by crystals that act as molecular designers for the topographic gradients that guide the surrounding silhouette and establish tissue head-tail positional identities. The structures are located in amniotic-like cavities and show characteristic somite-like embryologic segmentation. Immunophenotypic study has demonstrated exclusion factor positional identity in relation to enolase-immunopositive expression of embryoid body and human chorionic gonadotropin immunopositivity exclusion factor expression in the surrounding tissues. The significance of these observations is that they can also be predicted by experimental image data collected by the Large Hadron Collider (LHC accelerator at the European Organization for Nuclear Research, in which two-beam subatomic collision particles in the resulting debris show hyperorder domains similar to those identified by us in intercellular cancer collisions. Our findings suggest that we are dealing with true reverse biologic system information in an activated collective cancer stem cell

  7. Functional characterization and crystal structure of thermostable amylase from Thermotoga petrophila, reveals high thermostability and an unusual form of dimerization

    DEFF Research Database (Denmark)

    Hameed, Uzma; Price, Ian; Ikram-Ul-Haq

    2017-01-01

    and able to hydrolyze starch into dextrin between 90 and 100°C, with optimum activity at 98°C and pH8.5. The activity increased in the presence of Rb(1+), K(1+) and Ca(2+) ions, whereas other ions inhibited activity. The crystal structure of Tp-AmyS at 1.7Å resolution showed common features of the GH-13...... of salivary amylase from a previous crystal structure, and thus could be a functional feature of some amylases....

  8. Tungsten disilicide (WSi{sub 2}). Synthesis, characterization, and prediction of new crystal structures

    Energy Technology Data Exchange (ETDEWEB)

    Lukovic, Jelena; Zagorac, Dejan; Zagorac, Jelena; Jordanov, Dragana; Matovic, Branko [Institute of Nuclear Sciences Vinca, Materials Science Laboratory, University of Belgrade (Serbia); Materials Science Laboratory, Center for the Synthesis, Processing and Characterization of Materials for Use in Extreme Conditions, Belgrade (Serbia); Schoen, J. Christian [Materials Science Laboratory, Max Planck Institute for Solid State Research, Stuttgart (Germany); Volkov-Husovic, Tatjana [Faculty of Technology and Metallurgy, Department for Metallurgical Engineering, University of Belgrade (Serbia)

    2017-12-13

    Transition metal silicides have attracted great attention due to their potential applications in microelectronics, ceramics, and the aerospace industry. In this study, experimental and theoretical investigations of tungsten based silicides were performed. Tungsten disilicide (WSi{sub 2}) was synthesized by simple thermal treatment at 1350 C for 4 h in an argon atmosphere. These optimal synthesis conditions were obtained by variation of temperatures and times of heating, and the structure of the final synthesized compound was determined by XRPD analysis. In addition, new modifications for WSi{sub 2} were proposed and investigated using first-principles calculations within density-functional theory (DFT). Both LDA and PBE calculations show excellent agreement with experimental observations and previous calculations for the existing modifications, where available. (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  9. Synthesis, crystal structure and magnetic characterization of a cyanide-bridged Mo-Ni nanosized molecular wheel

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Daopeng; Zhang, Hongyan; Wang, Ping [Shandong Univ. of Technology, College of Chemical Engineering, Zibo (China); Kong, Lingqian [Liaocheng Univ. (China). Dongchang College

    2015-11-01

    By using K{sub 4}[Mo(CN){sub 8}] and [Ni(L)(H{sub 2}O){sub 2}][ClO{sub 4}]{sub 2} as reagents (L = 2,12-dimethyl-3,7,11,17-tetraazabicyclo [11.3.1]heptadeca-1(17),13,15-triene), a new cyanide-bridged Mo-Ni complex containing the building blocks [Ni(H{sub 2}O)(L)]{sup 2+} and [Ni(L)]{sup 2+} bridged by [Mo(CN){sub 8}]{sup 4-} units has been obtained. The complex with the formula {[Ni(H_2O)(L)][Ni(L)][Mo(CN)_8]}{sub 6} . 36H{sub 2}O . 2CH{sub 3}OH (1) was characterized by elemental analysis, IR spectroscopy and single-crystal X-ray diffraction. The structure determination reveals an octadecanuclear cluster in the form of a 36-membered macrocycle, in which the largest intramolecular W..W and Ni..Ni distances are 16.5 and 14.4 Aa, respectively, indicating that complex 1 is a nanosized molecular wheel. Investigation of its magnetic properties has shown weak antiferromagnetic coupling between the adjacent Ni(II) ions bridged by the diamagnetic [Mo(CN){sub 8}]{sup 4-} ions.

  10. Preparation and structural characterization of FeCo epitaxial thin films on insulating single-crystal substrates

    International Nuclear Information System (INIS)

    Nishiyama, Tsutomu; Ohtake, Mitsuru; Futamoto, Masaaki; Kirino, Fumiyoshi

    2010-01-01

    FeCo epitaxial films were prepared on MgO(111), SrTiO 3 (111), and Al 2 O 3 (0001) single-crystal substrates by ultrahigh vacuum molecular beam epitaxy. The effects of insulating substrate material on the film growth process and the structures were investigated. FeCo(110) bcc films grow on MgO substrates with two type domains, Nishiyama-Wassermann (NW) and Kurdjumov-Sachs (KS) relationships. On the contrary, FeCo films grown on SrTiO 3 and Al 2 O 3 substrates include FeCo(111) bcc crystal in addition to the FeCo(110) bcc crystals with NW and KS relationships. The FeCo(111) bcc crystal consists of two type domains whose orientations are rotated around the film normal by 180 deg. each other. The out-of-plane and the in-plane lattice spacings of FeCo(110) bcc and FeCo(111) bcc crystals formed on the insulating substrates are in agreement with those of the bulk Fe 50 Co 50 (at. %) crystal with small errors ranging between +0.2% and +0.4%, showing that the strains in the epitaxial films are very small.

  11. Synthesis, characterization, crystal structure and theoretical studies of new chiral Schiff base (E)-4-hydroxy[(1-phenylethyl)iminomethyl]benzyne

    Czech Academy of Sciences Publication Activity Database

    Khalaji, A.D.; Gholinejad, M.; Rad, S.M.; Grivani, G.; Fejfarová, Karla; Dušek, Michal

    2015-01-01

    Roč. 41, č. 3 (2015), 1635-1645 ISSN 0922-6168 R&D Projects: GA ČR(CZ) GC202/07/J007 Institutional support: RVO:68378271 Keywords : Schiff base * crystal structure * DFT calculation Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.833, year: 2015

  12. Synthesis, growth, morphology of the semiorganic nonlinear optical crystal L-glutamic acid hydrochloride and its structural, thermal and SHG characterizations

    Energy Technology Data Exchange (ETDEWEB)

    Dhanasekaran, P.; Srinivasan, K. [Crystal Growth Laboratory, Department of Physics, School of Physical Sciences, Bharathiar University, Coimbatore-641 046, Tamil Nadu (India)

    2012-12-15

    One of the halide derivatives of L-glutamic acid which was identified as a semiorganic nonlinear optical material, L-glutamic acid hydrochloride [HOOC(CH{sub 2}){sub 2}CH(NH{sub 2})COOH.HCl], was grown as bulk single crystal and its significant properties were characterized. The stoichiometric title compound was synthesized and the solubility of its recrystallized form in DD water was determined in the temperature range 30-80 C by gravimetric method. Structural confirmation was carried out by powder X-ray diffraction study through lattice parameter verification. Optical quality smaller dimension single crystals were grown from aqueous solution by self nucleation through slow evaporation of solvent method and a large dimension single crystal was grown by slow cooling method with reversible seed rotation technique. Morphological importances of different growth facets of the as grown crystals were studied through optical goniometry. Unit cell structure of the grown crystal was refined by single crystal X-ray diffraction analysis, functional groups present in the crystal responsible for various modes of vibrations were confirmed by FTIR spectroscopy analysis, thermal stability of the grown crystal was analysed by TG/DTA and DSC and second harmonic generation (SHG) of a fundamental Nd:YAG laser beam by Kurtz technique. Results indicate that the grown crystal is in stoichiometric composition and has significant improvement in its thermal and SHG properties when compared to pure L-glutamic acid polymorphs. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  13. Growth and Characterization of Tetraphenylphosphonium Bromide Crystal

    Directory of Open Access Journals (Sweden)

    Guangqiang Wang

    2017-05-01

    Full Text Available Multiple-phenyl phosphorous compounds are a group of chemical materials that have been used as reactants, pharmaceutical intermediates, extractants, and catalysts in organic synthetic reactions. However, the crystal growth of bulk crystals of multiple-phenyl phosphorous compounds, which may expand their applications in photonics technology, have been largely overlooked. In this article, the crystal growth of tetraphenylphosphonium bromide (TPPB has been studied in organic solvents and water. The crystal structures and crystallization features are analyzed by X-ray diffraction data. By a slow temperature-lowering method, a single-crystal of TPPB (2H2O with the size of 27 × 20 × 20 mm3 has been obtained in water. The basic thermal and optical properties were characterized. We find that the TPPB (2H2O crystal shows excellent transparent property in the near-IR region. Large Raman shifts and strong Raman scattering intensity indicate that TPPB is a potential candidate in Raman-scattering-based nonlinearity applications.

  14. Structural and biophysical characterization of an epitope-specific engineered Fab fragment and complexation with membrane proteins: implications for co-crystallization.

    Science.gov (United States)

    Johnson, Jennifer L; Entzminger, Kevin C; Hyun, Jeongmin; Kalyoncu, Sibel; Heaner, David P; Morales, Ivan A; Sheppard, Aly; Gumbart, James C; Maynard, Jennifer A; Lieberman, Raquel L

    2015-04-01

    Crystallization chaperones are attracting increasing interest as a route to crystal growth and structure elucidation of difficult targets such as membrane proteins. While strategies to date have typically employed protein-specific chaperones, a peptide-specific chaperone to crystallize multiple cognate peptide epitope-containing client proteins is envisioned. This would eliminate the target-specific chaperone-production step and streamline the co-crystallization process. Previously, protein engineering and directed evolution were used to generate a single-chain variable (scFv) antibody fragment with affinity for the peptide sequence EYMPME (scFv/EE). This report details the conversion of scFv/EE to an anti-EE Fab format (Fab/EE) followed by its biophysical characterization. The addition of constant chains increased the overall stability and had a negligible impact on the antigen affinity. The 2.0 Å resolution crystal structure of Fab/EE reveals contacts with larger surface areas than those of scFv/EE. Surface plasmon resonance, an enzyme-linked immunosorbent assay, and size-exclusion chromatography were used to assess Fab/EE binding to EE-tagged soluble and membrane test proteins: namely, the β-barrel outer membrane protein intimin and α-helical A2a G protein-coupled receptor (A2aR). Molecular-dynamics simulation of the intimin constructs with and without Fab/EE provides insight into the energetic complexities of the co-crystallization approach.

  15. Structural, physicochemical characterization and antimicrobial ...

    Indian Academy of Sciences (India)

    Structural, physicochemical characterization and antimicrobial activities of a new Tetraaqua ... Antimicrobial activity of 1 was tested. ... was prepared as good quality yellow single crystals .... at 540 nm. Increase of OD was compared to control.

  16. Synthesis, characterization and crystal structure of (2RS,4R)-2-(2-hydroxy-3-methoxyphenyl)thiazolidine-4-carboxylic acid

    Science.gov (United States)

    Muche, Simon; Müller, Matthias; Hołyńska, Małgorzata

    2018-03-01

    The condensation reaction of ortho-vanillin and L-cysteine leads to formation of a racemic mixture of (2RS,4R)-2-(2-hydroxy-3-methoxyphenyl)thiazolidine-4-carboxylic acid and not, as reported in the available literature, to a Schiff base. The racemic mixture was fully characterized by 1D and 2D NMR techniques, ESI-MS and X-ray diffraction. Addition of ZnCl2 led to formation of crystals in form of colorless needles, suitable for X-ray diffraction studies. The measured crystals were identified as the diastereomer (2R,4R)-2-(2-hydroxy-3-methoxyphenyl)thiazolidine-4-carboxylic acid 1. The bulk material is racemic. Thiazolidine exists as zwitterion in solid state, as indicated by the crystal structure.

  17. Structural characterization of metastable hcp-Ni thin films epitaxially grown on Au(100) single-crystal underlayers

    International Nuclear Information System (INIS)

    Ohtake, Mitsuru; Tanaka, Takahiro; Futamoto, Masaaki; Kirino, Fumiyoshi

    2010-01-01

    Ni(1120) epitaxial thin films with hcp structure were prepared on Au(100) single-crystal underlayers at 100 deg. C by ultra high vacuum molecular beam epitaxy. The detailed film structure is studied by in situ reflection high energy electron diffraction, x-ray diffraction, and transmission electron microscopy. The hcp-Ni film consists of two types of variants whose c-axes are rotated around the film normal by 90 deg. each other. An atomically sharp boundary is recognized between the film and the underlayer, where misfit dislocations are introduced. Presence of such dislocations seems to relieve the strain caused by the lattice mismatch between the film and the underlayer.

  18. Characterization of a defective PbWO4 crystal cut along the a-c crystallographic plane: structural assessment and a novel photoelastic stress analysis

    Science.gov (United States)

    Montalto, L.; Natali, P. P.; Daví, F.; Mengucci., P.; Paone, N.; Rinaldi, D.

    2017-12-01

    Among scintillators, the PWO is one of the most widely used, for instance in CMS calorimeter at CERN and PANDA project. Crystallographic structure and chemical composition as well as residual stress condition, are indicators of homogeneity and good quality of the crystal. In this paper, structural characterization of a defective PbWO4 (PWO) crystal has been performed by X-ray Diffraction (XRD), Energy Dispersive Spectroscopy (EDS) and Photoelasticity in the unusual (a, c) crystallographic plane. XRD and EDS analysis have been used to investigate crystallographic orientation and chemical composition, while stress distribution, which indicates macroscopic inhomogeneities and defects, has been obtained by photoelastic approaches, in Conoscopic and Sphenoscopic configuration. Since the sample is cut along the (a, c) crystallographic plane, a new method is proposed for the interpretation of the fringe pattern. The structural analysis has detected odds from the nominal lattice dimension, which can be attributed to the strong presence of Pb and W. A strong inhomogeneity over the crystal sample has been revealed by the photoelastic inspection. The results give reliability to the proposed procedure which is exploitable in crystals with other structures.

  19. Cultivation and characterization of GaInSe2 crystals

    International Nuclear Information System (INIS)

    Panakhov, T.M.; Kafarova, D.M.

    2013-01-01

    This work is the first systematic study devoted to the growth of GaInSe 2 crystals and their characterization by experimental methods such as X-ray diffraction, electron microscopy transmission with high resolution, sample electron diffraction. By the method of photoelectron roentgen spectroscopy it was studied the chemical structure of the GaInSe 2 crystals and the microprobe analysis indicated that the individual crystals have an excess of gallium. GaInSe 2 crystals were grown by the Bridgman method. Samples were prepared as single crystals by the Bridgman method. Studies showed that the GaInSe 2 crystals are hexagonal ones

  20. Structural and compositional characterization of LiNbO{sub 3} crystals implanted with high energy iron ions

    Energy Technology Data Exchange (ETDEWEB)

    Sada, C., E-mail: cinzia.sada@unipd.i [Universita di Padova and CNISM, Dipartimento di Fisica, Via Marzolo 8, 35131 Padova (Italy); Argiolas, N.; Bazzan, M.; Ciampolillo, M.V.; Zaltron, A.M.; Mazzoldi, P. [Universita di Padova and CNISM, Dipartimento di Fisica, Via Marzolo 8, 35131 Padova (Italy); Agarwal, D.C.; Avastshi, D.K. [Inter-University Accelerator Centre, Post Box-10502, New Delhi 110067 (India)

    2010-10-01

    Iron ions were implanted with a total fluence of 6 x 10{sup 17} ions/m{sup 2} into lithium niobate crystals by way of a sequential implantation at different energies of 95, 100 and 105 MeV respectively through an energy retarder Fe foil to get a uniform Fe doping of about few microns from the surface. The implanted crystals were then annealed in air in the range 200-400 {sup o}C for different durations to promote the crystalline quality that was damaged by implantation. In order to understand the basic phenomena underlying the implantation process, compositional in-depth profiles obtained by the secondary ion mass spectrometry were correlated to the structural properties of the implanted region measured by the high resolution X-ray diffraction depending on the process parameters. The optimised preparation conditions are outlined in order to recover the crystalline quality, essential for integrated photorefractive applications.

  1. 5-Arylidene derivatives of Meldrum's acid: Synthesis, structural characterization using single crystal and powder crystal X-ray diffraction, and electronic properties

    Science.gov (United States)

    Dey, Tanusri; Ghosh, Soumen; Ghosh, Somnath; Mukherjee, Alok Kumar

    2015-07-01

    Four 5-arylidene derivatives of Meldrum's acid, 5-(4-chlorobenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (2), 5-(3-hydroxybenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (3), 5-(3,4-dimethoxybenzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (4) and 5-(2,4-dimethoxy benzylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione (5) have been synthesized and their crystal structures have been determined using single crystal X-ray diffractometry for 2, 4 and 5 and X-ray powder diffraction for 3. The nature of intermolecular interactions in 2-5 has been analyzed through Hirshfeld surfaces and 2D fingerprint plots. The DFT optimized molecular geometries in 2-5 agree closely with those obtained from the crystallographic studies. The crystal packing in 2-5 exhibits an interplay of Osbnd H⋯O, Csbnd H⋯O, Csbnd H⋯Cl and Csbnd H⋯π (arene) hydrogen bonds and π⋯π interactions, which assemble molecules into three-dimensional architecture in 2, 3 and 5 and two-dimensional framework in 4. The Hirshfeld surface analyses of 2-5, Meldrum's acid (1) and a few related 5-arylidene derivatives of Meldrum's acid retrieved from the Cambridge Structural Database (CSD) indicate that about 85% of the Hirshfeld surface area (72% in 2 where H⋯Cl contribution is about 13%) in this class of compounds are due to H⋯H, O⋯H and C⋯H contacts. The HOMO-LUMO energy gap (>2.2 eV) in 2-5 indicates a significant degree of internal charge transfer within the molecule.

  2. Synthesis, characterization, crystal structures and DFT studies of some new 1,2,4-triazole and triazolidin derivatives

    Science.gov (United States)

    Abosadiya, Hamza M.; Anouar, El Hassane; Abusaadiya, Salima M.; Hasbullah, Siti Aishah; Yamin, Bohari M.

    2018-01-01

    A simple efficient method for synthesis of some new 1,2,4-Triazole and Triazolidin derivatives namely, 5-(4-methoxyphenyl)-2-phenyl-2,4-dihydro-3H-1,2,4-triazole-3-thione (1a), (2-chlorophenyl)(3,3-dimethyl-1-phenyl-5-thioxo-1,2,4-triazolidin-4-yl)methanone (1b) and (2-iodophenyl)(3,3-dimethyl-1-phenyl-5-thioxo-1,2,4-triazolidin-4-yl)methanone (1c) have been synthesized in high yields from the reaction of carbonoyl isothiocyanate with phenyl hydrazine. The final products were characterized by FT-IR, 1H and 13C NMR spectroscopic techniques. X-ray crystallographic studies showed that 1a crystallized in triclinic crystal system with space group Pī, while both 1b and 1c crystallized in orthorhombic crystal system with space group Pna21. The asymmetric unit of 1a consists two crystallographically independent molecules, while only one molecule in asymmetric unit for both 1b and 1c compounds. All molecules possess Csbnd H ….S intramolecular hydrogen bonds which formed a pseudo-six-membered ring. Experimental results have been confirmed by the state-of-art density functional theory (DFT) in gas and solvent phase by using five different hybrid functionals B3LYP, B3P86, CAM-B3LYP, M06-2X and PBE0 combined with 6-311++G(d, p) basis set. The experimental data are relatively well produced, and relatively good correlations are obtained between the predicted and experimental data.

  3. Synthesis, structure, growth and characterization of a novel organic NLO single crystal: Morpholin-4-ium p-aminobenzoate

    Energy Technology Data Exchange (ETDEWEB)

    Shanmugam, G. [Department of Physics, Anna University of Technology Tiruchirappalli, Tiruchirappalli 620024 (India); Ravi Kumar, K.; Sridhar, B. [X-ray Crystallography Division, Indian Institute of Chemical Technology, CSIR, Hyderabad 500007 (India); Brahadeeswaran, S., E-mail: sbrag67@yahoo.com [Department of Physics, Anna University of Technology Tiruchirappalli, Tiruchirappalli 620024 (India)

    2012-09-15

    Highlights: ► A new organic NLO crystal morpholin-4-ium p-aminobenzoate has been grown for the first time. ► The structure is reported for the first time in the literature. ► Thermal, optical and SHG studies suggest its suitability for various NLO applications. -- Abstract: The title compound, morpholin-4-ium p-aminobenzoate (MPABA)(C{sub 4}H{sub 10}NO{sup +},C{sub 7}H{sub 6}NO{sub 2}{sup −}), has been synthesized for the first time by the addition of morpholine with 4-aminobenzoic acid in equi-molar ratio and good quality single crystals have been grown by solution growth technique using methanol as a solvent. The molecular structure of the compound was solved and refined by Direct Methods using SHELXS97 and full-matrix least-squares technique using SHELXL97, respectively. MPABA crystallizes in a monoclinic system with unit cell parameters, a = 5.948(5) Å, b = 18.033(4) Å, c = 10.577(5) Å, β = 90.40(1)° and non-centrosymmetric space group Cc. The experimentally measured density and chemical compositions were found to be in good agreement with the theoretical values. The phases and functional groups of MPABA have been identified and confirmed through powder X-ray diffraction and Fourier transform infrared (FTIR) studies, respectively. The thermal stability and decomposition details were studied through TG/DTA thermograms. The UV–visible transmission spectra were recorded for the grown crystal and its NLO characteristic was explored by powder second harmonic generation (SHG) studies.

  4. Synthesis, structure, growth and characterization of a novel organic NLO single crystal: Morpholin-4-ium p-aminobenzoate

    International Nuclear Information System (INIS)

    Shanmugam, G.; Ravi Kumar, K.; Sridhar, B.; Brahadeeswaran, S.

    2012-01-01

    Highlights: ► A new organic NLO crystal morpholin-4-ium p-aminobenzoate has been grown for the first time. ► The structure is reported for the first time in the literature. ► Thermal, optical and SHG studies suggest its suitability for various NLO applications. -- Abstract: The title compound, morpholin-4-ium p-aminobenzoate (MPABA)(C 4 H 10 NO + ,C 7 H 6 NO 2 − ), has been synthesized for the first time by the addition of morpholine with 4-aminobenzoic acid in equi-molar ratio and good quality single crystals have been grown by solution growth technique using methanol as a solvent. The molecular structure of the compound was solved and refined by Direct Methods using SHELXS97 and full-matrix least-squares technique using SHELXL97, respectively. MPABA crystallizes in a monoclinic system with unit cell parameters, a = 5.948(5) Å, b = 18.033(4) Å, c = 10.577(5) Å, β = 90.40(1)° and non-centrosymmetric space group Cc. The experimentally measured density and chemical compositions were found to be in good agreement with the theoretical values. The phases and functional groups of MPABA have been identified and confirmed through powder X-ray diffraction and Fourier transform infrared (FTIR) studies, respectively. The thermal stability and decomposition details were studied through TG/DTA thermograms. The UV–visible transmission spectra were recorded for the grown crystal and its NLO characteristic was explored by powder second harmonic generation (SHG) studies.

  5. Crystal structure and characterization of the novel NH+⋯N hydrogen bonded polar crystal [NH2(CH2)4NH][BF4

    Science.gov (United States)

    Wojtaś, M.; Gaģor, A.; Czupiński, O.; Medycki, W.; Jakubas, R.

    2012-03-01

    Dielectric properties and phase transitions of the piperazinium tetrafluoroborate ([NH2(CH2)4NH][BF4], abbreviated as PFB) crystal are related to the one-dimensional arrangement of the cations linked by the bistable NH+⋯N hydrogen bonds and molecular motions of the [BF4]- units. The crystal structure of [NH2(CH2)4NH][BF4] is monoclinic at room temperature with the polar space group Pn. The polar/acentric properties of the room temperature phase IV have been confirmed by the piezoelectric and pyroelectric measurements. DSC measurements show that the compound undergoes three first-order structural phase transitions: at 421/411 K (heating/cooling), at 386/372 K and at 364/349 K. 1H and 19F NMR measurements indicate the reorientational motions of [BF4]- anions and piperazinium(+) cations as well as the proton motion in the hydrogen-bonded chains of piperazine along the [001] direction. Over the phase I the isotropic reorientational motions or even self-diffusion of the cations and anions are expected. The conductivity measurements in the vicinity of the II-I PT indicate a superionic phase over the phase I.

  6. Magnetic and optical holonomic manipulation of colloids, structures and topological defects in liquid crystals for characterization of mesoscale self-assembly and dynamics

    Science.gov (United States)

    Varney, Michael C. M.

    Colloidal systems find important applications ranging from fabrication of photonic crystals to direct probing of phenomena encountered in atomic crystals and glasses; topics of great interest for physicists exploring a broad range of scientific, industrial and biomedical fields. The ability to accurately control particles of mesoscale size in various liquid host media is usually accomplished through optical trapping methods, which suffer limitations intrinsic to trap laser intensity and force generation. Other limitations are due to colloid properties, such as optical absorptivity, and host properties, such as viscosity, opacity and structure. Therefore, alternative and/or novel methods of colloidal manipulation are of utmost importance in order to advance the state of the art in technical applications and fundamental science. In this thesis, I demonstrate a magnetic-optical holonomic control system to manipulate magnetic and optical colloids in liquid crystals and show that the elastic structure inherent to nematic and cholesteric liquid crystals may be used to assist in tweezing of particles in a manner impossible in other media. Furthermore, I demonstrate the utility of this manipulation in characterizing the structure and microrheology of liquid crystals, and elucidating the energetics and dynamics of colloids interacting with these structures. I also demonstrate the utility of liquid crystal systems as a table top model system to probe topological defects in a manner that may lead to insights into topologically related phenomena in other fields, such as early universe cosmology, sub-atomic and high energy systems, or Skrymionic structures. I explore the interaction of colloid surface anchoring with the structure inherent in cholesteric liquid crystals, and how this affects the periodic dynamics and localization metastability of spherical colloids undergoing a "falling" motion within the sample. These so called "metastable states" cause colloidal dynamics to

  7. Crystal structure determination of Efavirenz

    International Nuclear Information System (INIS)

    Popeneciu, Horea; Dumitru, Ristoiu; Tripon, Carmen; Borodi, Gheorghe; Pop, Mihaela Maria

    2015-01-01

    Needle-shaped single crystals of the title compound, C 14 H 9 ClF 3 NO 2 , were obtained from a co-crystallization experiment of Efavirenz with maleic acid in a (1:1) ratio, using methanol as solvent. Crystal structure determination at room temperature revealed a significant anisotropy of the lattice expansion compared to the previously reported low-temperature structure. In both low- and room temperature structures the cyclopropylethynyl fragment in one of the asymmetric unit molecules is disordered. While at low-temperature only one C atom exhibits positional disorder, at room temperature the disorder is present for two C atoms of the cyclopropane ring

  8. Introduction to crystal growth and characterization

    CERN Document Server

    Benz, Klaus-Werner

    2014-01-01

    This new textbook provides for the first time a comprehensive treatment of the basics of contemporary crystallography and crystal growth in a single volume. The reader will be familiarized with the concepts for the description of morphological and structural symmetry of crystals. The architecture of crystal structures of selected inorganic and molecular crystals is illustrated. The main crystallographic databases as data sources of crystal structures are described. Nucleation processes, their kinetics and main growth mechanism will be introduced in fundamentals of crystal growth. Some phase d

  9. Structural and electronic characterization of 355 nm laser-crystallized silicon: Interplay of film thickness and laser fluence

    International Nuclear Information System (INIS)

    Semler, Matthew R.; Swenson, Orven F.; Hoey, Justin M.; Guruvenket, Srinivasan; Gette, Cody R.; Hobbie, Erik K.

    2014-01-01

    We present a detailed study of the laser crystallization of amorphous silicon thin films as a function of laser fluence and film thickness. Silicon films grown through plasma-enhanced chemical vapor deposition were subjected to a Q-switched, diode-pumped solid-state laser operating at 355 nm. The crystallinity, morphology, and optical and electronic properties of the films are characterized through transmission and reflectance spectroscopy, resistivity measurements, Raman spectroscopy, X-ray diffraction, atomic force microscopy, and optical and scanning-electron microscopy. Our results reveal a unique surface morphology that strongly couples to the electronic characteristics of the films, with a minimum laser fluence at which the film properties are optimized. A simple scaling model is used to relate film morphology to conductivity in the laser-processed films

  10. Chromium(III) Complex Obtained from Dipicolinic Acid: Synthesis, Characterization, X-Ray Crystal Structure and Electrochemical Studies

    Energy Technology Data Exchange (ETDEWEB)

    Ghasemi, Khaled; Rezvani, Ali Reza; Ghasemi, Fatemeh [Univ. of Sistan and Baluchestan, Zahedan (Iran, Islamic Republic of); Razak, Ibrahim Abdul; Rosli, Mohd Mustaqim [Universiti Sains Malaysia, Penang (Malaysia)

    2013-10-15

    The synthesis, X-ray crystallography, spectroscopic (IR, UV-vis), and electrochemical properties of the title compound, [H{sub 3}O][Cr(dipic){sub 2}] [H{sub 3}O{sup +}.Cl{sup -}] (1), (H{sub 2}dipic = 2,6-pyridinedicarboxylic acid), are reported. This complex crystallizes in the monoclinic space group Cc with a = 14.9006(10) A, b = 12.2114(8) A, c = 8.6337(6) A, α = 90.00 .deg., β = 92.7460(10) .deg., γ = 90.00 .deg., and V = 1569.16(18) A3 with Z = 4. The hydrogen bonding and noncovalent interactions play roles in the stabilization of the structure. In order to gain a better understanding of the most important geometrical parameters in the structure of the complex, atoms in molecules (AIM) method at B3LYP/6-31G level of theory has been employed.

  11. Prediction of molecular crystal structures

    International Nuclear Information System (INIS)

    Beyer, Theresa

    2001-01-01

    The ab initio prediction of molecular crystal structures is a scientific challenge. Reliability of first-principle prediction calculations would show a fundamental understanding of crystallisation. Crystal structure prediction is also of considerable practical importance as different crystalline arrangements of the same molecule in the solid state (polymorphs)are likely to have different physical properties. A method of crystal structure prediction based on lattice energy minimisation has been developed in this work. The choice of the intermolecular potential and of the molecular model is crucial for the results of such studies and both of these criteria have been investigated. An empirical atom-atom repulsion-dispersion potential for carboxylic acids has been derived and applied in a crystal structure prediction study of formic, benzoic and the polymorphic system of tetrolic acid. As many experimental crystal structure determinations at different temperatures are available for the polymorphic system of paracetamol (acetaminophen), the influence of the variations of the molecular model on the crystal structure lattice energy minima, has also been studied. The general problem of prediction methods based on the assumption that the experimental thermodynamically stable polymorph corresponds to the global lattice energy minimum, is that more hypothetical low lattice energy structures are found within a few kJ mol -1 of the global minimum than are likely to be experimentally observed polymorphs. This is illustrated by the results for molecule I, 3-oxabicyclo(3.2.0)hepta-1,4-diene, studied for the first international blindtest for small organic crystal structures organised by the Cambridge Crystallographic Data Centre (CCDC) in May 1999. To reduce the number of predicted polymorphs, additional factors to thermodynamic criteria have to be considered. Therefore the elastic constants and vapour growth morphologies have been calculated for the lowest lattice energy

  12. Prediction of molecular crystal structures

    Energy Technology Data Exchange (ETDEWEB)

    Beyer, Theresa

    2001-07-01

    The ab initio prediction of molecular crystal structures is a scientific challenge. Reliability of first-principle prediction calculations would show a fundamental understanding of crystallisation. Crystal structure prediction is also of considerable practical importance as different crystalline arrangements of the same molecule in the solid state (polymorphs)are likely to have different physical properties. A method of crystal structure prediction based on lattice energy minimisation has been developed in this work. The choice of the intermolecular potential and of the molecular model is crucial for the results of such studies and both of these criteria have been investigated. An empirical atom-atom repulsion-dispersion potential for carboxylic acids has been derived and applied in a crystal structure prediction study of formic, benzoic and the polymorphic system of tetrolic acid. As many experimental crystal structure determinations at different temperatures are available for the polymorphic system of paracetamol (acetaminophen), the influence of the variations of the molecular model on the crystal structure lattice energy minima, has also been studied. The general problem of prediction methods based on the assumption that the experimental thermodynamically stable polymorph corresponds to the global lattice energy minimum, is that more hypothetical low lattice energy structures are found within a few kJ mol{sup -1} of the global minimum than are likely to be experimentally observed polymorphs. This is illustrated by the results for molecule I, 3-oxabicyclo(3.2.0)hepta-1,4-diene, studied for the first international blindtest for small organic crystal structures organised by the Cambridge Crystallographic Data Centre (CCDC) in May 1999. To reduce the number of predicted polymorphs, additional factors to thermodynamic criteria have to be considered. Therefore the elastic constants and vapour growth morphologies have been calculated for the lowest lattice energy

  13. The Crystal Structure of a High-Spin Oxoiron(IV) Complex and Characterization of Its Self-Decay Pathway

    Energy Technology Data Exchange (ETDEWEB)

    England, J.; Guo, Y; Farquhar, E; Young, Jr., V; Münck, E; Que, Jr., L

    2010-01-01

    [Fe{sup IV}(O)(TMG{sub 3}tren)]{sup 2+} (1; TMG{sub 3}tren = 1,1,1-tris{l_brace}2-[N{sup 2}-(1,1,3,3-tetramethylguanidino)]ethyl{r_brace}amine) is a unique example of an isolable synthetic S = 2 oxoiron(IV) complex, which serves as a model for the high-valent oxoiron(IV) intermediates observed in nonheme iron enzymes. Congruent with DFT calculations predicting a more reactive S = 2 oxoiron(IV) center, 1 has a lifetime significantly shorter than those of related S = 1 oxoiron(IV) complexes. The self-decay of 1 exhibits strictly first-order kinetic behavior and is unaffected by solvent deuteration, suggesting an intramolecular process. This hypothesis was supported by ESI-MS analysis of the iron products and a significant retardation of self-decay upon use of a perdeuteromethyl TMG{sub 3}tren isotopomer, d{sub 36}-1 (KIE = 24 at 25 C). The greatly enhanced thermal stability of d{sub 36}-1 allowed growth of diffraction quality crystals for which a high-resolution crystal structure was obtained. This structure showed an Fe=O unit (r = 1.661(2) {angstrom}) in the intended trigonal bipyramidal geometry enforced by the sterically bulky tetramethylguanidinyl donors of the tetradentate tripodal TMG{sub 3}tren ligand. The close proximity of the methyl substituents to the oxoiron unit yielded three symmetrically oriented short C-D {hor_ellipsis} O nonbonded contacts (2.38-2.49 {angstrom}), an arrangement that facilitated self-decay by rate-determining intramolecular hydrogen atom abstraction and subsequent formation of a ligand-hydroxylated iron(III) product. EPR and Moessbauer quantification of the various iron products, referenced against those obtained from reaction of 1 with 1,4-cyclohexadiene, allowed formulation of a detailed mechanism for the self-decay process. The solution of this first crystal structure of a high-spin (S = 2) oxoiron(IV) center represents a fundamental step on the path toward a full understanding of these pivotal biological intermediates.

  14. Structural characterization and DFT study of a new optical crystal: 2-amino-3-methylpyridinium-3,5-dinitrobenzoate

    Science.gov (United States)

    Sathya, K.; Dhamodharan, P.; Dhandapani, M.

    2018-05-01

    A new proton transfer complex was synthesized by the reaction between 2-amino-3-methyl pyridine with 3,5-dinitro benzoic acid in methanol solvent at room temperature. Chemical composition and stoichiometry of the synthesized complex 2-amino-3-methylpyridinium 3,5-dinitrobenzoate (AMPDB) were verified by CHN analysis. The AMPDB crystals were subjected to FT-IR spectral analysis to confirm the functional groups in the compound. UV-Vis-NIR spectral studies revealed that the AMPDB has a large optical transparency window. Single crystal XRD analysis reveals that AMPDB belongs to a monoclinic system with P21/c space group. NMR spectroscopic data indicate the exact carbon skeleton and hydrogen environment in the molecular structure of AMPDB. The thermal stability of the compound was investigated by thermogravimetry (TG). Computational studies such as optimisation of molecular geometry, natural bond analysis (NBO), Mulliken population analysis and HOMO-LUMO analysis were performed using Gaussian 09 software by B3LYP method at 6-311 G(d p) basis set. The first order hyperpolarizability (β) value is 37 times greater than that of urea. The optical nonlinearities of AMPDB have been investigated by Z-scan technique with He-Ne laser radiation of wavelength 632.8 nm. Hirshfeld analysis indicate O⋯H/H⋯O interactions are the superior interactions confirming intensive hydrogen bond net work.

  15. Structural characterization of framework-gas interactions in the metal-organic framework Co2(dobdc) by in situ single-crystal X-ray diffraction.

    Science.gov (United States)

    Gonzalez, Miguel I; Mason, Jarad A; Bloch, Eric D; Teat, Simon J; Gagnon, Kevin J; Morrison, Gregory Y; Queen, Wendy L; Long, Jeffrey R

    2017-06-01

    The crystallographic characterization of framework-guest interactions in metal-organic frameworks allows the location of guest binding sites and provides meaningful information on the nature of these interactions, enabling the correlation of structure with adsorption behavior. Here, techniques developed for in situ single-crystal X-ray diffraction experiments on porous crystals have enabled the direct observation of CO, CH 4 , N 2 , O 2 , Ar, and P 4 adsorption in Co 2 (dobdc) (dobdc 4- = 2,5-dioxido-1,4-benzenedicarboxylate), a metal-organic framework bearing coordinatively unsaturated cobalt(ii) sites. All these molecules exhibit such weak interactions with the high-spin cobalt(ii) sites in the framework that no analogous molecular structures exist, demonstrating the utility of metal-organic frameworks as crystalline matrices for the isolation and structural determination of unstable species. Notably, the Co-CH 4 and Co-Ar interactions observed in Co 2 (dobdc) represent, to the best of our knowledge, the first single-crystal structure determination of a metal-CH 4 interaction and the first crystallographically characterized metal-Ar interaction. Analysis of low-pressure gas adsorption isotherms confirms that these gases exhibit mainly physisorptive interactions with the cobalt(ii) sites in Co 2 (dobdc), with differential enthalpies of adsorption as weak as -17(1) kJ mol -1 (for Ar). Moreover, the structures of Co 2 (dobdc)·3.8N 2 , Co 2 (dobdc)·5.9O 2 , and Co 2 (dobdc)·2.0Ar reveal the location of secondary (N 2 , O 2 , and Ar) and tertiary (O 2 ) binding sites in Co 2 (dobdc), while high-pressure CO 2 , CO, CH 4 , N 2 , and Ar adsorption isotherms show that these binding sites become more relevant at elevated pressures.

  16. Optical and structural characterization of GaSb and Te-doped GaSb single crystals

    International Nuclear Information System (INIS)

    Tirado-Mejia, L.; Villada, J.A.; Rios, M. de los; Penafiel, J.A.; Fonthal, G.; Espinosa-Arbelaez, D.G.; Ariza-Calderon, H.; Rodriguez-Garcia, M.E.

    2008-01-01

    Optical and structural properties of GaSb and Te-doped GaSb single crystals are reported herein. Utilizing the photoreflectance technique, the band gap energy for doped samples was obtained at 0.814 eV. Photoluminescence (PL) spectra showed a peak at 0.748 eV that according to this research, belongs to electronic states of pure GaSb and not to the longitudinal optical (LO) phonon replica as has been reported by other authors. Analysis of the full width at half maximum (FWHM) values of X-ray diffraction, as well as micro-Raman peaks showed that the inclusion of Te decreases the crystalline quality

  17. Syntheses and structure characterization of ten acid-base hybrid crystals based on imidazole derivatives and mineral acids

    Science.gov (United States)

    Hu, Kaikai; Deng, Bowen; Jin, Shouwen; Ding, Aihua; Jin, Shide; Zhu, Jin; Zhang, Huan; Wang, Daqi

    2018-04-01

    Cocrystallization of the imidazole derivatives with a series of mineral acids gave a total of ten hybrid salts with the compositions: [(H2bzm)(Cl)2·3H2O] (1), [(H2bzm)(ClO4)2] (2), [(H2bze)(Cl)2·2H2O] (3), [(H2bze)(Br)2·2H2O] (4), [(H2bzp)(Cl)2·4H2O] (5), [(H2bzp)(Br)2·4H2O] (6), (2-(imidazol-1-yl)-1-phenylethanone): (phosphoric acid) [(Himpeta)+(H2PO4)-] (7), [(H2impd)(Br)2] (8), [(H2impd)(ClO4)2] (9), and [(Hbzml)(Cl)] (10). The ten salts have been characterised by X-ray diffraction analysis, IR, and elemental analysis, and the melting points of all the salts were also reported. And their structural and supramolecular aspects are fully analyzed. The result reveals that among the ten investigated crystals the ring N atoms of the imidazole are protonated when the acids are deprotonated, and the crystal packing is interpreted in terms of the strong charge-assisted classical H-bonds between the NH+ and deprotonated acidic groups. Further analysis of the crystal packing of the salts indicated that a different set of additional CHsbnd O, CH2sbnd O, CHsbnd Cl, CH2sbnd Cl, CHsbnd N, CHsbnd Br, CH2sbnd Br, Osbnd O, O-π, Br-π, CH-π, and π-π associations contribute to the stabilization and expansion of the total high-dimensional frameworks. For the coexistence of the various weak nonbonding interactions these structures adopted homo or hetero supramolecular synthons or both. Some classical supramolecular synthons, such as R21(7), R22(7), R22(8), and R42(8), usually observed in the organic solids, were again shown to be involved in constructing some of these H-bonding networks.

  18. Crystal structure of cafenstrole

    Directory of Open Access Journals (Sweden)

    Gihaeng Kang

    2015-08-01

    Full Text Available The title compound (systematic name: N,N-diethyl-3-mesitylsulfonyl-1H-1,2,4-triazole-1-carboxamide, C16H22N4O3S, is a triazole herbicide. The dihedral angle between the planes of the triazole and benzene ring planes is 88.14 (10°. In the crystal, C—H...O hydrogen bonds and weak C—H...π interactions link adjacent molecules, forming one-dimensional chains along the a axis.

  19. Crystal structure of pseudoguainolide

    Directory of Open Access Journals (Sweden)

    Noureddine Beghidja

    2015-03-01

    Full Text Available The lactone ring in the title molecule, C15H22O3 (systematic name: 3,4a,8-trimethyldodecahydroazuleno[6,5-b]furan-2,5-dione, assumes an envelope conformation with the methine C atom adjacent to the the methine C atom carrying the methyl substituent being the flap atom. The other five-membered ring adopts a twisted conformation with the twist being about the methine–methylene C—C bond. The seven-membered ring is based on a twisted boat conformation. No specific interactions are noted in the the crystal packing.

  20. Crystal structure and biochemical characterization of beta-keto thiolase B from polyhydroxyalkanoate-producing bacterium Ralstonia eutropha H16

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Eun-Jung; Son, Hyeoncheol Francis [Structural and Molecular Biology Laboratory, School of Life Sciences and Biotechnology, Kyungpook National University, Daehak-ro 80, Buk-ku, Daegu 702-701 (Korea, Republic of); Kim, Sangwoo [Structural and Molecular Biology Laboratory, School of Life Sciences and Biotechnology, Kyungpook National University, Daehak-ro 80, Buk-ku, Daegu 702-701 (Korea, Republic of); School of Nono-Bioscience and Chemical Engineering, Ulsan National Institute of Science and Technology (UNIST), Ulsan 689-798 (Korea, Republic of); Ahn, Jae-Woo [Structural and Molecular Biology Laboratory, School of Life Sciences and Biotechnology, Kyungpook National University, Daehak-ro 80, Buk-ku, Daegu 702-701 (Korea, Republic of); Kim, Kyung-Jin, E-mail: kkim@knu.ac.kr [Structural and Molecular Biology Laboratory, School of Life Sciences and Biotechnology, Kyungpook National University, Daehak-ro 80, Buk-ku, Daegu 702-701 (Korea, Republic of)

    2014-02-14

    Highlights: • We determined a crystal structure of β-keto thiolase from Ralstonia eutropha H16 (ReBktB). • Distinct substrate binding mode ReBktB was elucidated. • Enzymatic kinetic parameters of ReBktB were revealed. - Abstract: ReBktB is a β-keto thiolase from Ralstonia eutropha H16 that catalyzes condensation reactions between acetyl-CoA with acyl-CoA molecules that contains different numbers of carbon atoms, such as acetyl-CoA, propionyl-CoA, and butyryl-CoA, to produce valuable bioproducts, such as polyhydroxybutyrate, polyhydroxybutyrate-hydroxyvalerate, and hexanoate. We solved a crystal structure of ReBktB at 2.3 Å, and the overall structure has a similar fold to that of type II biosynthetic thiolases, such as PhbA from Zoogloea ramigera (ZrPhbA). The superposition of this structure with that of ZrPhbA complexed with CoA revealed the residues that comprise the catalytic and substrate binding sites of ReBktB. The catalytic site of ReBktB contains three conserved residues, Cys90, His350, and Cys380, which may function as a covalent nucleophile, a general base, and second nucleophile, respectively. For substrate binding, ReBktB stabilized the ADP moiety of CoA in a distinct way compared to ZrPhbA with His219, Arg221, and Asp228 residues, whereas the stabilization of β-mercaptoethyamine and pantothenic acid moieties of CoA was quite similar between these two enzymes. Kinetic study of ReBktB revealed that K{sub m}, V{sub max}, and K{sub cat} values of 11.58 μM, 1.5 μmol/min, and 102.18 s{sup −1}, respectively, and the catalytic and substrate binding sites of ReBktB were further confirmed by site-directed mutagenesis experiments.

  1. Synthesis, crystal structure and characterization of a new organic-inorganic hybrid material 4-(ammonium methyl) pipyridinium hexachloro stanate (II) trihydrate

    Science.gov (United States)

    Lassoued, Mohamed Saber; Abdelbaky, Mohammed S. M.; Lassoued, Abdelmajid; Ammar, Salah; Gadri, Abdellatif; Ben Salah, Abdelhamid; García-Granda, Santiago

    2018-03-01

    The present paper undertakes the study of (C6H16N2) SnCl6·3H2O which is a new hybrid compound. It was prepared and characterized by single crystal X-ray diffraction, X-ray powder, Hirshfeld surface, Spectroscopy measurement, thermal study and photoluminescence properties. The single crystal X-ray diffraction studies revealed that the compound crystallizes in monoclinic Cc space group with cell parameters a = 8.3309(9) Å, b = 22.956(2) Å, c = 9.8381(9) Å, β = 101.334(9) ° and Z = 4. The atomic arrangement shows an alternation of organic and inorganic entities. The cohesion between these entities is performed via Nsbnd H⋯Cl, Nsbnd H⋯O, Osbnd H⋯Cl and Osbnd H⋯O hydrogen bonding to form a three-dimensional network. Hirshfeld surface analysis was used to investigate intermolecular interactions, as well 2D finger plots were conducted to reveal the contribution of these interactions in the crystal structure quantitatively. The X-ray powder is in agreement with the X-ray structure. Scanning electron microscope (SEM) was carried out. Furthermore, the room temperature infrared (IR) spectrum of the title compound was recorded and analyzed on the basis of data found in the literature. Solid state 13C NMR spectrum shows four signals, confirming the solid state structure determined by X-ray diffraction. Besides, the thermal analysis studies were performed, but no phase transition was found in the temperature range between 30 and 450 °C. The optical and PL properties of the compound were investigated in the solid state at room temperature and exhibited three bands at 348 and 401 cm-1 and a strong fluorescence at 480 nm.

  2. Crystal structure and characterization of a novel layered copper-lithium phosphonate with antiferromagnetic intrachain Cu(II)···Cu(II) interactions

    Energy Technology Data Exchange (ETDEWEB)

    Abdelbaky, Mohammed S.M. [Departments of Physical and Analytical Chemistry and Organic and Inorganic Chemistry, University of Oviedo-CINN, 33006 Oviedo (Spain); Amghouz, Zakariae [Scientific and Technical Services, University of Oviedo-CINN, 33006 Oviedo (Spain); Department of Materials Science and Metallurgical Engineering, University of Oviedo, Campus Universitario, 33203 Gijón (Spain); Blanco, David Martínez [Scientific and Technical Services, University of Oviedo-CINN, 33006 Oviedo (Spain); García-Granda, Santiago; García, José R. [Departments of Physical and Analytical Chemistry and Organic and Inorganic Chemistry, University of Oviedo-CINN, 33006 Oviedo (Spain)

    2017-04-15

    Novel metal phosphonate [CuLi(PPA)] [H{sub 3}PPA=3-phosphonopropionic acid] was synthesized hydrothermally and characterized by single-crystal X-ray diffraction, powder X-ray diffraction, scanning electron microscopy, infrared spectroscopy, and thermogravimetric analysis. It crystallizes in the space group C2/c, with cell parameters a=21.617(2) Å, b=4.9269(2) Å, c=14.342(1) Å, β=132.3(2)°, and Z=8. Its framework is built up from a main trimer, acting as a secondary building unit (SBU), which is formed by vertex-shared between two (LiO{sub 4}) and one (Cu(1)O{sub 4}) polyhedra. These units repeat along b-axis forming infinite inorganic chains, these chains are in turn cross-linked by corner sharing with (Cu(2)O{sub 4}) polyhedra to produce inorganic layers lying in the bc-plane. The neighboring layers are connected through the PPA ligand, leading to a 3D pillared-layered structure. The topological analysis reveals that the compound exhibits 3,4,10-c net. Finally, magnetic susceptibility measurement of this compound over the temperature range of 2–300 K reveals the occurrence of weak antiferromagnetic intrachain interactions. - Graphical abstract: Hydrothermal synthesis and structural characterization of a novel lithium-copper phosphonate, formulated as [CuLi(PPA)] (H{sub 3}PPA=3-phosphonopropionic acid), have been reported. This compound has a 3D pillared-layered structure with 3,4,10-c net topology. The magnetic susceptibility data over the temperature range of 2–300 K reveals the occurrence of weak antiferromagnetic interactions. - Highlights: • Novel metal phosphonate, [CuLi(PPA)] (1), has been synthesized and characterized. • Compound 1 has a 3D pillared-layered structure with 3,4,10-c net topology. • Magnetic susceptibility data reveals the occurrence of weak antiferromagnetic interactions.

  3. Crystal structure refinement with SHELXL

    Energy Technology Data Exchange (ETDEWEB)

    Sheldrick, George M., E-mail: gsheldr@shelx.uni-ac.gwdg.de [Department of Structural Chemistry, Georg-August Universität Göttingen, Tammannstraße 4, Göttingen 37077 (Germany)

    2015-01-01

    New features added to the refinement program SHELXL since 2008 are described and explained. The improvements in the crystal structure refinement program SHELXL have been closely coupled with the development and increasing importance of the CIF (Crystallographic Information Framework) format for validating and archiving crystal structures. An important simplification is that now only one file in CIF format (for convenience, referred to simply as ‘a CIF’) containing embedded reflection data and SHELXL instructions is needed for a complete structure archive; the program SHREDCIF can be used to extract the .hkl and .ins files required for further refinement with SHELXL. Recent developments in SHELXL facilitate refinement against neutron diffraction data, the treatment of H atoms, the determination of absolute structure, the input of partial structure factors and the refinement of twinned and disordered structures. SHELXL is available free to academics for the Windows, Linux and Mac OS X operating systems, and is particularly suitable for multiple-core processors.

  4. Crystal structure of pymetrozine

    Directory of Open Access Journals (Sweden)

    Youngeun Jeon

    2015-07-01

    Full Text Available The title compound, C10H11N5O {systematic name: 6-methyl-4-[(E-(pyridin-3-ylmethylideneamino]-4,5-dihydro-1,2,4-triazin-3(2H-one}, C10H11N5O, is used as an antifeedant in pest control. The asymmetric unit comprises two independent molecules, A and B, in which the dihedral angles between the pyridinyl and triazinyl ring planes [r.m.s. deviations = 0.0132 and 0.0255 ] are 11.60 (6 and 18.06 (4°, respectively. In the crystal, N—H...O, N—H...N, C—H...N and C—H...O hydrogen bonds, together with weak π–π interactions [ring-centroid separations = 3.5456 (9 and 3.9142 (9 Å], link the pyridinyl and triazinyl rings of A molecules, generating a three-dimensional network.

  5. Preparation, crystal structure, and dielectric characterization of Li2W2O7 ceramic at RF and microwave frequency range

    Directory of Open Access Journals (Sweden)

    Jinwu Chen

    2017-02-01

    Full Text Available Single phase Li2W2O7 with anorthic structure was prepared by the conventional solid-state reaction method at 550∘C and the anorthic structure was stable up to 660∘C. The dielectric properties at radio frequency (RF and microwave frequency range were characterized. The sample sintered at 640∘C exhibited the optimum microwave dielectric properties with a relative permittivity of 12.2, a quality factor value of 17,700GHz (at 9.8GHz, and a temperature coefficient of the resonant frequency of −232ppm/∘C as well as a high relative density ∼94.1%. Chemical compatibility measurement indicated Li2W2O7 did not react with aluminum electrodes when sintered at 640∘C for 4h.

  6. Crystal structure, Hirshfeld surface analysis, quantum mechanical study and spectroscopic characterization of the non-centrosymmetric coordination compound bis(4-fluoroaniline)dichloridozincate

    Science.gov (United States)

    Ben Nasr, M.; Soudani, S.; Lefebvre, F.; Jelsch, C.; Ben Nasr, C.

    2017-06-01

    The Zn(II) complex with the monodentate ligand 4-fluoroaniline, ZnCl2(C6H4FNH2)2, has been prepared and characterized by single crystal X-ray diffraction, solid state nuclear magnetic resonance, infrared spectroscopy and differential scanning calorimetry. The Zn(II) ion is tetracoordinated by two nitrogen atoms of two monodentate 4-fluoroaniline ligands and two chlorine atoms. In the molecular arrangement, the ZnCl2(C6H4FNH2)2 entities are interconnected via Nsbnd H⋯Cl hydrogen bonds to form layers parallel to the (a, b) plane. The nature and proportion of contacts in the crystal packing were investigated through the Hirshfeld surfaces. The crystal is mainly maintained by electrostatic attractions Cl- … Hsbnd N and by extensive hydrophobic contacts as revealed by the Hirshfeld 2D fingerprint plots and statistical analysis. The13C and 19F CP-MAS NMR spectra are in agreement with the X-ray structure and confirm the phase purity of the crystalline sample. The vibrational absorption bands were identified by infrared spectroscopy. A calorimetric study shows that the title compound is stable until 262.5 °C.

  7. Negative Refraction Angular Characterization in One-Dimensional Photonic Crystals

    OpenAIRE

    Lugo, Jesus Eduardo; Doti, Rafael; Faubert, Jocelyn

    2011-01-01

    Background Photonic crystals are artificial structures that have periodic dielectric components with different refractive indices. Under certain conditions, they abnormally refract the light, a phenomenon called negative refraction. Here we experimentally characterize negative refraction in a one dimensional photonic crystal structure; near the low frequency edge of the fourth photonic bandgap. We compare the experimental results with current theory and a theory based on the group velocity de...

  8. Crystal growth and structure, electrical, and optical characterization of the semiconductor Cu2SnSe3

    International Nuclear Information System (INIS)

    Marcano, G.; Rincon, C.; Chalbaud, L. M. de; Bracho, D. B.; Perez, G. Sanchez

    2001-01-01

    X-ray powder diffraction by p-type Cu 2 SnSe 3 , prepared by the vertical Bridgman--Stockbarger technique, shows that this material crystallizes in a monoclinic structure, space group Cc, with unit cell parameters a=6.5936(1)Aa, b=12.1593(4)Aa, c=6.6084(3)Aa, and β=108.56(2) o . The temperature variation of the hole concentration p obtained from the Hall effect and electrical resistivity measurements from about 160 to 300 K, is explained as due to the thermal activation of an acceptor level with an ionization energy of 0.067 eV, whereas below 100 K, the conduction in the impurity band dominates the electrical transport process. From the analysis of the p vs T data, the density-of-states effective mass of the holes is estimated to be nearly of the same magnitude as the free electron mass. In the valence band, the temperature variation of the hole mobility is analyzed by taking into account the scattering of charge carriers by ionized and neutral impurities, and acoustic phonons. In the impurity band, the mobility is explained as due to the thermally activated hopping transport. From the analysis of the optical absorption spectra at room temperature, the fundamental energy gap was determined to be 0.843 eV. The photoconductivity spectra show the presence of a narrow band gap whose main peak is observed at 0.771 eV. This band is attributed to a free-to-bound transition from the defect acceptor level to the conduction band. The origin of this acceptor state, consistent with the chemical composition of the samples and screening effects, is tentatively attributed to selenium interstitials. copyright 2001 American Institute of Physics

  9. Crystal growth and structure, electrical, and optical characterization of the semiconductor Cu{sub 2}SnSe{sub 3}

    Energy Technology Data Exchange (ETDEWEB)

    Marcano, G.; Rincon, C.; de Chalbaud, L. M.; Bracho, D. B.; Perez, G. Sanchez

    2001-08-15

    X-ray powder diffraction by p-type Cu{sub 2}SnSe{sub 3}, prepared by the vertical Bridgman--Stockbarger technique, shows that this material crystallizes in a monoclinic structure, space group Cc, with unit cell parameters a=6.5936(1)Aa, b=12.1593(4)Aa, c=6.6084(3)Aa, and {beta}=108.56(2){sup o}. The temperature variation of the hole concentration p obtained from the Hall effect and electrical resistivity measurements from about 160 to 300 K, is explained as due to the thermal activation of an acceptor level with an ionization energy of 0.067 eV, whereas below 100 K, the conduction in the impurity band dominates the electrical transport process. From the analysis of the p vs T data, the density-of-states effective mass of the holes is estimated to be nearly of the same magnitude as the free electron mass. In the valence band, the temperature variation of the hole mobility is analyzed by taking into account the scattering of charge carriers by ionized and neutral impurities, and acoustic phonons. In the impurity band, the mobility is explained as due to the thermally activated hopping transport. From the analysis of the optical absorption spectra at room temperature, the fundamental energy gap was determined to be 0.843 eV. The photoconductivity spectra show the presence of a narrow band gap whose main peak is observed at 0.771 eV. This band is attributed to a free-to-bound transition from the defect acceptor level to the conduction band. The origin of this acceptor state, consistent with the chemical composition of the samples and screening effects, is tentatively attributed to selenium interstitials. {copyright} 2001 American Institute of Physics.

  10. Synthesis, characterization, crystal structure and HSA binding of two new N,O,O-donor Schiff-base ligands derived from dihydroxybenzaldehyde and tert-butylamine

    Science.gov (United States)

    Khosravi, Iman; Hosseini, Farnaz; Khorshidifard, Mahsa; Sahihi, Mehdi; Rudbari, Hadi Amiri

    2016-09-01

    Two new o-hydroxy Schiff-bases compounds, L1 and L2, were derived from the 1:1 M condensation of 2,3-dihydroxybenzaldehyde and 2,4-dihydroxybenzaldehyde with tert-butylamine and were characterized by elemental analysis, FT-IR, 1H and 13C NMR spectroscopies. The crystal structure of L2 was also determined by single crystal X-ray analysis. The crystal structure of L2 showed that the compound exists as a zwitterionic form in the solid state, with the H atom of the phenol group being transferred to the imine N atom. It adopts an E configuration about the central Cdbnd N double bond. Furthermore, binding of these Schiff base ligands to Human Serum Albumin (HSA) was investigated by fluorescence quenching, absorption spectroscopy, molecular docking and molecular dynamics (MD) simulation methods. The fluorescence emission of HSA was quenched by ligands. Also, suitable models were used to analyze the UV-vis absorption spectroscopy data for titration of HSA solution by various amounts of Schiff bases. The spectroscopic studies revealed that these Schiff bases formed 1:1 complex with HSA. Energy transfer mechanism of quenching was discussed and the values of 3.35 and 1.57 nm as the mean distances between the bound ligands and the HSA were calculated for L1 and L2, respectively. Molecular docking results indicated that the main active binding site for these Schiff bases ligands is in subdomain IB. Moreover, MD simulation results suggested that this Schiff base complex can interact with HSA, with a slight modification of its tertiary structure.

  11. Characterization of the local layer structure of a broad wall in a surface stabilized ferroelectric liquid crystal using synchrotron X-ray micro-diffraction

    International Nuclear Information System (INIS)

    Iida, Atsuo; Noma, Takashi; Miyata, Hirokatsu.

    1996-01-01

    The local layer structure of the broad wall of a zig-zag defect in a thin-surface stabilized ferroelectric liquid crystal cell was characterized using a synchrotron X-ray microbeam of less than 5 μm spatial resolution. By using a rocking curve measurement at the broad wall, multiple or broad peaks were observed between a pair of peaks due to a chevron structure. These new peaks are clear evidence of a modified pseudo-bookshelf structure at the wall. For 1.5 μm thick cells, a bookshelf layer is relatively flat, but is accompanied by small areas of inclined layer connecting the bookshelf and the chevron structures. For 10 μm thick cells, the pseudo-bookshelf structure bends or undulates both perpendicular and parallel to the rubbing direction. No appreciable change in the layer spacing was observed in the modified pseudo-bookshelf structure. The temperature dependence of the broad wall layer structure was also measured. (author)

  12. Characterization of the local layer structure of a broad wall in a surface stabilized ferroelectric liquid crystal using synchrotron X-ray micro-diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Iida, Atsuo [National Lab. for High Energy Physics, Tsukuba, Ibaraki (Japan); Noma, Takashi; Miyata, Hirokatsu

    1996-01-01

    The local layer structure of the broad wall of a zig-zag defect in a thin-surface stabilized ferroelectric liquid crystal cell was characterized using a synchrotron X-ray microbeam of less than 5 {mu}m spatial resolution. By using a rocking curve measurement at the broad wall, multiple or broad peaks were observed between a pair of peaks due to a chevron structure. These new peaks are clear evidence of a modified pseudo-bookshelf structure at the wall. For 1.5 {mu}m thick cells, a bookshelf layer is relatively flat, but is accompanied by small areas of inclined layer connecting the bookshelf and the chevron structures. For 10 {mu}m thick cells, the pseudo-bookshelf structure bends or undulates both perpendicular and parallel to the rubbing direction. No appreciable change in the layer spacing was observed in the modified pseudo-bookshelf structure. The temperature dependence of the broad wall layer structure was also measured. (author)

  13. Synthesis, Characterization, Crystal Structure and Antibacterial Activities of Transition Metal(II Complexes of the Schiff Base 2-[(4-Methylphenyliminomethyl]-6-methoxyphenol

    Directory of Open Access Journals (Sweden)

    Guo-Liang Zhao

    2009-05-01

    Full Text Available Five transition metal(II complexes, [ML2Cl2] 1~5, were synthesized from the reaction of MCl2·nH2O (M = Mn, Co, Ni, Cu, Cd and the Schiff base ligand 2-[(4-methylphenyliminomethyl]-6-methoxyphenol (C15H15NO2, L, obtained by condensation of o-vanillin (2-hydroxy-3-methoxybenzaldehyde with p-toluidine. They were characterized by elemental analysis, molar conductance, FT-IR spectra, thermal analysis. The structure of complex 1 was determined by single-crystal X-ray diffraction. Its crystal structure is of monoclinic system, space group P21/c with a = 9.0111(18 Å, b = 11.222(2 Å, c =28.130 (6 Å, α = 90 º, β = 92.29(3 º, γ = 90 º, V = 2867.6(10 Å3, Z = 4. The Mn atom is six-coordinate and displays distorted octahedral geometry.The Schiff base ligand and its complexes have been tested in vitro to evaluate their antibacterial activity against bacteria, viz., Escherichia coli, Staphylococcus aureus and Bacillus subtilis. It has been found that the complexes have higher activity than the corresponding free Schiff base ligand against the same bacteria.

  14. Tris(bipyridineMetal(II-Templated Assemblies of 3D Alkali-Ruthenium Oxalate Coordination Frameworks: Crystal Structures, Characterization and Photocatalytic Activity in Water Reduction

    Directory of Open Access Journals (Sweden)

    Alla Dikhtiarenko

    2016-02-01

    Full Text Available A series of 3D oxalate-bridged ruthenium-based coordination polymers with the formula of {[ZII(bpy3][MIRu(C2O43]}n (ZII = Zn2+ (1, Cu2+ (3, 4, Ru2+ (5, 6, Os2+ (7, 8; MI = Li+, Na+; bpy = 2,2’-bipyridine and {[ZnII(bpy3](H2O[LiRu(C2O43]}n (2 has been synthesized at room temperature through a self-assembly reaction in aqueous media and characterized by single-crystal and powder X-ray diffraction, elemental analysis, infrared and diffuse reflectance UV–Vis spectroscopy and thermogravimetric analysis. The crystal structures of all compounds comprise chiral 3D honeycomb-like polymeric nets of the srs-type, which possess triangular anionic cages where [ZII(bpy3]2+ cationic templates are selectively embedded. Structural analysis reveals that the electronic configuration of the cationic guests is affected by electrostatic interaction with the anionic framework. Moreover, the MLCT bands gaps values for 1–8 can be tuned in a rational way by judicious choice of [ZII(bpy3]2+ guests. The 3D host-guest polymeric architectures can be used as self-supported heterogeneous photocatalysts for the reductive splitting of water, exhibiting photocatalytic activity for the evolution of H2 under UV light irradiation.

  15. The purification, crystallization and preliminary structural characterization of PhzM, a phenazine-modifying methyltransferase from Pseudomonas aeruginosa

    International Nuclear Information System (INIS)

    Gohain, Neelakshi; Thomashow, Linda S.; Mavrodi, Dmitri V.; Blankenfeldt, Wulf

    2006-01-01

    PhzM, an S-adenosylmethionine-dependent methyltransferase enzyme that catalyzes a reaction involved in the biosynthesis of pyocyanin in P. aeruginosa, was cloned, overexpressed and crystallized. Data collection from native and selenomethionine-labelled crystals is reported. Pyocyanin, phenazine-1-carboxylic acid and more than 70 related compounds collectively known as phenazines are produced by various species of Pseudomonas, including the fluorescent pseudomonad P. aeruginosa, a Gram-negative opportunistic pathogen in humans and animals. P. aeruginosa synthesizes a characteristic blue water-soluble compound called pyocyanin (1-hydroxy-5-methyl-phenazine). Two enzymes designated PhzM and PhzS are involved in the terminal steps of its synthesis and very little is known about these enzymes. In this study, PhzM, a dimeric S-adenosylmethionine-dependent methyltransferase, was purified and crystallized from PEG 3350/sodium cacodylate/sodium citrate pH 6.5. The crystals belong to space group P1, with unit-cell parameters a = 46.1, b = 61.8, c = 69.6 Å, α = 96.3, β = 106.6, γ = 106.9°. They contain one dimer in the asymmetric unit and diffract to a resolution of 1.8 Å. Anomalous data to 2.3 Å resolution have been collected from seleno-l-methionine-labelled PhzM

  16. Synthesis, characterization, crystal structure and theoretical studies on 4-bromo-2-[(E)-6-methyl-2-pyridyliminomethyl]phenol

    Czech Academy of Sciences Publication Activity Database

    Khalaji, A.D.; Mighani, H.; Kazemnejadi, M.; Gotoh, K.; Ishida, H.; Fejfarová, Karla; Dušek, Michal

    2017-01-01

    Roč. 10, May (2017), s. 1808-1813 ISSN 1878-5352 Grant - others:AV ČR(CZ) Praemium Academiae Institutional support: RVO:68378271 Keywords : Schiff base * single-crystal * spectroscopy * DFT * hydrogen bond Subject RIV: BM - Solid Matter Physics ; Magnetism OBOR OECD: Condensed matter physics (including formerly solid state physics, supercond.) Impact factor: 4.553, year: 2016

  17. Characterization of molecular associations involving L-ornithine and α-ketoglutaric acid: crystal structure of L-ornithinium α-ketoglutarate.

    Science.gov (United States)

    Allouchi, H; Céolin, R; Berthon, L; Tombret, F; Rietveld, I B

    2014-07-01

    The crystal structure of L-ornithinium α-ketoglutarate (C5H13N2O2, C5H5O5) has been solved by direct methods using single crystal X-ray diffraction data. It crystallizes in the monoclinic system, space group P21, unit cell parameters a=15.4326(3), b=5.2015(1), c=16.2067(3) Å and β=91.986(1)°, containing two independent pairs of molecular ions in the asymmetric unit. An extensive hydrogen-bond network and electrostatic charges due to proton transfer provide an important part of the cohesive energy of the crystal. The conformational versatility of L-ornithine and α-ketoglutaric acid is illustrated by the present results and crystal structures available from the Cambridge Structural Database. Copyright © 2014 Elsevier Masson SAS. All rights reserved.

  18. AB stacked few layer graphene growth by chemical vapor deposition on single crystal Rh(1 1 1) and electronic structure characterization

    International Nuclear Information System (INIS)

    Kordatos, Apostolis; Kelaidis, Nikolaos; Giamini, Sigiava Aminalragia; Marquez-Velasco, Jose; Xenogiannopoulou, Evangelia; Tsipas, Polychronis; Kordas, George; Dimoulas, Athanasios

    2016-01-01

    Highlights: • Growth of non-defective few layer graphene on Rh(1 1 1) substrates using an ambient- pressure CVD method. • Control of graphene stacking order via the cool-down rate. • Graphene is grown with a mainly AB-stacking geometry on single-crystalline Rhodium for a slow cool-down rate and non-AB for a very fast cool-down. • Good epitaxial orientation of the surface is presented through the RHEED data and confirmed with ARPES characterization for the lower cool-down rate, where graphene's ΓK direction a perfectly aligned with the ΓK direction of the Rh(1 1 1) single crystal. - Abstract: Graphene synthesis on single crystal Rh(1 1 1) catalytic substrates is performed by Chemical Vapor Deposition (CVD) at 1000 °C and atmospheric pressure. Raman analysis shows full substrate coverage with few layer graphene. It is found that the cool-down rate strongly affects the graphene stacking order. When lowered, the percentage of AB (Bernal) -stacked regions increases, leading to an almost full AB stacking order. When increased, the percentage of AB-stacked graphene regions decreases to a point where almost a full non AB-stacked graphene is grown. For a slow cool-down rate, graphene with AB stacking order and good epitaxial orientation with the substrate is achieved. This is indicated mainly by Raman characterization and confirmed by Reflection high-energy electron diffraction (RHEED) imaging. Additional Scanning Tunneling Microscopy (STM) topography data confirm that the grown graphene is mainly an AB-stacked structure. The electronic structure of the graphene/Rh(1 1 1) system is examined by Angle resolved Photo-Emission Spectroscopy (ARPES), where σ and π bands of graphene, are observed. Graphene's ΓK direction is aligned with the ΓK direction of the substrate, indicating no significant contribution from rotated domains.

  19. AB stacked few layer graphene growth by chemical vapor deposition on single crystal Rh(1 1 1) and electronic structure characterization

    Energy Technology Data Exchange (ETDEWEB)

    Kordatos, Apostolis [National Center for Scientific Research “Demokritos”, Athens, 15310 (Greece); Kelaidis, Nikolaos, E-mail: n.kelaidis@inn.demokritos.gr [National Center for Scientific Research “Demokritos”, Athens, 15310 (Greece); Giamini, Sigiava Aminalragia [National Center for Scientific Research “Demokritos”, Athens, 15310 (Greece); University of Athens, Department of Physics, Section of Solid State Physics, Athens, 15684 Greece (Greece); Marquez-Velasco, Jose [National Center for Scientific Research “Demokritos”, Athens, 15310 (Greece); National Technical University of Athens, Department of Physics, Athens, 15784 Greece (Greece); Xenogiannopoulou, Evangelia; Tsipas, Polychronis; Kordas, George; Dimoulas, Athanasios [National Center for Scientific Research “Demokritos”, Athens, 15310 (Greece)

    2016-04-30

    Highlights: • Growth of non-defective few layer graphene on Rh(1 1 1) substrates using an ambient- pressure CVD method. • Control of graphene stacking order via the cool-down rate. • Graphene is grown with a mainly AB-stacking geometry on single-crystalline Rhodium for a slow cool-down rate and non-AB for a very fast cool-down. • Good epitaxial orientation of the surface is presented through the RHEED data and confirmed with ARPES characterization for the lower cool-down rate, where graphene's ΓK direction a perfectly aligned with the ΓK direction of the Rh(1 1 1) single crystal. - Abstract: Graphene synthesis on single crystal Rh(1 1 1) catalytic substrates is performed by Chemical Vapor Deposition (CVD) at 1000 °C and atmospheric pressure. Raman analysis shows full substrate coverage with few layer graphene. It is found that the cool-down rate strongly affects the graphene stacking order. When lowered, the percentage of AB (Bernal) -stacked regions increases, leading to an almost full AB stacking order. When increased, the percentage of AB-stacked graphene regions decreases to a point where almost a full non AB-stacked graphene is grown. For a slow cool-down rate, graphene with AB stacking order and good epitaxial orientation with the substrate is achieved. This is indicated mainly by Raman characterization and confirmed by Reflection high-energy electron diffraction (RHEED) imaging. Additional Scanning Tunneling Microscopy (STM) topography data confirm that the grown graphene is mainly an AB-stacked structure. The electronic structure of the graphene/Rh(1 1 1) system is examined by Angle resolved Photo-Emission Spectroscopy (ARPES), where σ and π bands of graphene, are observed. Graphene's ΓK direction is aligned with the ΓK direction of the substrate, indicating no significant contribution from rotated domains.

  20. Towards accurate structural characterization of metal centres in protein crystals: the structures of Ni and Cu T6 bovine insulin derivatives

    DEFF Research Database (Denmark)

    Frankær, Christian Grundahl; Mossin, Susanne; Ståhl, Kenny

    2014-01-01

    Using synchrotron radiation (SR), the crystal structures of T6 bovine insulin complexed with Ni2+ and Cu2+ were solved to 1.50 and 1.45 Å resolution, respectively. The level of detail around the metal centres in these structures was highly limited, and the coordination of water in Cu site II...... of the copper insulin derivative was deteriorated as a consequence of radiation damage. To provide more detail, X-ray absorption spectroscopy (XAS) was used to improve the information level about metal coordination in each derivative. The nickel derivative contains hexacoordinated Ni2+ with trigonal symmetry...... by electron paramagnetic resonance (EPR). The coordination distances were refined from EXAFS with standard deviations within 0.01 Å. The insulin derivative containing Cu2+ is sensitive towards photoreduction when exposed to SR. During the reduction of Cu2+ to Cu+, the coordination geometry of copper changes...

  1. Crystal structure and characterization of the novel NH{sup +} Midline-Horizontal-Ellipsis N hydrogen bonded polar crystal [NH{sub 2}(CH{sub 2}){sub 4}NH][BF{sub 4}

    Energy Technology Data Exchange (ETDEWEB)

    Wojtas, M., E-mail: maciej.wojtas@chem.uni.wroc.pl [Faculty of Chemistry, University of Wroclaw, Joliot-Curie 14, 50-383 Wroclaw (Poland); Gagor, A. [W. Trzebiatowski Institute of Low Temperature and Structure Research, Polish Academy of Science, PO Box 1410, 50-950 Wroclaw (Poland); Czupinski, O. [Faculty of Chemistry, University of Wroclaw, Joliot-Curie 14, 50-383 Wroclaw (Poland); Medycki, W. [Institute of Molecular Physics, Polish Academy of Science, Smoluchowskiego 17, 60-179 Poznan (Poland); Jakubas, R. [Faculty of Chemistry, University of Wroclaw, Joliot-Curie 14, 50-383 Wroclaw (Poland)

    2012-03-15

    Dielectric properties and phase transitions of the piperazinium tetrafluoroborate ([NH{sub 2}(CH{sub 2}){sub 4}NH][BF{sub 4}], abbreviated as PFB) crystal are related to the one-dimensional arrangement of the cations linked by the bistable NH{sup +} Midline-Horizontal-Ellipsis N hydrogen bonds and molecular motions of the [BF{sub 4}]{sup -} units. The crystal structure of [NH{sub 2}(CH{sub 2}){sub 4}NH][BF{sub 4}] is monoclinic at room temperature with the polar space group Pn. The polar/acentric properties of the room temperature phase IV have been confirmed by the piezoelectric and pyroelectric measurements. DSC measurements show that the compound undergoes three first-order structural phase transitions: at 421/411 K (heating/cooling), at 386/372 K and at 364/349 K. {sup 1}H and {sup 19}F NMR measurements indicate the reorientational motions of [BF{sub 4}]{sup -} anions and piperazinium(+) cations as well as the proton motion in the hydrogen-bonded chains of piperazine along the [001] direction. Over the phase I the isotropic reorientational motions or even self-diffusion of the cations and anions are expected. The conductivity measurements in the vicinity of the II-I PT indicate a superionic phase over the phase I. - Graphical abstract: It must be emphasized that the titled compound represents the first organic-inorganic simple salt containing the single-protonated piperazinium cation which was studied by means of the wide variety of experimental techniques. A survey of Cambridge Structural Database (CSD version 5.32 (November 2010) and updates (May 2011)) for structure containing the piperazinium cations yields 248 compounds with the doubly protonated piperazinium(2+) cations and only eight compounds with the singly protonated piperazinium(+) cations. Among these structures only one is the hybrid organic-inorganic material. This is piperazinium nitrate characterized structurally. The crystal packing of [NH{sub 2}(CH{sub 2}){sub 4}NH][BF{sub 4}], phase IV. The

  2. Quantitative characterization of new supramolecular synthons involving fluorine atoms in the crystal structures of di- and tetrafluorinated benzamides.

    Science.gov (United States)

    Mondal, Pradip Kumar; Yadav, Hare Ram; Choudhury, Angshuman Roy; Chopra, Deepak

    2017-10-01

    Strong hydrogen bonds play a significant role in crystal packing. In particular, the involvement of interactions involving fluorine in controlling the crystal packing requires appropriate attention, especially in the presence of other strong hydrogen bonds. In the present study, a detailed quantitative assessment has been performed of the nature, energetics and topological properties derived from the electron density in model compounds based on fluorinated benzamides (a total of 46 fluorine-substituted benzamides containing multiple fluorine atoms) in the solid state. The primary motivation in the design of such molecules is to enhance the acidity of the interacting H atoms in the presence of an increasing number of F atoms on the molecular scaffold, resulting in increased propensity towards the formation of intermolecular interactions involving organic fluorine. This exercise has resulted in the identification of new and frequently occurring supramolecular synthons involving F atoms in the packing of molecules in the solid state. The energetics associated with short and directional intermolecular Csp 2 -H...F-Csp 2 interactions with significantly high electrostatic contributions is noteworthy, and the topological analysis reveals the bonding character of these ubiquitous interactions in crystal packing in addition to the presence of Csp 2 -F...F-Csp 2 contacts.

  3. Nickel(II) and copper(II) complexes of N,N-dialkyl-N‧-3-chlorobenzoylthiourea: Synthesis, characterization, crystal structures, Hirshfeld surfaces and antimicrobial activity

    Science.gov (United States)

    Binzet, Gun; Gumus, Ilkay; Dogen, Aylin; Flörke, Ulrich; Kulcu, Nevzat; Arslan, Hakan

    2018-06-01

    We synthesized four new N,N-dialkyl-N‧-3-chlorobenzoylthiourea ligands (Alkyl: Dimethyl, diethyl, di-n-propyl and di-n-butyl) and their metal complexes with copper and nickel atoms. The structure of all synthesized compounds was fully characterized by physicochemical, spectroscopic and single crystal X-ray diffraction analysis techniques. The physical, spectral and analytical data of the newly synthesized metal complexes have shown the formation of 1:2 (metal:ligand) ratio. The benzoylthiourea ligands coordinate with metal atoms through oxygen and sulphur atoms. The metal atoms are in slightly distorted square-planar coordination geometry in Ni(II) or Cu(II) complex. Two oxygen and two sulphur atoms are mutually cis to each other in Ni(II) or Cu(II) complex. The intermolecular contacts in the compounds, which are HL1 and HL3, were examined by Hirshfeld surfaces and fingerprint plots using the data obtained from X-ray single crystal diffraction measurement. Besides these, their antimicrobial activities against Gram-positive bacteria (Bacillus subtilis, Staphylococcus aureus, Streptococcus pyogenes and Enterococcus faecalis) and Gram-negative bacteria (Escherichia coli and Pseudomonas aeruginosa) and anti-yeast activity (Candida glabrata, Candida parapsilosis and Candida albicans) were investigated. This exhibited some promising results towards testing organism. Among all the compounds, Ni(L1)2 complex showed high activity against Bacillus subtilis with MIC values at 7.81 μg/mL.

  4. Structural characterization of Li1.2v3o8 insertion electrodes by single-crystal x-ray-diffraction

    CSIR Research Space (South Africa)

    De Picciotto, LA

    1993-08-01

    Full Text Available The crystal structures of Li1.2V3O8 and a lithiated product Li4.0V3O8 have been determined by single-crystal X-ray diffraction methods. The structure refinement of Li1.2V308 confirms that of Li1+xV3O8(x almost-equal-to 0) reported by Wadsley thirty...

  5. Crystal structure and magnetic susceptibility of UOSe single crystals

    International Nuclear Information System (INIS)

    Kaczorowski, D.; Muenster Univ.; Poettgen, R.; Jeitschko, W.; Gajek, Z.; Zygmunt, A.

    1993-01-01

    The crystal structure and magnetic susceptibility behaviour of UOSe single crystals have been studied. UOSe crystalizes in the tetragonal PbFC1-type structure (space group P4/nmm) with the lattice parameters: a = 390.38(5) pm and c = 698.05(9) pm. It orders antiferromagnetically at T N =100±2 K and exhibits a very strong anisotropy in the susceptibility vs temperature variation. The magnetic and thermodynamic properties of UOSe are successfully interpreted in the framework of a perturbative ab initio crystal field approach. (Author)

  6. Crystal structure and magnetic susceptibility of UOSe single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Kaczorowski, D. (Polish Academy of Sciences, Wroclaw (Poland). Inst. for Low Temperature and Structure Research Muenster Univ. (Germany). Anorganisch-Chemisches Inst.); Poettgen, R.; Jeitschko, W. (Muenster Univ. (Germany). Anorganisch-Chemisches Inst.); Gajek, Z.; Zygmunt, A. (Polish Academy of Sciences, Wroclaw (Poland). Inst. for Low Temperature and Structure Research)

    1993-01-01

    The crystal structure and magnetic susceptibility behaviour of UOSe single crystals have been studied. UOSe crystalizes in the tetragonal PbFC1-type structure (space group P4/nmm) with the lattice parameters: a = 390.38(5) pm and c = 698.05(9) pm. It orders antiferromagnetically at T[sub N]=100[+-]2 K and exhibits a very strong anisotropy in the susceptibility vs temperature variation. The magnetic and thermodynamic properties of UOSe are successfully interpreted in the framework of a perturbative ab initio crystal field approach. (Author).

  7. Towards accurate structural characterization of metal centres in protein crystals: the structures of Ni and Cu T6 bovine insulin derivatives

    International Nuclear Information System (INIS)

    Frankaer, Christian Grundahl; Mossin, Susanne; Ståhl, Kenny; Harris, Pernille

    2013-01-01

    The level of structural detail around the metal sites in Ni 2+ and Cu 2+ T 6 insulin derivatives was significantly improved by using a combination of single-crystal X-ray crystallography and X-ray absorption spectroscopy. Photoreduction and subsequent radiation damage of the Cu 2+ sites in Cu insulin was followed by XANES spectroscopy. Using synchrotron radiation (SR), the crystal structures of T 6 bovine insulin complexed with Ni 2+ and Cu 2+ were solved to 1.50 and 1.45 Å resolution, respectively. The level of detail around the metal centres in these structures was highly limited, and the coordination of water in Cu site II of the copper insulin derivative was deteriorated as a consequence of radiation damage. To provide more detail, X-ray absorption spectroscopy (XAS) was used to improve the information level about metal coordination in each derivative. The nickel derivative contains hexacoordinated Ni 2+ with trigonal symmetry, whereas the copper derivative contains tetragonally distorted hexacoordinated Cu 2+ as a result of the Jahn–Teller effect, with a significantly longer coordination distance for one of the three water molecules in the coordination sphere. That the copper centre is of type II was further confirmed by electron paramagnetic resonance (EPR). The coordination distances were refined from EXAFS with standard deviations within 0.01 Å. The insulin derivative containing Cu 2+ is sensitive towards photoreduction when exposed to SR. During the reduction of Cu 2+ to Cu + , the coordination geometry of copper changes towards lower coordination numbers. Primary damage, i.e. photoreduction, was followed directly by XANES as a function of radiation dose, while secondary damage in the form of structural changes around the Cu atoms after exposure to different radiation doses was studied by crystallography using a laboratory diffractometer. Protection against photoreduction and subsequent radiation damage was carried out by solid embedment of Cu insulin

  8. Amine free crystal structure: The crystal structure of d(CGCGCG)2 and methylamine complex crystal

    International Nuclear Information System (INIS)

    Ohishi, Hirofumi; Tsukamoto, Koji; Hiyama, Yoichi; Maezaki, Naoyoshi; Tanaka, Tetsuaki; Ishida, Toshimasa

    2006-01-01

    We succeeded in the crystallization of d(CGCGCG) 2 and methylamine Complex. The crystal was clear and of sufficient size to collect the X-ray crystallographic data up to 1.0 A resolution using synchrotron radiation. As a result of X-ray crystallographic analysis of 2F o - F c map was much clear and easily traced. It is First time monoamine co-crystallizes with d(CGCGCG) 2 . However, methylamine was not found from the complex crystal of d(CGCGCG) 2 and methylamine. Five Mg ions were found around d(CGCGCG) 2 molecules. These Mg ions neutralized the anion of 10 values of the phosphate group of DNA with five Mg 2+ . DNA stabilized only by a metallic ion and there is no example of analyzing the X-ray crystal structure like this. Mg ion stabilizes the conformation of Z-DNA. To use monoamine for crystallization of DNA, we found that we can get only d(CGCGCG) 2 and Mg cation crystal. Only Mg cation can stabilize the conformation of Z-DNA. The method of using the monoamine for the crystallization of DNA can be applied to the crystallization of DNA of long chain of length in the future like this

  9. Phenoxo bridged dinuclear Zn(II) Schiff base complex as new precursor for preparation zinc oxide nanoparticles: Synthesis, characterization, crystal structures and photoluminescence studies

    Energy Technology Data Exchange (ETDEWEB)

    Saeednia, S., E-mail: sami_saeednia@yahoo.com [Department of Chemistry, Faculty of Science, Vali-e-Asr University of Rafsanjan, Rafsanjan 77188-97111 (Iran, Islamic Republic of); Iranmanesh, P. [Department of physics, Faculty of Science, Vali-e-Asr University of Rafsanjan, Rafsanjan 77188-97111 (Iran, Islamic Republic of); Ardakani, M. Hatefi; Mohammadi, M.; Norouzi, Gh. [Department of Chemistry, Faculty of Science, Vali-e-Asr University of Rafsanjan, Rafsanjan 77188-97111 (Iran, Islamic Republic of)

    2016-06-15

    Highlights: • A novel nano-scale Zn(II) complex was synthesized by solvothermal method. • Chemical structure of the nanostructures was characterized as well as bulk complex. • The photoluminescence property of the complex was investigated at room temperature. • The thermogravimetry and differential thermal analysis were carried out. • Thermal decomposition of the nanostructures was prepared zinc oxide nanoparticles. - Abstract: Nanoparticles of a novel Zn(II) Schiff base complex, [Zn(HL)NO{sub 3}]{sub 2} (1), (H{sub 2}L = 2-[(2-hydroxy-propylimino) methyl] phenol), was synthesized by using solvothermal method. Shape, morphology and chemical structure of the synthesized nanoparticles were characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), Fourier Transform Infrared Spectoscopy (FT-IR) and UV–vis spectroscopy. Structural determination of compound 1 was determined by single-crystal X-ray diffraction. The results were revealed that the zinc complex is a centrosymmetric dimer in which deprotonated phenolates bridge the two five-coordinate metal atoms and link the two halves of the dimer. The thermal stability of compound 1 was analyzed by thermal gravimetric analysis (TGA) and differential scanning calorimetry (DSC). The effect of the initial substrates concentration and reaction time on size and morphology of compound 1 nanostructure was investigated as well. Furthermore, the luminescent properties of the complex 1 were examined. ZnO nanoparticles with diameter between 15 and 20 nm were simply synthesized by solid-state transformation of compound 1 at 700 °C.

  10. Syntheses and structure characterization of ten acid-base hybrid crystals based on N-containing aromatic brønsted bases and mineral acids

    Science.gov (United States)

    Lin, Zhihao; Jin, Shouwen; Li, Xiaoliang; Xiao, Xiao; Hu, Kaikai; Guo, Ming; Chi, Xinchen; Liu, Hui; Wang, Daqi

    2017-10-01

    Cocrystallization of the aromatic brønsted bases with a series of mineral acids gave a total of ten hybrid salts with the compositions: (2-methylquinoline)2: (hydrochloride acid): 3H2O [(HL1)+. (L1)·· (Cl-) · (H2O)3] (1), (6-bromobenzo[d]thiazol-2-amine): (hydrochloride acid) [(HL2)+. (Cl-)] (2), (6-bromobenzo[d]thiazol-2-amine): (nitric acid) [(HL2)+. (NO3-)] (3), (6-bromobenzo[d]thiazol-2-amine): (sulfuric acid) [(HL2)+ · (HSO4)-] (4), (6-bromobenzo[d]thiazol-2-amine): (phosphoric acid) [(HL2)+ · (H2PO4)-] (5), (5,7-dimethyl-1,8-naphthyridine-2-amine): (hydrochloride acid): 3H2O [(HL3)+ · (Cl-) (H2O)3] (6), (5,7-dimethyl-1,8-naphthyridine-2-amine): (hydrobromic acid): CH3OH [(HL3)+ · (Br)- · CH3OH] (7), (5,7-dimethyl-1,8-naphthyridine-2-amine): (sulfuric acid): H2O [(HL3)+ · (HSO4)- · H2O] (8), (2-aminophenol): (phosphoric acid) [(HL4)+ · (H2PO4)-] (9), and (2-amino-4-chlorophenol): (phosphoric acid) [(HL5)+ · (H2PO4)-] (10). The ten salts have been characterized by X-ray diffraction analysis, IR, and elemental analysis, and the melting points of all the salts were also reported. And their structural and supramolecular aspects are fully analyzed. The result reveals that among the ten investigated crystals the ring N of the heterocycle or the NH2 in the aminophenol are protonated when the acids are deprotonated, and the crystal packing is interpreted in terms of the strong charge-assisted classical hydrogen bonds between the NH+/NH3+ and deprotonated acidic groups. Further analysis of the crystal packing of the salts indicated that a different family of additional CHsbnd O, CHsbnd Cl, CH3sbnd N, CH3sbnd O, CHsbnd Br, CH3sbnd Br, Brsbnd Cl, Clsbnd S, Osbnd S, Osbnd O, Brsbnd S, Hsbnd H, and π-π associations contribute to the stabilization and expansion of the total high-dimensional frameworks. For the coexistence of the various weak nonbonding interactions these structures adopted homo or hetero supramolecular synthons or both. Some classical

  11. Studies on the syntheses, structural Characterization, antimicrobial of the CO-CRYSTAL 1,10-phenanthrolin-1-IUM(1,10-phenH+)-caffeine(caf)-hexafluorophosphate

    Science.gov (United States)

    El Hamdani, H.; El Amane, M.; Duhayon, C.

    2018-03-01

    Co-crystal of 1,10-phenanthrolin-1-ium-caffeine-hexafluorophosphate was synthesized, studied by FTIR, 1H, 13C NMR, DSC and X-ray structure and crystallized in the monoclinic space group C2/c. The unit cell parameters are a = 19.3761 (3), b = 17.9548 (3), c = 13.8074 (3) with β = 117.8132 (10). The final R value is 0.069 for 29,522 measured reflections. The co-crystal structure analysis indicate the 1,10-phenanthroline is protonated by one nitrogen atom and formed the 1,10-phenanthrolin-1-ium cation, which is stabilized by hydrogen bonds N+-H…Odbnd C interaction with carbonyl and imidazol ring in caffeine molecule. The intermolecular hydrogen bonds: Csbnd H...O, Csbnd H...N, Nsbnd H...O, Csbnd H...F and intramolecular hydrogen bond: C1sbnd H12...O14, together play a vital role in stabilizing the structure of co-crystal. The X-ray structural analysis confirm the assignments of the structure from infrared, 1H, 13C NMR, spectroscopic data DSC and molar conductivity analysis. The antimicrobial activity of the co-crystal was studied.

  12. Synthesis, crystal structure and characterizations of a new red phosphor K{sub 3}EuB{sub 6}O{sub 12}

    Energy Technology Data Exchange (ETDEWEB)

    Zhao, Dan, E-mail: iamzd1996@163.com [College of Chemistry and Chemical Engineering, Henan Polytechnic University, Jiaozuo, Henan, 454000 (China); State Key Laboratory of Structural Chemistry, Fuzhou, Fujian, 350002 (China); Ma, Fa-Xue; Wu, Zhi-Qiang; Zhang, Lei [College of Chemistry and Chemical Engineering, Henan Polytechnic University, Jiaozuo, Henan, 454000 (China); Wei, Wei, E-mail: wwei@cnu.edu.cn [Department of Chemistry, Capital Normal University, Beijing, 100048 (China); Yang, Juan; Zhang, Rong-Hua; Chen, Peng-Fei; Wu, Shan-Xuan [College of Chemistry and Chemical Engineering, Henan Polytechnic University, Jiaozuo, Henan, 454000 (China)

    2016-10-01

    A new potassium europium borate K{sub 3}EuB{sub 6}O{sub 12} has been prepared using a high temperature molten salt method and structurally characterized by single crystal X-ray diffraction (SC-XRD) analyses. Its structure features a three-dimensional (3D) framework composed of isolated [B{sub 5}O{sub 10}]{sup 5−} anions that are bridged by K{sup +} and Eu{sup 3+} ions. In this structure, one crystallographic distinct atom site is mixed occupied by K/Eu at a molar ratio of 1:1. The self-activated photoluminescence (PL) of K{sub 3}EuB{sub 6}O{sub 12} was studied. The excitation spectrum covers a wide range from 322 to 466 nm, which suggests that the K{sub 3}EuB{sub 6}O{sub 12} phosphors can be effectively excited by a near-UV light source. The emission spectrum consists of groups of lines in the red spectral region due to the {sup 5}D{sub 0}→{sup 7}F{sub j} (j = 1, 2, 3, 4) electronic transitions of Eu{sup 3+} ions, with the most intense line at 611 nm. We may expect that K{sub 3}EuB{sub 6}O{sub 12} has the potential to be a red phosphor pumped by near-UV LED chips. - Highlights: • A new red phosphor K{sub 3}EuB{sub 6}O{sub 12} was prepared. • The crystal structure of K{sub 3}EuB{sub 6}O{sub 12} was determined for the first time. • The photoluminescence properties of K{sub 3}EuB{sub 6}O{sub 12} are studied. • K{sub 3}EuB{sub 6}O{sub 12} show intense self-activated red emission under near-UV light excitation.

  13. Structural, electrical and magnetic characterization of in-situ crystallized ZnO:Co thin films synthesized by reactive magnetron sputtering

    Energy Technology Data Exchange (ETDEWEB)

    Lardjane, Soumia, E-mail: lardjanesoumia@yahoo.fr [IRTES-LERMPS, UTBM, Site de Montbéliard, 90010 Belfort Cedex (France); Division Etude et Prédiction des Matériaux, Unité de Recherche Matériaux et Energies Renouvelables, Université Abou Bekr Belkaid, Tlemcen (Algeria); Pour Yazdi, Mohammad Arab [IRTES-LERMPS, UTBM, Site de Montbéliard, 90010 Belfort Cedex (France); Martin, Nicolas [FEMTO-ST, Département MN2S, UMR 6174 CNRS, Université de Franche-Comté, ENSMM, UTBM, 32, Avenue de l’Observatoire, 25044 Besancon Cedex (France); Bellouard, Christine [Laboratoire de Physique des Matériaux, Nancy University, CNRS, 54506 Vandoeuvre-lès-Nancy Cedex (France); Fenineche, Nour-eddine [IRTES-LERMPS, UTBM, Site de Montbéliard, 90010 Belfort Cedex (France); Schuler, Andreas [Solar Energy and Buildings Physics Laboratory, EPFL ENAC IIC LESO-PB, Station 18, Bâtiment LE, 1015 Lausanne (Switzerland); Merad, Ghouti [Division Etude et Prédiction des Matériaux, Unité de Recherche Matériaux et Energies Renouvelables, Université Abou Bekr Belkaid, Tlemcen (Algeria); Billard, Alain [IRTES-LERMPS, UTBM, Site de Montbéliard, 90010 Belfort Cedex (France)

    2015-07-01

    Zn{sub 1−x}Co{sub x}O (0 < x < 0.146) conductive thin films have been deposited by reactive magnetron sputtering of metallic Zn and Co targets at high pressure and temperature. The structural properties have been investigated by using X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). It has been observed that all as-deposited films are crystallized in pure hcp ZnO structure and neither traces of metallic nor oxide Co-rich clusters were detected. The average grain size estimated from full width at half maximum of XRD results varied between 65 and 83 nm. XPS analyses exhibit that Co ions are successfully entered into ZnO lattice as Co{sup +2}. The electrical properties including conductivity, carrier density and carrier mobility were determined by Hall effect measurements in a temperature range from 300 K to 475 K. The conductivity of the films decreases from σ{sub 300K} = 2.2 × 10{sup 4} to 2.3 × 10{sup −1} Sm{sup −1} as the Co content changes from 0 to 0.146. Magnetic measurements reveal the absence of ferromagnetism even at 3 K and a paramagnetic Curie–Weiss behavior associated to magnetic clusters. - Highlights: • Zn{sub 1−x}Co{sub x}O conductive thin films were synthesized by reactive magnetron sputtering. • Structural characterization exhibited the absence of Co clusters or secondary phases. • The film conductivity decreased with increasing of Co concentration. • No ferromagnetism was observed in all Co doped ZnO samples. • Magnetic properties are described by a Curie–Weiss behavior associated to clusters.

  14. Preparation and characterization of superfine ammonium perchlorate (AP) crystals through ceramic membrane anti-solvent crystallization

    Science.gov (United States)

    Ma, Zhenye; Li, Cheng; Wu, Rujun; Chen, Rizhi; Gu, Zhenggui

    2009-10-01

    In this paper, a novel ceramic membrane anti-solvent crystallization (CMASC) method was proposed for the safe and rapid preparation ammonium perchlorate (AP) crystals, in which the acetone and ethyl acetate were chosen as solvent and anti-solvent, respectively. Comparing with the conventional liquid anti-solvent crystallization (LASC), CMASC which successfully introduces ceramic membrane with regular pore structure to the LASC as feeding medium, is favorable to control the rate of feeding rate and, therefore, to obtain size and morphology controllable AP. Several kinds of micro-sized AP particles with different morphology were obtained including polyhedral-like, quadrate-like to rod-like. The effect of processing parameters on the crystal size and shape of AP crystals such as volume ratio of anti-solvent to solvent, feeding pressure and crystallization temperature were investigated. It is found that higher volume ratio of anti-solvent to solvent, higher feeding pressure and higher temperature result in smaller particle size. Scaning electron microscopy (SEM) and X-ray diffraction (XRD) were used to characterize the resulting AP crystals. The nucleation and growth kinetic of the resulting AP crystals were also discussed.

  15. Synthesis, characterization, and crystal structure of 2-amino-7-methyl-5-oxo-4-phenyl-4,5-dihydropyrano[3,2-c] pyran-3-carbonitrile

    Energy Technology Data Exchange (ETDEWEB)

    Sharma, S. [University of Jammu, X-ray Crystallography Laboratory, Post-Graduate Department of Physics and Electronics (India); Banerjee, B.; Brahmachari, G. [Visva-Bharati (a Central University), Laboratory of Natural Products & Organic Synthesis, Department of Chemistry (India); Kant, Rajni; Gupta, V. K., E-mail: vivek-gupta2k2@hotmail.com [University of Jammu, X-ray Crystallography Laboratory, Post-Graduate Department of Physics and Electronics (India)

    2015-12-15

    2-Amino-7-methyl-5-oxo-4-phenyl-4,5-dihydropyrano[3,2-c] pyran-3-carbonitrile, C{sub 16}H{sub 12}N{sub 2}O{sub 3} is synthesized via one-pot multi-component reaction at room temperature using commercially available urea as inexpensive and environmentally benign organo-catalyst. Its structure is determined by single-crystal X-ray diffraction technique The crystals are monoclinic, a = 10.7357(12), b = 8.7774(8), c = 15.0759(16) Å, β = 103.575(11)°, Z = 4, sp. gr. P2{sub 1}/n, R = 0.0551 for 1696 observed reflections. The crystal structure is stabilized by N–H···N, C–H···O, and C–H···π interactions.

  16. Non-covalent interactions in 2-methylimidazolium copper(II) complex (MeImH)2[Cu(pfbz)4]: Synthesis, characterization, single crystal X-ray structure and packing analysis

    Science.gov (United States)

    Sharma, Raj Pal; Saini, Anju; Kumar, Santosh; Kumar, Jitendra; Sathishkumar, Ranganathan; Venugopalan, Paloth

    2017-01-01

    A new anionic copper(II) complex, (MeImH)2 [Cu(pfbz)4] (1) where, MeImH = 2-methylimidazolium and pfbz = pentafluorobenzoate has been isolated by reacting copper(II) sulfate pentahydrate, pentafluorobenzoic acid and 2-methylimidazole in ethanol: water mixture in 1:2:2 molar ratio. This complex 1 has been characterized by elemental analysis, thermogravimetric analysis, spectroscopic techniques (UV-Vis, FT-IR) and conductance measurements. The complex salt crystallizes in monoclinic crystal system with space group C2/c. Single crystal X-ray structure determination revealed the presence of discrete ions: [Cu(pfbz)4]2- anion and two 2-methylimidazolium cation (C4H7N2)+. The crystal lattice is stabilized by strong hydrogen bonding and F⋯F interactions between cationic-anionic and the anionic-anionic moieties respectively, besides π-π interactions.

  17. Crystal structure and optical properties of silver nanorings

    Science.gov (United States)

    Zhou, Li; Fu, Xiao-Feng; Yu, Liao; Zhang, Xian; Yu, Xue-Feng; Hao, Zhong-Hua

    2009-04-01

    We report the polyol synthesis and crystal structure characterization of silver nanorings, which have perfect circular shape, smooth surface, and elliptical wire cross-section. The characterization results show that the silver nanorings have well-defined crystal of singly twinned along the whole ring. The spatial distribution of the scattering of a silver nanoring with slanted incidence reveals the unique focus effect of the nanoring, and the focus scattering varies with the incident wavelength. The silver nanorings with perfect geometry and well-defined crystal have potential applications in nanoscaled photonics, plasmonic devices, and optical manipulation.

  18. A new oxidovanadium(IV) Schiff base complex containing asymmetric tetradentate ONN′O′ Schiff base ligand: synthesis, characterization, crystal structure determination, thermal study and catalytic activity

    Czech Academy of Sciences Publication Activity Database

    Grivani, G.; Ghavami, A.; Eigner, Václav; Dušek, Michal; Khalaji, A.D.

    2015-01-01

    Roč. 26, č. 6 (2015), s. 779-784 ISSN 1001-8417 R&D Projects: GA ČR(CZ) GA14-03276S Institutional support: RVO:68378271 Keywords : oxidovanadium(IV) * Schiff base * crystal structure * nanoparticle * epoxidation Subject RIV: CC - Organic Chemistry Impact factor: 1.947, year: 2015

  19. Single crystal growth of yttrium calcium oxy borate (YCOB) crystals by flux technique and their characterization. CP-3.5

    International Nuclear Information System (INIS)

    Arun Kumar, R.; Senthilkumar, M.; Dhanasekaran, R.

    2007-01-01

    Yttrium calcium oxy borate single crystals were grown by the flux technique for the first time. Polycrystalline YCOB material was prepared by solid state reaction method. Single crystals of YCOB were grown using boron-tri-oxide flux. Several transparent single crystals of dimensions 10 x 5 x 5 mm 3 were obtained. The grown crystals were characterized by powder XRD and UV- VIS-NIR studies. The results of powder XRD confirm the crystalline structure of YCOB. The UV- VIS-NIR transmission spectrum reveals that the crystal is highly transparent (above 75%) from ultraviolet (220 nm) to near IR regions enabling it as a suitable candidate for high power UV applications

  20. SYNTHESIS, CHARACTERIZATION AND CRYSTAL STRUCTURES ...

    African Journals Online (AJOL)

    B. S. Chandravanshi

    Cambridge CB2 1EZ, UK (e-mail for deposition: deposit@ccdc.cam.ac.uk). REFERENCES. 1. Guilherme, L.R.; Massabni, A.C.; Cuin, A.; Oliveira, L.A.A.; Castellano, E.E.; Heinrich,. T.A.; Costa-Neto, C.M. J. Coord. Chem. 2009, 62, 1561. 2. Ashiq, U.; Ara, R.; Mahroof-Tahir, M.; Maqsood, Z.T.; Khan, K.M.; Khan, S.N.; Siddiqui,.

  1. Simple and Efficient One-Pot Synthesis, Spectroscopic Characterization and Crystal Structure of Methyl 5-(4-Chlorobenzoyloxy-1-phenyl-1H-pyrazole-3-carboxylate

    Directory of Open Access Journals (Sweden)

    Imtiaz Khan

    2012-07-01

    Full Text Available A facile one-pot synthesis of methyl 5-(4-chlorobenzoyloxy-1-phenyl-1H-pyrazole-3-carboxylate (4 is described. The title compound was efficiently synthesized by the reaction of phenyl hydrazine, dimethyl acetylenedicarboxylate and 4-chlorobenzoyl chloride in dichloromethane under reflux in good yield. The structure of the target compound was deduced by modern spectroscopic and analytical techniques and unequivocally confirmed by a single crystal X-ray diffraction analysis. The crystal of the title compound belongs to orthorhombic system, space group P 21 21 21 with cell parameters a = 6.6491(3 Å, b = 7.9627(6 Å, c = 30.621(5 Å, α = β = γ = 90° and Z = 4. The crystal packing of the compound (4 is stabilized by an offset π-stacking between the planar benzoyl-substituted diazole moieties.

  2. Synthesis, characterization and crystal structure determination of a new Zn(II Schiff base complex derived from condensation of a new asymmetrical tripodal amine, 3-((4-aminobutyl(pyridin-2-ylmethylaminopropan-1-ol and 2-hydroxy-3-methoxybenzaldehyde

    Directory of Open Access Journals (Sweden)

    Majid Rezaeivala

    2017-05-01

    Full Text Available A new tripodal amine, 3-((4-aminobutyl(pyridin-2-ylmethylaminopropan-1-ol (HL has been prepared. This has been used to synthesize a new Schiff base complex by template condensation with 2-hydroxy-3-methoxybenzaldehyde in the presence of Zn(II metal ion in methanol. The complex has been characterized using spectroscopic methods and the crystal structure of [ZnL]BF4, L:3-((4-aminobutyl(pyridin-2-ylmethylaminopropan-1-ol was confirmed by single crystal X-ray diffraction studies. Single crystal X-ray structure analysis showed that in the mononuclear Zn(II complex, [ZnL]BF4 the Zn(II ion is in a distorted square pyramidal environment.

  3. What makes a crystal structure report valid?

    NARCIS (Netherlands)

    Spek, Anthony L.|info:eu-repo/dai/nl/156517566

    2018-01-01

    Single crystal X-ray crystallography has developed into a unique, highly automated and accessible tool to obtain detailed information on molecular structures. Proper archival makes that referees, readers and users of the results of reported crystal structures no longer need to depend solely on the

  4. Crystal structure of prethrombin-1

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Zhiwei; Pelc, Leslie A.; Di Cera, Enrico (St. Louis-MED)

    2010-11-15

    Prothrombin is the zymogen precursor of the clotting enzyme thrombin, which is generated by two sequential cleavages at R271 and R320 by the prothrombinase complex. The structure of prothrombin is currently unknown. Prethrombin-1 differs from prothrombin for the absence of 155 residues in the N-terminal domain and is composed of a single polypeptide chain containing fragment 2 (residues 156-271), A chain (residues 272-320), and B chain (residues 321-579). The X-ray crystal structure of prethrombin-1 solved at 2.2-{angstrom} resolution shows an overall conformation significantly different (rmsd = 3.6 {angstrom}) from that of its active form meizothrombin desF1 carrying a cleavage at R320. Fragment 2 is rotated around the y axis by 29{sup o} and makes only few contacts with the B chain. In the B chain, the oxyanion hole is disrupted due to absence of the I16-D194 ion pair and the Na{sup +} binding site and adjacent primary specificity pocket are highly perturbed. A remarkable feature of the structure is that the autolysis loop assumes a helical conformation enabling W148 and W215, located 17 {angstrom} apart in meizothrombin desF1, to come within 3.3 {angstrom} of each other and completely occlude access to the active site. These findings suggest that the zymogen form of thrombin possesses conformational plasticity comparable to that of the mature enzyme and have significant implications for the mechanism of prothrombin activation and the zymogen {yields} protease conversion in trypsin-like proteases.

  5. Crystal structure of 2-pentyloxybenzamide

    Directory of Open Access Journals (Sweden)

    Bernhard Bugenhagen

    2014-10-01

    Full Text Available In the title molecule, C12H17NO2, the amide NH2 group is oriented toward the pentyloxy substituent and an intramolecular N—H...O hydrogen bond is formed with the pentyloxy O atom. The benzene ring forms dihedral angles of 2.93 (2 and 5.60 (2° with the amide group and the pentyloxy group mean planes, respectively. In the crystal, molecules are linked by pairs of N—H...O hydrogen bonds, forming inversion dimers with their molecular planes parallel, but at an offset of 0.45 (1 Å to each other. These dimers are ordered into two types of symmetry-related columns extended along the a axis, with the mean plane of one set of dimers in a column approximately parallel to (121 and the other in a column approximately parallel to (1-21. The two planes form a dihedral angle of 85.31 (2°, and are linked via C—H...O hydrogen bonds and C—H...π interactions, forming a three-dimensional framework structure.

  6. Method of fabricating patterned crystal structures

    KAUST Repository

    Yu, Liyang

    2016-12-15

    A method of manufacturing a patterned crystal structure for includes depositing an amorphous material. The amorphous material is modified such that a first portion of the amorphous thin-film layer has a first height/volume and a second portion of the amorphous thin-film layer has a second height/volume greater than the first portion. The amorphous material is annealed to induce crystallization, wherein crystallization is induced in the second portion first due to the greater height/volume of the second portion relative to the first portion to form patterned crystal structures.

  7. Crystal Structure and Functional Characterization of the Complement Regulator Mannose-binding Lectin (MBL)/Ficolin-associated Protein-1 (MAP-1)

    DEFF Research Database (Denmark)

    Skjoedt, M.-o.; Roversi, P.; Hummelshoj, T.

    2012-01-01

    .5 nM, respectively. We studied structural aspects of MAP-1 and could show by multi-angle laser light scattering that MAP-1 forms a calcium-dependent homo-dimer in solution. We were able to determine the crystal structure of MAP-1, which also contains a head-to-tail dimer approximately 146 Angstrom...... long. This structure of MAP-1 also enables modeling and assembly of the MASP-1 molecule in its entirety. Finally we found that MAP-1 competes with all three MASPs for ligand binding and is able to mediate a strong dose dependent inhibitory effect on the lectin pathway activation, as measured by levels...

  8. Photonic Crystal Laser-Driven Accelerator Structures

    International Nuclear Information System (INIS)

    Cowan, B

    2004-01-01

    The authors discuss simulated photonic crystal structure designs for laser-driven particle acceleration. They focus on three-dimensional planar structures based on the so-called ''woodpile'' lattice, demonstrating guiding of a speed-of-light accelerating mode by a defect in the photonic crystal lattice. They introduce a candidate geometry and discuss the properties of the accelerating mode. They also discuss the linear beam dynamics in the structure present a novelmethod for focusing the beam. In addition they describe ongoing investigations of photonic crystal fiber-based structures

  9. Structure characterization of Pd/Co/Pd tri-layer films epitaxially grown on MgO single-crystal substrates

    Energy Technology Data Exchange (ETDEWEB)

    Tobari, Kousuke, E-mail: tobari@futamoto.elect.chuo-u.ac.jp; Ohtake, Mitsuru; Nagano, Katsumasa; Futamoto, Masaaki

    2011-09-30

    Pd/Co/Pd tri-layer films were prepared on MgO substrates of (001), (111), and (011) orientations at room temperature by ultra high vacuum rf magnetron sputtering. The detailed film structures around the Co/Pd and the Pd/Co interfaces are investigated by reflection high energy electron diffraction. Pd layers of (001){sub fcc}, (111){sub fcc}, and (011){sub fcc} orientations epitaxially grow on the respective MgO substrates. Strained fcc-Co(001) single-crystal layers are formed on the Pd(001){sub fcc} layers by accommodating the fairly large lattice mismatch between the Co and the Pd layers. On the Co layers,, Pd polycrystalline layers are formed. When Co films are formed on the Pd(111){sub fcc} and the Pd(011){sub fcc} layers, atomic mixing is observed around the Co/Pd interfaces and fcc-CoPd alloy phases are coexisting with Co crystals. The Co crystals formed on the Pd(111){sub fcc} layers consist of hcp(0001) + fcc(111) and Pd(111){sub fcc} epitaxial layers are formed on the Co layers. Co crystals epitaxially grow on the Pd(011){sub fcc} layers with two variants, hcp(11-bar 00) and fcc(111). On the Co layers, Pd(011){sub fcc} epitaxial layers are formed.

  10. Structural characterization of silver nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Garcia, Paulo Ricardo; Sousa, Edi Carlos Pereira de; Pontuschka, Walter Maigon; Oliveira, Cristiano Luis Pinto de, E-mail: pauloricardoafg@yahoo.com.br [Universidade de Sao Paulo (USP), Sao Paulo, SP (Brazil). Instituto de Fisica

    2016-07-01

    Full text: Due to magnetic, optical and electrical properties metallic nanoparticles have been extensively studied to potential applications in biosensor production, separation of biological molecules, image techniques, drug delivery among several others. For such applications, it is crucial to have crystals with morphology and well defined structure. In this work we presented a detailed structured characterization of silver nanoparticles using small angle x-rays and light scattering methods. The comparison and correlation of these results with electron microscopy images permitted the determination of interesting structural parameters for the studied systems. The oscillations of the intensity curve of SAXS data reveal that this sample has particles with reasonable stability and well defined sizes. The mean radius obtained from the size distribution curve is in good agreement with the ones obtained by TEM images. As will be shown, the combination of several techniques and the correct analysis for the obtained experimental data provides unique information on the structure of the studied systems. (author)

  11. Synthesis, crystal structure, spectroscopic characterization, docking simulation and density functional studies of 1-(3,4-dimethoxyphenyl) -3-(4-flurophenyl)-propan-1-one

    Science.gov (United States)

    Khamees, Hussien Ahmed; Jyothi, Mahima; Khanum, Shaukath Ara; Madegowda, Mahendra

    2018-06-01

    The compound 1-(3,4-dimethoxyphenyl)-3-(4-flurophenyl)-propan-1-one (DFPO) was synthesized by Claisen-Schmidt condensation reaction and the single crystals were obtained by slow evaporation method. Three-dimensional structure was confirmed by single crystal X-ray diffraction method and exhibiting the triclinic crystal system with space group P-1. The crystal structure is stabilized by Csbnd H⋯O intermolecular and weak interactions. Computed molecular geometry has been obtained by density functional theory (DFT) and compared with experimental results. The spectra of both FT-IR in the range (4000-400 cm-1) and FT- Raman (3500-50 cm-1) of DFPO were recorded experimentally and computed by (DFT) using B3LYP/6-311G (d,p) as basis sets. Intramolecular charge transfer has been scanned using natural bond orbital (NBO) analysis and revealed the various contribution of bonding and lone pair to the stabilization of molecule. Nonlinear optical activity (NLO) of the title compound has been determined by second harmonic generation (SHG) and computed using DFT method. Hyperpolarizability, HOMO-LUMO energy gap, hardness, softness electronegativity and others Global reactivity descriptors of DFPO has been calculated and revealed complete picture of chemical reactivity of DFPO. Hirshfeld surface analyses were applied to investigate the intermolecular interactions and revealed that more than two-thirds of the inter contacts are associated with O⋯H, C⋯H and H⋯H interactions. Docking studies of DFPO showed inhibition of Vascular endothelial growth Factor human receptor (VEGFR-2) signalling pathway, which indicates DFPO as anti-angiogenesis, that play pivotal role in cancer, so we suggest it for clinical studies to evaluate its potential to treat human cancers.

  12. Hydrothermal synthesis, crystal structure and luminescence property ...

    Indian Academy of Sciences (India)

    The design and construction of ... dination polymers. It is difficult to design coordination .... The first endotherm at about 180 ... graphic data for coordination polymer 1. ... Sheldrick G M 1997 SHELXS-97: Program for solution of crystal structures ...

  13. imide, crystal structure, thermal and dielectric studies

    Indian Academy of Sciences (India)

    methyl imidazolium methylidene bis(trifluoromethanesulfonyl)imide, crystal structure, thermal and dielectric studies. BOUMEDIENE HADDAD1,2,3,∗, TAQIYEDDINE MOUMENE2, DIDIER VILLEMIN1,. JEAN-FRANÇOIS LOHIER1 and EL-HABIB ...

  14. SYNTHESIS, CRYSTAL STRUCTURE AND MAGNETIC ...

    African Journals Online (AJOL)

    Preferred Customer

    Much of the current effort on such extended hybrid metal organic complexes is ... In this paper, we report the synthesis, single crystal X-ray diffraction analysis and ..... with g = 2.0 (0.37 cm3 mol−1 K), and smoothly increases to a value of 0.45 ...

  15. Fabrication of GO/Cement Composites by Incorporation of Few-Layered GO Nanosheets and Characterization of Their Crystal/Chemical Structure and Properties.

    Science.gov (United States)

    Lv, Shenghua; Hu, Haoyan; Zhang, Jia; Luo, Xiaoqian; Lei, Ying; Sun, Li

    2017-12-18

    Original graphene oxide (GO) nanosheets were prepared using the Hummers method and found to easily aggregate in aqueous and cement composites. Using carboxymethyl chitosan (CCS) as a dispersant, few-layered GO nanosheets (1-2 layers) were obtained by forming CCS/GO intercalation composites. The testing results indicated that the few-layered GO nanosheets could uniformly spread, both in aqueous and cement composites. The cement composites were prepared with GO dosages of 0.03%, 0.05% and 0.07% and we found that they had a compact microstructure in the whole volume. A special feature was determined, namely that the microstructures consisted of regular-shaped crystals created by self-crosslinking. The X-ray diffraction (XRD) results indicated that there was a higher number of cement hydration crystals in GO/cement composites. Meanwhile, we also found that partially-amorphous Calcium-Silicate-Hydrate (C-S-H) gel turned into monoclinic crystals. At 28 days, the GO/cement composites reached the maximum compressive and flexural strengths at a 0.05% dosage. These strengths were 176.64 and 31.67 MPa and, compared with control samples, their increased ratios were 64.87% and 149.73%, respectively. Durability parameters, such as penetration, freeze-thaw, carbonation, drying-shrinkage value and pore structure, showed marked improvement. The results indicated that it is possible to obtain cement composites with a compact microstructure and with high performances by introducing CCS/GO intercalation composites.

  16. Synthesis, characterization and crystal structure of 6-Chloro-4,4‧-dimethyl-2,2‧-bipyridine and 4,4‧-Dimethyl 2,2‧-bipyridine N-Oxide

    Science.gov (United States)

    Conterosito, Eleonora; Magistris, Claudio; Barolo, Claudia; Croce, Gianluca; Milanesio, Marco

    2016-03-01

    The synthesis, the NMR characterization and the crystal structure of 6-Chloro 4,4‧-dimethyl 2,2‧-bipyridine and of the reaction intermediate 4,4‧-Dimethyl 2,2‧-bipyridine N-Oxide are here reported. The target compound crystallizes in the orthorhombic system while the intermediate is monoclinic. In both structures, the molecules are linked by weak interactions. The structure of the reaction intermediate N-oxide is characterized by a dihedral angle between the two phenyl rings of 161.77° while the other is almost planar with a dihedral angle of 179.15°. The crystal packing was investigated, also with the aid of Hirshfeld surface analysis. In the N-oxide reaction intermediate the packing is governed by CH-O interactions, while in the product the packing is simply driven by minimizing the voids and thus maximizing the density, with a prevalence of H•••H and C•••H contacts, as indicated by fingerprint decomposition analysis.

  17. CuLi2Sn and Cu2LiSn: Characterization by single crystal XRD and structural discussion towards new anode materials for Li-ion batteries.

    Science.gov (United States)

    Fürtauer, Siegfried; Effenberger, Herta S; Flandorfer, Hans

    2014-12-01

    The stannides CuLi 2 Sn (CSD-427095) and Cu 2 LiSn (CSD-427096) were synthesized by induction melting of the pure elements and annealing at 400 °C. The phases were reinvestigated by X-ray powder and single-crystal X-ray diffractometry. Within both crystal structures the ordered CuSn and Cu 2 Sn lattices form channels which host Cu and Li atoms at partly mixed occupied positions exhibiting extensive vacancies. For CuLi 2 Sn, the space group F-43m. was verified (structure type CuHg 2 Ti; a =6.295(2) Å; wR 2 ( F ²)=0.0355 for 78 unique reflections). The 4( c ) and 4( d ) positions are occupied by Cu atoms and Cu+Li atoms, respectively. For Cu 2 LiSn, the space group P 6 3 / mmc was confirmed (structure type InPt 2 Gd; a =4.3022(15) Å, c =7.618(3) Å; wR 2 ( F ²)=0.060 for 199 unique reflections). The Cu and Li atoms exhibit extensive disorder; they are distributed over the partly occupied positions 2( a ), 2( b ) and 4( e ). Both phases seem to be interesting in terms of application of Cu-Sn alloys as anode materials for Li-ion batteries.

  18. short communication synthesis and crystal structure of a polymeric

    African Journals Online (AJOL)

    Preferred Customer

    A new polymeric zinc(II) complex, [ZnL2(PDA)]n, has been prepared by the reaction of zinc sulfate ... complex has been characterized by single-crystal X-ray diffraction. .... Molecular structure of the complex at 30% probability displacement.

  19. Structural and compositional characterization of X-cut LiNbO3 crystals implanted with high energy oxygen and carbon ions

    International Nuclear Information System (INIS)

    Bentini, G.G.; Bianconi, M.; Cerutti, A.; Chiarini, M.; Pennestri, G.; Sada, C.; Argiolas, N.; Bazzan, M.; Mazzoldi, P.; Guzzi, R.

    2005-01-01

    High energy implantation of medium-light elements such as oxygen and carbon was performed in X-cut LiNbO 3 single crystals in order to prepare high quality optical waveguides. The compositional and damage profiles, obtained by exploiting the secondary ion mass spectrometry and Rutherford back-scattering techniques respectively, were correlated to the structural properties measured by the high resolution X-ray diffraction. This study evidences the development of tensile strain induced by the ion implantation that can contribute to the decrease of the ordinary refractive index variation through the photo-elastic effect

  20. Crystal structure from one-electron theory

    DEFF Research Database (Denmark)

    Skriver, H. L.

    1985-01-01

    The authors have studied the crystal structure of all the 3d, 4d, and 5d transition metals at zero pressure and temperature by means of the linear muffin-tin orbital method and Andersen's force theorem. They find that, although the structural energy differences seem to be overestimated by the the......The authors have studied the crystal structure of all the 3d, 4d, and 5d transition metals at zero pressure and temperature by means of the linear muffin-tin orbital method and Andersen's force theorem. They find that, although the structural energy differences seem to be overestimated...

  1. Synthesis, crystal structure and biological activity of novel diester cyclophanes

    International Nuclear Information System (INIS)

    Zhang, Pengfei; Yang, Bingqin; Fang, Xianwen; Cheng, Zhao; Yang, Meipan

    2012-01-01

    A series of novel diester cyclophanes was synthesized by esterification of 1,2-benzenedicarbonyl chloride with eight different diols under high dilution conditions. The structures of the compounds were verified by elemental analysis, 1 H nuclear magnetic resonance (NMR), IR spectroscopy and high resolution mass spectrometry (HRMS). The crystal structures of two compounds were characterized by single crystal X-ray diffractometry (XRD). All the new cyclophanes were evaluated for biological activities and the results showed that some of these compounds have low antibacterial or antifungal activities (author)

  2. Synthesis, crystal structure and biological activity of novel diester cyclophanes

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Pengfei; Yang, Bingqin; Fang, Xianwen; Cheng, Zhao; Yang, Meipan, E-mail: yangbq@nwu.edu.cn [Department of Chemistry, Key Laboratory of Synthetic and Natural Functional Molecule Chemistry, Northwest University, Shaanxi (China)

    2012-10-15

    A series of novel diester cyclophanes was synthesized by esterification of 1,2-benzenedicarbonyl chloride with eight different diols under high dilution conditions. The structures of the compounds were verified by elemental analysis, {sup 1}H nuclear magnetic resonance (NMR), IR spectroscopy and high resolution mass spectrometry (HRMS). The crystal structures of two compounds were characterized by single crystal X-ray diffractometry (XRD). All the new cyclophanes were evaluated for biological activities and the results showed that some of these compounds have low antibacterial or antifungal activities (author)

  3. Photonic crystals, light manipulation, and imaging in complex nematic structures

    Science.gov (United States)

    Ravnik, Miha; Å timulak, Mitja; Mur, Urban; Čančula, Miha; Čopar, Simon; Žumer, Slobodan

    2016-03-01

    Three selected approaches for manipulation of light by complex nematic colloidal and non-colloidal structures are presented using different own custom developed theoretical and modelling approaches. Photonic crystals bands of distorted cholesteric liquid crystal helix and of nematic colloidal opals are presented, also revealing distinct photonic modes and density of states. Light propagation along half-integer nematic disclinations is shown with changes in the light polarization of various winding numbers. As third, simulated light transmission polarization micrographs of nematic torons are shown, offering a new insight into the complex structure characterization. Finally, this work is a contribution towards using complex soft matter in optics and photonics for advanced light manipulation.

  4. Synthesis, characterization and crystal structure of [Cu2(LH2]•(ClO42. Influence of the weak Cu•••O(perchlorate interaction on the structure of Cu2N2O2 metallocycle

    Directory of Open Access Journals (Sweden)

    Mirković Marija

    2014-01-01

    Full Text Available The diimine-dioxime ligand, 4,9-diaza-3,10-diethyl-3,9-dodecadiene-2,11-dione bisoxime (LH2, containing a N4 donor set was prepared by Schiff base condensation of 2-hydroxyimino-3-pentanone and 1,4-diaminobutane in two ways: in protic and in aprotic solvent. Higher yield of (LH2 imine was obtained when the synthesis was carried out using protic solvent (C2H5OH instead of aprotic benzene (78% and 30%, respectively. Cu(II metal complex of diimine-dioxime was synthesized in CH3OH from metal salt and LH2 in mole ratio 1:1. The isolated complex was characterized by the elemental analysis, IR spectroscopy and cyclic voltammetry. The structure of [Cu2(LH2]•(ClO42 was determined by the single-crystal X-ray diffraction analysis. Comparison with the structurally related diimine-dioxime Cu(II complexes revealed the influence of the weak Cu•••O(perchlorate interaction on the geometry of the metallocycle. [Projekat Ministarstva nauke Republike Srbije, br. 45015, br. 172013, br. 172065 i br. 172014

  5. Growth and Characterization of ZnTe Crystal

    International Nuclear Information System (INIS)

    Nann Thazin

    2011-12-01

    High quality ZnTe crystals have been synthesized by vapor Transport method. The grown crystals were p-type. The concentration and mobility were 2.5 x 10 16 cm-3 and 23 cm2/Vs at 300K, according to Hall effect measurements. Surface morphology of the crystal was investigated by scanning electron microscope (SEM). Crystal orientation and lattice parameters of the crystals were also analysed by XRD. From X-ray diffraction studies the structure of the grown crystals were found to be zinc-blende. The crystal emitted light in the visible range at room temperature.

  6. Two-dimensional photonic crystal accelerator structures

    Directory of Open Access Journals (Sweden)

    Benjamin M. Cowan

    2003-10-01

    Full Text Available Photonic crystals provide a method of confining a synchronous speed-of-light mode in an all-dielectric structure, likely a necessary feature in any optical accelerator. We explore computationally a class of photonic crystal structures with translational symmetry in a direction transverse to the electron beam. We demonstrate synchronous waveguide modes and discuss relevant parameters of such modes. We then explore how accelerator parameters vary as the geometry of the structure is changed and consider trade-offs inherent in the design of an accelerator of this type.

  7. Crystal structure of enolase from Drosophila melanogaster.

    Science.gov (United States)

    Sun, Congcong; Xu, Baokui; Liu, Xueyan; Zhang, Zhen; Su, Zhongliang

    2017-04-01

    Enolase is an important enzyme in glycolysis and various biological processes. Its dysfunction is closely associated with diseases. Here, the enolase from Drosophila melanogaster (DmENO) was purified and crystallized. A crystal of DmENO diffracted to 2.0 Å resolution and belonged to space group R32. The structure was solved by molecular replacement. Like most enolases, DmENO forms a homodimer with conserved residues in the dimer interface. DmENO possesses an open conformation in this structure and contains conserved elements for catalytic activity. This work provides a structural basis for further functional and evolutionary studies of enolase.

  8. Crystal structure of isomeric boron difluoride acetylnaphtholates

    International Nuclear Information System (INIS)

    Bukvetskij, B.V.; Fedorenko, E.V.; Mirochnik, A.G.; Karasev, V.E.

    2006-01-01

    Crystal structures of luminescent isomeric acetylnaphtholates of boron difluoride are investigated. Full X-ray structural analysis is done at 293 K. Coordinated of atoms, bond angles, bond lengths, interatomic distances are determined. Results of comparative evaluations of the isomers are represented [ru

  9. Crystal structure of levomepromazine maleate

    Directory of Open Access Journals (Sweden)

    Gyula Tamás Gál

    2016-05-01

    Full Text Available The asymmetric unit of the title salt, C19H25N2OS+·C4H3O4− [systematic name: (S-3-(2-methoxyphenothiazin-10-yl-N,N,2-trimethylpropanaminium hydrogen maleate], comprises two (S-levomepromazine cations and two hydrogen maleate anions. The conformations of the two cations are similar. The major difference relates to the orientation of the methoxy substituent at the phenothiazine ring system. The crystal components form a three-dimensional supramolecular network via N—H...O, C—H...O and C—H...π interactions. A comparison of the conformations of the levomepromazine cations with those of the neutral molecule and similar protonated molecules reveals significant conformational flexibility of the phenothiazine ring system and the substituent at the phenothiazine N atom.

  10. Lead sulfide nano crystal preparation and characterization

    International Nuclear Information System (INIS)

    Sasani Ghamsari, M.

    1999-01-01

    Nanometer sized semiconductor particles have attracted much attention duo to their novel electronic and optical optical proportion, originating from quantum confinement. Pb S is one of the most important semiconductor material. In this project Pb S semiconductor nano crystal is synthesized in order to decrease particle size and study the modifications of their optical properties in relation to their size. The synthesis is carried out by using the technique of colloid chemistry. In this method we use lead nitrate extra pure and H2 S gas which is solved in the water. EDTA is used for controlling of particle size. A fast evolution of the optical absorption spectrum will be noticed following synthesis. Immediately after the synthesis reaction. The sample, exhibit a structured absorption spectrum with well defined excitonic peak in 240 nm theoretical relations is that shown this peak belong to 5 A particles. X-ray diffraction is used to establish the identity, phase and the size of these clusters

  11. Phase equilibria in the NaF-CdO-NaPO{sub 3} system at 873 K and crystal structure and physico-chemical characterizations of the new Na{sub 2}CdPO{sub 4}F fluorophosphate

    Energy Technology Data Exchange (ETDEWEB)

    Aboussatar, Mohamed [Université Clermont Auvergne, Université Blaise Pascal, Institut de Chimie de Clermont-Ferrand, UMR 6296 CNRS, BP 10448, F-63000 Clermont-Ferrand (France); Laboratoire de Physico-Chimie de l’État Solide, Faculté des Sciences de Sfax, Université de Sfax, BP 1171, 3000 Sfax (Tunisia); Mbarek, Aïcha [Laboratoire de Chimie Industrielle, Ecole Nationale d’Ingénieurs de Sfax, Université de Sfax, BP W3038, 3000 Sfax (Tunisia); Naili, Houcine [Laboratoire de Physico-Chimie de l’État Solide, Faculté des Sciences de Sfax, Université de Sfax, BP 1171, 3000 Sfax (Tunisia); El-Ghozzi, Malika [Université Clermont Auvergne, Université Blaise Pascal, Institut de Chimie de Clermont-Ferrand, UMR 6296 CNRS, BP 10448, F-63000 Clermont-Ferrand (France); Chadeyron, Geneviève [Université Clermont Auvergne, Institut de Chimie de Clermont-Ferrand, UMR 6296 CNRS/UBP/SIGMA, BP 10448, F-63000 Clermont-Ferrand (France); Avignant, Daniel [Université Clermont Auvergne, Université Blaise Pascal, Institut de Chimie de Clermont-Ferrand, UMR 6296 CNRS, BP 10448, F-63000 Clermont-Ferrand (France); Zambon, Daniel, E-mail: Daniel.Zambon@univ-bpclermont.fr [Université Clermont Auvergne, Université Blaise Pascal, Institut de Chimie de Clermont-Ferrand, UMR 6296 CNRS, BP 10448, F-63000 Clermont-Ferrand (France)

    2017-04-15

    Isothermal sections of the diagram representing phase relationships in the NaF-CdO-NaPO{sub 3} system have been investigated by solid state reactions and powder X-ray diffraction. This phase diagram investigation confirms the polymorphism of the NaCdPO{sub 4} side component and the structure of the ß high temperature polymorph (orthorhombic, space group Pnma and unit cell parameters a=9.3118(2), b=7.0459(1), c=5.1849(1) Å has been refined. A new fluorophosphate, Na{sub 2}CdPO{sub 4}F, has been discovered and its crystal structure determined and refined from powder X-ray diffraction data. It exhibits a new 3D structure with orthorhombic symmetry, space group Pnma and unit cell parameters a=5.3731(1), b=6.8530(1), c=12.2691(2) Å. The structure is closely related to those of the high temperature polymorph of the nacaphite Na{sub 2}CaPO{sub 4}F and the fluorosilicate Ca{sub 2}NaSiO{sub 4}F but differs essentially in the cationic repartition since the structure is fully ordered with one Na site (8d) and one Cd site (4c). Relationships with other Na{sub 2}M{sup II}PO{sub 4}F (M{sup II}=Mg, Ca, Mn, Fe, Co, Ni) have been examined and the crystal-chemical and topographical analysis of these fluorophosphates is briefly reviewed. IR, Raman, optical and {sup 19}F, {sup 23}Na, {sup 31}P MAS NMR characterizations of Na{sub 2}CdPO{sub 4}F have been investigated. - Graphical abstract: The structure of the compound Na{sub 2}CdPO{sub 4}F, discovered during the study of the phase relationships in the NaF-CdO-NaPO{sub 3} system, has been determined and compared with other Na{sub 2}M{sup II}PO{sub 4}F fluorophosphates. - Highlights: • XRD analysis of the isothermal section of the NaF-CdO-NaPO{sub 3} system at 923 K. • Rietveld refinement of the high temperature polymorph β-NaCdPO{sub 4}. • Crystal structure of the new Na{sub 2}CdPO{sub 4}F fluorophosphate determined from powder XRD. • Crystal structure - composition relationships of Na{sub 2}M{sup II}PO{sub 4}F compounds

  12. Crystal structure of rubidium methyldiazotate

    Directory of Open Access Journals (Sweden)

    Tobias Grassl

    2017-02-01

    Full Text Available The title compound, Rb+·H3CN2O−, has been crystallized in liquid ammonia as a reaction product of the reductive ammonolysis of the natural compound streptozocin. Elemental rubidium was used as reduction agent as it is soluble in liquid ammonia, forming a blue solution. Reductive bond cleavage in biogenic materials under kinetically controlled conditions offers a new approach to gain access to sustainably produced raw materials. The anion is nearly planar [dihedral angle O—N—N—C = −0.4 (2°]. The Rb+ cation has a coordination number of seven, and coordinates to five anions. One anion is bound via both its N atoms, one by both O and N, two anions are bound by only their O atoms, and the last is bound via the N atom adjacent to the methyl group. The diazotate anions are bridged by cations and do not exhibit any direct contacts with each other. The cations form corrugated layers that propagate in the (-101 plane.

  13. Alignment structures in ferroelectric liquid crystals

    Energy Technology Data Exchange (ETDEWEB)

    Islam, N.U

    1998-07-01

    Although for many years liquid crystals were of purely scientific interest, they have now become ubiquitous in everyday life. The use of the nematic liquid crystal phase in flat panel display applications has been the main factor in this popularity. However, with the advent of the SuperTwist Nematic (STN) device, the limits to which this phase could be exploited for display applications was perhaps reached. With the discovery by Clark et al. of the Surface Stabilised Ferroelectric Liquid Crystal (SSFLC) configuration, the possibility arose of using chiral smectic liquid crystals to create large area, passively addressed, fast switching, flat panel displays. Unfortunately, the structures that form within smectic liquid crystals, and the dynamics of the switching within these, are still not fully understood. In this thesis we address the former of these, making a detailed the study of the structures that form within tilted smectic liquid crystal devices. We present here the first complete theoretical and experimental study of various different ferroelectric liquid crystal materials, where we employed theoretical models based on a simple set of assumptions to understand the behaviour of a set of increasingly complex experimental systems. We started with the simplest of these, Freely Suspended Smectic Films (FSSFs) and then worked with progressively more realistic systems in the form of homeotropically, and later, homogeneously aligned liquid crystal cells. The equilibrium structures that form get particularly complex in the last case, taking the form of tilted and chevron layering structures. In each of these cases, the predictions of the modelling are compared with our experimental results. Further, we present here the first model of the chevron cusp that seeks to include the effects of biaxiality in the S{sub C} phase. We also present a model that seeks to analyse the stability of the chevron layering structure and its relationship with tilted layers. This includes

  14. Alignment structures in ferroelectric liquid crystals

    International Nuclear Information System (INIS)

    Islam, N.U.

    1998-01-01

    Although for many years liquid crystals were of purely scientific interest, they have now become ubiquitous in everyday life. The use of the nematic liquid crystal phase in flat panel display applications has been the main factor in this popularity. However, with the advent of the SuperTwist Nematic (STN) device, the limits to which this phase could be exploited for display applications was perhaps reached. With the discovery by Clark et al. of the Surface Stabilised Ferroelectric Liquid Crystal (SSFLC) configuration, the possibility arose of using chiral smectic liquid crystals to create large area, passively addressed, fast switching, flat panel displays. Unfortunately, the structures that form within smectic liquid crystals, and the dynamics of the switching within these, are still not fully understood. In this thesis we address the former of these, making a detailed the study of the structures that form within tilted smectic liquid crystal devices. We present here the first complete theoretical and experimental study of various different ferroelectric liquid crystal materials, where we employed theoretical models based on a simple set of assumptions to understand the behaviour of a set of increasingly complex experimental systems. We started with the simplest of these, Freely Suspended Smectic Films (FSSFs) and then worked with progressively more realistic systems in the form of homeotropically, and later, homogeneously aligned liquid crystal cells. The equilibrium structures that form get particularly complex in the last case, taking the form of tilted and chevron layering structures. In each of these cases, the predictions of the modelling are compared with our experimental results. Further, we present here the first model of the chevron cusp that seeks to include the effects of biaxiality in the S C phase. We also present a model that seeks to analyse the stability of the chevron layering structure and its relationship with tilted layers. This includes an

  15. Synthesis, crystal structures, and characterization of double complex salts [Au(en)2][Rh(NO2)6]·2H2O and [Au(en)2][Rh(NO2)6

    Science.gov (United States)

    Plyusnin, Pavel E.; Makotchenko, Evgenia V.; Shubin, Yury V.; Baidina, Iraida A.; Korolkov, Ilya V.; Sheludyakova, Liliya A.; Korenev, Sergey V.

    2015-11-01

    Double complex salts of rhodium(III) and gold(III) of the composition [Au(en)2][Rh(NO2)6]·2H2O (1) and [Au(en)2][Rh(NO2)6] (2) have been prepared. Crystal structures of the compounds have been determined by single crystal X-ray diffraction. The compounds have been characterized by PXRD, IR, far-IR, CHN and DTA. The complexes have a layered structures. The presence of water in 1 makes the structure of the hydrated DCS less dense as compared to the anhydrous one. The environment of the cation and the anion in the two structures is the same, oxygen atoms of the nitro groups are involved in hydrogen bonds N-H⋯O, N⋯O distances being approximately the same. The structures of 1 and 2 are notable in having shortened contacts between the gold atoms and the oxygen atoms of the nitro groups of the neighboring complex anions. The thermal behavior of the complexes in a hydrogen atmosphere was investigated. The final product of thermolysis prepared at the temperature 600°C is a two-phase mixture of pure metallic gold and the solid solution Rh0.93Au0.07.

  16. Crystal structure of clathrates of Hofmann dma-type

    International Nuclear Information System (INIS)

    NIshikiori, Sh.; Ivamoto, T.

    1999-01-01

    Seven new clathrates Cd(DMA) 2 Ni(CN) 4 ·xG (x=1, G=aniline, 2,3-xylidine, 2,4-xylidine, 2,5-xylidine, 2,6-xylidine, 3,5-xylidine, and x=2, G=2,4,6-trimethylaniline) of Hofmann type are synthesized by amine substitution for dimethylamine (DMA). On the base of x-ray diffraction data it is shown that geometry of guest molecule in cage-like hollow determines the structure of the host and crystal structure of clathrates. Two-dimension metallocomplex of the host of studied clathrates is characterized by elastic folded structure appearing as a result of angular deformation of bond between Cd atoms and host cyanide bridge. Guest molecule orientation is fixed by hydrogen bond. Structural elasticity of the host complex directs to differences in crystal structure of clathrates formed and to considerable variety of incorporated guests [ru

  17. Synthesis and crystal structures of three new benzotriazolylpropanamides

    Directory of Open Access Journals (Sweden)

    Donna S. Amenta

    2017-06-01

    Full Text Available The base-catalyzed Michael addition of 2-methylacrylamide to benzotriazole afforded 3-(1H-benzotriazol-1-yl-2-methylpropanamide, C10H12N4O (1, in 32% yield in addition to small amounts of isomeric 3-(2H-benzotriazol-2-yl-2-methylpropanamide, C10H12N4O (2. In a similar manner, 3-(1H-benzotriazol-1-yl-N,N-dimethylpropanamide, C11H14N4O (3, was prepared from benzotriazole and N,N-dimethylacrylamide. All three products have been structurally characterized by single-crystal X-ray diffraction. The crystal structures of 1 and 2 comprise infinite arrays formed by N—H...O and N—H...N bridges, as well as π–π interactions, while the molecules of 3 are aggregated to simple π-dimers in the crystal.

  18. Information and crystal structure estimation

    International Nuclear Information System (INIS)

    Wilkins, S.W.; Commonwealth Scientific and Industrial Research Organization, Clayton; Varghese, J.N.; Steenstrup, S.

    1984-01-01

    The conceptual foundations of a general information-theoretic based approach to X-ray structure estimation are reexamined with a view to clarifying some of the subtleties inherent in the approach and to enhancing the scope of the method. More particularly, general reasons for choosing the minimum of the Shannon-Kullback measure for information as the criterion for inference are discussed and it is shown that the minimum information (or maximum entropy) principle enters the present treatment of the structure estimation problem in at least to quite separate ways, and that three formally similar but conceptually quite different expressions for relative information appear at different points in the theory. One of these is the general Shannon-Kullback expression, while the second is a derived form pertaining only under the restrictive assumptions of the present stochastic model for allowed structures, and the third is a measure of the additional information involved in accepting a fluctuation relative to an arbitrary mean structure. (orig.)

  19. Synthesis, crystal structure, spectroscopic characterization, Hirshfeld surface analysis, and DFT calculations of 1,4-dimethyl-2-oxo-pyrimido[1,2-a]benzimidazole hydrate

    Science.gov (United States)

    El Bakri, Youness; Anouar, El Hassane; Ramli, Youssef; Essassi, El Mokhtar; Mague, Joel T.

    2018-01-01

    Imidazopyrimidine derivatives are organic synthesized compounds with a pyrimido[1,2-a]benzimidazole as basic skeleton. They are known for their various biological properties and as an important class of compounds in medicinal chemistry. A new 1,4-dimethyl-2-oxo-pyrimido[1,2-a]benzimidazole hydrate derivative of the tilted group has been synthesized and characterized by spectroscopic techniques NMR and FT-IR; and by a single crystal X-ray diffraction. The X-ray results showed that the tricyclic core of the title compound, C12H11N3O·H2O, is almost planar. The molecules stack along the a-axis direction in head-to- tail fashion through π-stacking interactions involving all three rings. The stacks are tied together by direct Csbnd H⋯O hydrogen bonds and by Osbnd H⋯O, Osbnd N⋯N and Csbnd H⋯O hydrogen bonds with the lattice water. DFT calculations at B3LYP/6-311++G(d,p) in gas phase an polarizable continuum model have been carried out to predict the spectral and geometrical data of the tilted compound. The obtained results showed relatively good correlations between the predicted and experimental data with correlation coefficients higher than 98%.

  20. Synthesis, NMR characterization, X-ray crystal structure of Co(II) Ni(II) and Cu(II) complexes of a pyridine containing self-assembling

    International Nuclear Information System (INIS)

    Ranjbar, M.; Taghavipour, M.; Moghimi, A.; Aghabozorg, H.

    2002-01-01

    In the recent years, the self-assembling systems have been attracted chemists. The intermolecular bond in such systems mainly consists of ion pairing and hydrogen bonding [1,2]. The reaction between self-assembling system liquid LH 2 (py dc=2,6-pyridinedicarboxylic acid and py da=2,6- pyridine diamin) with cobalt (II) nitrate, nickel (II) chloride, and copper (II) acetate in water leads to the formation of self- assemble coordination complexes, [py da.H] 2 [M(py dc) 2 ]. H 2 O, M=Co(II),Ni(II), and Cu(II). The characterization was performed using elemental analysis, ESI mass spectroscopy, 1 H and 13 C NMR and X-ray crystallography. The crystal systems are monoclinic with space group P2 1 /n and four molecules per unit cell. These complexes shows 13 C NMR resonances of cationic counter ion [(py dc,H)] + in DMSO- d 6 but no signal corresponding to the two coordinated ligands [py dc] 2- The metal atoms are six-coordinated with a distorted octahedral geometry. The two [py de] 2- units are almost perpendicular to each other

  1. Shear induced structures in crystallizing cocoa butter

    Science.gov (United States)

    Mazzanti, Gianfranco; Guthrie, Sarah E.; Sirota, Eric B.; Marangoni, Alejandro G.; Idziak, Stefan H. J.

    2004-03-01

    Cocoa butter is the main structural component of chocolate and many cosmetics. It crystallizes in several polymorphs, called phases I to VI. We used Synchrotron X-ray diffraction to study the effect of shear on its crystallization. A previously unreported phase (phase X) was found and a crystallization path through phase IV under shear was observed. Samples were crystallized under shear from the melt in temperature controlled Couette cells, at final crystallization temperatures of 17.5^oC, 20^oC and 22.5^oC in Beamline X10A of NSLS. The formation of phase X was observed at low shear rates (90 s-1) and low crystallization temperature (17.5^oC), but was absent at high shear (720 s-1) and high temperature (20^oC). The d-spacing and melting point suggest that this new phase is a mixture rich on two of the three major components of cocoa butter. We also found that, contrary to previous reports, the transition from phase II to phase V can happen through the intermediate phase IV, at high shear rates and temperature.

  2. Structure analysis on synthetic emerald crystals

    Science.gov (United States)

    Lee, Pei-Lun; Lee, Jiann-Shing; Huang, Eugene; Liao, Ju-Hsiou

    2013-05-01

    Single crystals of emerald synthesized by means of the flux method were adopted for crystallographic analyses. Emerald crystals with a wide range of Cr3+-doping content up to 3.16 wt% Cr2O3 were examined by X-ray single crystal diffraction refinement method. The crystal structures of the emerald crystals were refined to R 1 (all data) of 0.019-0.024 and w R 2 (all data) of 0.061-0.073. When Cr3+ substitutes for Al3+, the main adjustment takes place in the Al-octahedron and Be-tetrahedron. The effect of substitution of Cr3+ for Al3+ in the beryl structure results in progressively lengthening of the Al-O distance, while the length of the other bonds remains nearly unchanged. The substitution of Cr3+ for Al3+ may have caused the expansion of a axis, while keeping the c axis unchanged in the emerald lattice. As a consequence, the Al-O-Si and Al-O-Be bonding angles are found to decrease, while the angle of Si-O-Be increases as the Al-O distance increases during the Cr replacement.

  3. Synthesis, crystal structure, thermal analysis and dielectric ...

    Indian Academy of Sciences (India)

    [13] Perry C H and Lowdes R P 1969 J. Chem. Phys. 51 3648. [14] Sheldrick G M 1997 SHELXS9, Program for the Refinement of Crystal Structures (Germany: University of Gottingen). [15] Loukil M, Kabadou A, Salles Ph and Ben Salah A 2004 Chem. Phys. 300 247. [16] Rolies M M and De Ranter C J 1978 Acta Crystallogr.

  4. Crystal growth and characterization of Ir-Te compounds

    Energy Technology Data Exchange (ETDEWEB)

    Kurzhals, Philipp; Weber, Frank; Zocco, Diego; Adelmann, Peter; Merz, Michael; Wolf, Thomas; Kuntz, Sebastian; Grube, Kai [Karlsruhe Institute of Technology, Institute for Solid State Physics, Karlsruhe (Germany)

    2016-07-01

    IrTe{sub 2} is distinguished by a structural phase transition whose origin is not understood up to the present day. We grew crystals using the self-flux method starting from the reagents iridium and tellurium and got specimen with varying amounts of IrTe{sub 2} and Ir{sub 3}Te{sub 8}, analyzed by x-ray powder diffraction. We studied the transition near T = 280 K in magnetization measurements down to T = 1.8 K probing also for superconductivity, which was reported for intercalated samples. Results indicate that the structural transition happens over an extended range in temperature and superconductivity is absent in our samples. Ir{sub 3}Te{sub 8} is not studied to such an extent as IrTe{sub 2}. In previous publications a structural phase transition is reported. We characterized the transition by performing magnetization measurements and X-ray diffraction.

  5. Crystal Structure of Human Enterovirus 71

    Energy Technology Data Exchange (ETDEWEB)

    Plevka, Pavel; Perera, Rushika; Cardosa, Jane; Kuhn, Richard J.; Rossmann, Michael G. (Purdue); (Sentinext)

    2013-04-08

    Enterovirus 71 is a picornavirus associated with fatal neurological illness in infants and young children. Here, we report the crystal structure of enterovirus 71 and show that, unlike in other enteroviruses, the 'pocket factor,' a small molecule that stabilizes the virus, is partly exposed on the floor of the 'canyon.' Thus, the structure of antiviral compounds may require a hydrophilic head group designed to interact with residues at the entrance of the pocket.

  6. Modular crystals as modulated structures

    DEFF Research Database (Denmark)

    Elcoro, L.; Perez-Mato, J.M.; Friese, K.

    2008-01-01

    The use of the superspace formalism is extended to the description and refinement of the homologous series of modular structures with two symmetry-related modules with different orientations. The lillianite homologous series has been taken as a study case. Starting from a commensurate modulated...... composite description with two basic subsystems corresponding to the two different modules, it is shown how a more efficient description can be achieved using so-called zigzag modulation functions. These linear zigzag modulations, newly implemented in the program JANA2006, have very large fixed amplitudes...... and introduce in the starting model the two orientations of the underlying module sublattices. We show that a composite approach with this type of function, which treats the cations and anions as two separate subsystems forming a misfit compound, is the most appropriate and robust method for the refinements....

  7. Ruthenium(II) bipyridine complexes bearing quinoline-azoimine (NN'N″) tridentate ligands: synthesis, spectral characterization, electrochemical properties and single-crystal X-ray structure analysis.

    Science.gov (United States)

    Al-Noaimi, Mousa; Abdel-Rahman, Obadah S; Fasfous, Ismail I; El-khateeb, Mohammad; Awwadi, Firas F; Warad, Ismail

    2014-05-05

    Four octahedral ruthenium(II) azoimine-quinoline complexes having the general molecular formula [Ru(II)(L-Y)(bpy)Cl](PF6) {L-Y=YC6H4N=NC(COCH3)=NC9H6N, Y=H (1), CH3 (2), Br (3), NO2 (4) and bpy=2,2'-bipyrdine} were synthesized. The azoimine-quinoline based ligands behave as NN'N″ tridentate donors and coordinated to ruthenium via azo-N', imine-N' and quinolone-N″ nitrogen atoms. The composition of the complexes has been established by elemental analysis, spectral methods (FT-IR, electronic, (1)H NMR, UV/Vis and electrochemical (cyclic voltammetry) techniques. The crystal structure of complex 1 is reported. The Ru(II) oxidation state is greatly stabilized by the novel tridentate ligands, showing Ru(III/II) couples ranging from 0.93-1.27 V vs. Cp2Fe/Cp2Fe(+). The absorption spectrum of 1 in dichloromethane was modeled by time-dependent density functional theory (TD-DFT). Copyright © 2014 Elsevier B.V. All rights reserved.

  8. Growth and characterization of La2CoMnO6 crystals doped with Pb

    International Nuclear Information System (INIS)

    Milenov, T.I.; Rafailov, P.M.; Abrashev, M.V.; Nikolova, R.P.; Nakatsuka, A.; Avdeev, G.V.; Veleva, M.N.; Dobreva, S.; Yankova, L.; Gospodinov, M.M.

    2010-01-01

    Crystals of La 2 CoMnO 6 doped with Pb were grown by the high temperature solution growth method. Several crystals were examined by scanning electron microscopy (SEM), energy-dispersive X-ray analysis (EDAX), X-ray single-crystal diffractometry and polarized Raman spectroscopy. Some variations in the composition of different crystals are observed, however, within the volume of each distinct crystal the composition is found to be fairly constant. Crystals with lateral dimensions larger than 2 mm and thicker than 1 mm contain structural defects as twin lamellae and surface roughness. The results from the characterization of the grown crystals with X-ray diffraction and Raman spectroscopy are consistent with an assumption for a coexistence of an ordered monoclinic and a disordered orthorhombic phase.

  9. Photonic Crystal Laser-Driven Accelerator Structures

    International Nuclear Information System (INIS)

    Cowan, Benjamin M.

    2007-01-01

    Laser-driven acceleration holds great promise for significantly improving accelerating gradient. However, scaling the conventional process of structure-based acceleration in vacuum down to optical wavelengths requires a substantially different kind of structure. We require an optical waveguide that (1) is constructed out of dielectric materials, (2) has transverse size on the order of a wavelength, and (3) supports a mode with speed-of-light phase velocity in vacuum. Photonic crystals---structures whose electromagnetic properties are spatially periodic---can meet these requirements. We discuss simulated photonic crystal accelerator structures and describe their properties. We begin with a class of two-dimensional structures which serves to illustrate the design considerations and trade-offs involved. We then present a three-dimensional structure, and describe its performance in terms of accelerating gradient and efficiency. We discuss particle beam dynamics in this structure, demonstrating a method for keeping a beam confined to the waveguide. We also discuss material and fabrication considerations. Since accelerating gradient is limited by optical damage to the structure, the damage threshold of the dielectric is a critical parameter. We experimentally measure the damage threshold of silicon for picosecond pulses in the infrared, and determine that our structure is capable of sustaining an accelerating gradient of 300 MV/m at 1550 nm. Finally, we discuss possibilities for manufacturing these structures using common microfabrication techniques

  10. Structural templating in a nonplanar phthalocyanine using single crystal copper iodide

    OpenAIRE

    Rochford, L. A. (Luke A.); Ramadan, Alexandra J.; Keeble, Dean S.; Ryan, Mary P.; Heutz, Sandrine; Jones, T. S. (Tim S.)

    2015-01-01

    Solution-grown copper iodide crystals are used as substrates for the templated growth of the nonplanar vanadyl phthalocyanine using organic molecular beam deposition. Structural characterization reveals a single molecular orientation produced by the (111) Miller plane of the copper iodide crystals. These fundamental measurements show the importance of morphology and structure in templating interactions for organic electronics applications.

  11. Growth and characterization of heavily doped silicon crystals

    Energy Technology Data Exchange (ETDEWEB)

    Scala, R.; Porrini, M. [MEMC Electronic Materials SpA, via Nazionale 59, 39012 Merano (Italy); Borionetti, G. [MEMC Electronic Materials SpA, viale Gherzi 31, Novara (Italy)

    2011-08-15

    Silicon crystals grown with the Czochralski method are still the most common material used for the production of electronic devices. In recent years, a growing need of large diameter crystals with increasingly higher doping levels is observed, especially to support the expanding market of discrete devices and its trend towards lower and lower resistivity levels for the silicon substrate. The growth of such heavily doped, large-diameter crystals poses several new challenges to the crystal grower, and the presence of a high dopant concentration in the crystal affects significantly its main properties, requiring also the development of dedicated characterization techniques. This paper illustrates the recent advances in the growth and characterization of silicon crystals heavily doped with antimony, arsenic, phosphorus and boron. (copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  12. Crystal structure of riboflavin synthase

    Energy Technology Data Exchange (ETDEWEB)

    Liao, D.-I.; Wawrzak, Z.; Calabrese, J.C.; Viitanen, P.V.; Jordan, D.B. (DuPont); (NWU)

    2010-03-05

    Riboflavin synthase catalyzes the dismutation of two molecules of 6,7-dimethyl-8-(1'-D-ribityl)-lumazine to yield riboflavin and 4-ribitylamino-5-amino-2,6-dihydroxypyrimidine. The homotrimer of 23 kDa subunits has no cofactor requirements for catalysis. The enzyme is nonexistent in humans and is an attractive target for antimicrobial agents of organisms whose pathogenicity depends on their ability to biosynthesize riboflavin. The first three-dimensional structure of the enzyme was determined at 2.0 {angstrom} resolution using the multiwavelength anomalous diffraction (MAD) method on the Escherichia coli protein containing selenomethionine residues. The homotrimer consists of an asymmetric assembly of monomers, each of which comprises two similar {beta} barrels and a C-terminal {alpha} helix. The similar {beta} barrels within the monomer confirm a prediction of pseudo two-fold symmetry that is inferred from the sequence similarity between the two halves of the protein. The {beta} barrels closely resemble folds found in phthalate dioxygenase reductase and other flavoproteins. The three active sites of the trimer are proposed to lie between pairs of monomers in which residues conserved among species reside, including two Asp-His-Ser triads and dyads of Cys-Ser and His-Thr. The proposed active sites are located where FMN (an analog of riboflavin) is modeled from an overlay of the {beta} barrels of phthalate dioxygenase reductase and riboflavin synthase. In the trimer, one active site is formed, and the other two active sites are wide open and exposed to solvent. The nature of the trimer configuration suggests that only one active site can be formed and be catalytically competent at a time.

  13. Synthesis, characterization, crystal structure, and thermal analysis of 2-chloro-N-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl) acetamide

    Energy Technology Data Exchange (ETDEWEB)

    Sharma, R. [University of Jammu, X-ray Crystallography Laboratory, Post-Graduate Department of Physics & Electronics (India); Nayak, P. S.; Narayana, B. [Mangalore University, Mangalagangotri, Department of Studies in Chemistry (India); Kant, R., E-mail: rkvk.paper11@gmail.com [University of Jammu, X-ray Crystallography Laboratory, Post-Graduate Department of Physics & Electronics (India)

    2015-12-15

    The title compound, C{sub 13}H{sub 14}O{sub 2}N{sub 3}Cl, has been synthesized by the reaction of chloroacetyl chloride with 4-aminoantipyrine in basic media and characterized by FT-IR, CHN elemental analysis, UV-Vis, TGA, DTA, DSC and single crystal X-ray diffraction. crystals are monoclinic, sp. gr. P2{sub 1}/c, a = 6.9994(6), b = 12.4035(13), c = 15.836(2) Å, β = 100.367(9)°, Z = 4. The crystal structure is stabilized by N–H···O and C–H···O interactions, the former interactions result in the formation of dimers corresponding to R{sub 2}{sup 2} (10) graphset motif and the dimers are further connected by C–H···O hydrogen bonding forming chains. In addition, the thermal stability of the compound was determined by TGA, DTA, DSC analysis, and absorption at λ{sub max} = 298 nm was determined by UV-Vis spectrophotometer.

  14. In Vitro Antifungal, Anticancer Activities and POM Analyses of a Novel Bioactive Schiff Base 4-(((E)-furan-2-ylmethylidene)amino)p-henol: Synthesis, Characterization and Crystal Structure

    International Nuclear Information System (INIS)

    Tighadouni, S.; Radi, S.; Sirajuddin, M.; Akkurt, M.; Ozdemir, N.; Mabkhot, Y. N.; Hadda, T. B.

    2016-01-01

    The title compound (1), C/sub 11/H/sub 9/NO/sub 2/, was synthesized and characterized by FT-IR, 1H NMR, /sup 13/C NMR spectroscopy, mass spectrometry and single crystal analysis. It was crystallized in a monoclinic system with a space group P21/n. The dihedral angle between the planes of furan and benzene ring is 21.24 (11)Degree. The torsion angle of bridge C-C-N-C is -177.81(15) Degree. The crystal structure is stabilized by intermolecular hydrogen bonds between O-H-N and C-H-O forming a three dimensional network. The synthesized compound was screened for the in vitro antifungal against the Fusarium oxysporum f.sp albedinis FAO fungal strains and showed good activity. It was also tested for the anticancer activities against breast (MDA-MB231) and colorectal (LOVO) cancer cell lines and exhibited IC50 values of 6.9 μg/mL and 14.6 μg/mL, respectively. POM calculations of molecular properties of 1 are in good agreement with the mode of antifungal action of the compound bearing (XδYδ) pharmacophore site. Also it shows a drug score of 43 percent which is an important parameter for the compound possessing the drug character. (author)

  15. Nonlinear coherent structures in granular crystals

    Science.gov (United States)

    Chong, C.; Porter, Mason A.; Kevrekidis, P. G.; Daraio, C.

    2017-10-01

    The study of granular crystals, which are nonlinear metamaterials that consist of closely packed arrays of particles that interact elastically, is a vibrant area of research that combines ideas from disciplines such as materials science, nonlinear dynamics, and condensed-matter physics. Granular crystals exploit geometrical nonlinearities in their constitutive microstructure to produce properties (such as tunability and energy localization) that are not conventional to engineering materials and linear devices. In this topical review, we focus on recent experimental, computational, and theoretical results on nonlinear coherent structures in granular crystals. Such structures—which include traveling solitary waves, dispersive shock waves, and discrete breathers—have fascinating dynamics, including a diversity of both transient features and robust, long-lived patterns that emerge from broad classes of initial data. In our review, we primarily discuss phenomena in one-dimensional crystals, as most research to date has focused on such scenarios, but we also present some extensions to two-dimensional settings. Throughout the review, we highlight open problems and discuss a variety of potential engineering applications that arise from the rich dynamic response of granular crystals.

  16. The crystal structure and the phase transitions of pyridinium trifluoromethanesulfonate

    International Nuclear Information System (INIS)

    Jesariew, Dominik; Ilczyszyn, Maria M; Pietraszko, Adam

    2014-01-01

    The calorimetric and optical studies and the structural properties of pyridinium trifluoromethanesulfonate (abbreviated as PyHOTf) are reported. A sequence of four fully reversible solid–solid phase transitions, at 223.0, 309.0, 359.9 and 394.3 K, has been discovered. The phase transition sequence was confirmed by x-ray diffraction data. The crystal structures of three phases (V, IV and III) have been determined from the single crystal x-ray diffraction data. Structural properties of the high temperature phases are characterized using powder x-ray diffraction data measured in the 290–425 K temperature range. The structural changes triggered by the temperature change are discussed in relation to the phase transitions. Two low temperature phases (V and IV) belong to the P4 3 2 1 2 space group of the tetragonal system. The intermediate phases (III and II) are monoclinic and the prototype high temperature phase (I) is a pseudo-cubic (tetragonal) one. The low temperature phases (V and IV) are well ordered. The crystal structure of intermediate (III and II) and prototype (I) phases are characterized by high disorder of the pyridinium cations and triflate anions. (papers)

  17. Numerical characterization of nanopillar photonic crystal waveguides and directional couplers

    DEFF Research Database (Denmark)

    Chigrin, Dmitry N.; Lavrinenko, Andrei; Sotomayor Torres, Clivia M.

    2005-01-01

    We numerically characterize a novel type of a photonic crystal waveguide, which consists of several rows of periodically arranged dielectric cylinders. In such a nanopillar photonic crystal waveguide, light confinement is due to the total internal reflection. A nanopillar waveguide is a multimode...

  18. Synthesis and physicochemical characterization of two lead(II) complexes with O-, N-donor ligands. Lone pair functionality and crystal structure

    Science.gov (United States)

    Masternak, Joanna; Barszcz, Barbara; Hodorowicz, Maciej; Khavryuchenko, Oleksiy V.; Majka, Alina

    2015-02-01

    A dinuclear [Pb2(4-CHO-5-MeIm)6(NO3)2](NO3)2 (1) and a polynuclear [Pb(2-pzc)2(H2O)]n (2) complexes (where 5(4)-carbaldehyde-4(5)-methylimidazole (5(4)-CHO-4(5)-MeIm) and pyrazine-2-carboxylic acid (2-pzcH)) have been synthesized and characterized by elemental analysis, IR spectroscopy and X-ray crystallography. Structural determination for complex 1 reveals a cationic species [Pb(4-CHO-5-MeIm)3]2+ connected through bridging nitrate(V) ions. There are also an uncoordinated nitrate ions as counterions. Complex 2 is a three-dimensional architecture consisting of Pb6O12 building units. The pyrazine-2-carboxylato ligand behaves as a chelating agent and a bi-connective bridge. The coordination polyhedra around lead(II) ion could be described as a distorted docecahedron (1) or monocapped trigonal prism (2). The luminescent properties of 1 and 2 investigated in the solid state at room temperature indicate structure-dependent photoluminescent properties. The DFT calculations and the X-ray structural data point on rather hemidirected type of coordination around Pb(II) ions of 1 and 2.

  19. Solving crystal structures from neutron diffraction data

    International Nuclear Information System (INIS)

    Wilson, C.C.

    1987-07-01

    In order to pursue crystal structure determination using neutron diffraction data, and given the wide experience available of solving structures using X-ray data, the codes used in X-ray structural analysis should be adapted to the different requirements of a neutron experiment. Modifications have been made to a direct methods program MITHRIL and to a Patterson methods program PATMET to incorporate into these the features of neutron rather than X-ray diffraction. While to date these modifications have been fairly straightforward and many sophistications remain to be exploited, results obtained from the neutron versions of both programs are promising. (author)

  20. Crystal structure of tris(hydroxylammonium orthophosphate

    Directory of Open Access Journals (Sweden)

    Malte Leinemann

    2015-11-01

    Full Text Available The crystal structure of the title salt, ([H3NOH]+3·[PO4]3−, consists of discrete hydroxylammonium cations and orthophosphate anions. The atoms of the cation occupy general positions, whereas the anion is located on a threefold rotation axis that runs through the phosphorus atom and one of the phosphate O atoms. In the crystal structure, cations and anions are linked by intermolecular O—H...O and N—H...O hydrogen bonds into a three-dimensional network. Altogether, one very strong O—H...O, two N—H...O hydrogen bonds of medium strength and two weaker bifurcated N—H...O interactions are observed.

  1. CCDC 1416891: Experimental Crystal Structure Determination : Methyl-triphenyl-germanium

    KAUST Repository

    Bernatowicz, Piotr; Shkurenko, Aleksander; Osior, Agnieszka; Kamieński, Bohdan; Szymański, Sławomir

    2015-01-01

    An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from

  2. Optically induced structural phase transitions in ion Coulomb crystals

    DEFF Research Database (Denmark)

    Horak, Peter; Dantan, Aurelien Romain; Drewsen, Michael

    2012-01-01

    We investigate numerically the structural dynamics of ion Coulomb crystals confined in a three-dimensional harmonic trap when influenced by an additional one-dimensional optically induced periodical potential. We demonstrate that transitions between thermally excited crystal structures, such as b......We investigate numerically the structural dynamics of ion Coulomb crystals confined in a three-dimensional harmonic trap when influenced by an additional one-dimensional optically induced periodical potential. We demonstrate that transitions between thermally excited crystal structures...

  3. Synthesis and crystal structure analysis of uranyl triple acetates

    Energy Technology Data Exchange (ETDEWEB)

    Klepov, Vladislav V., E-mail: vladislavklepov@gmail.com [Institute for Energy and Climate Research (IEK-6), Forschungszentrum Jülich GmbH, 52428 Jülich (Germany); Department of Chemistry, Samara National Research University, 443086 Samara (Russian Federation); Serezhkina, Larisa B.; Serezhkin, Victor N. [Department of Chemistry, Samara National Research University, 443086 Samara (Russian Federation); Alekseev, Evgeny V., E-mail: e.alekseev@fz-juelich.de [Institute for Energy and Climate Research (IEK-6), Forschungszentrum Jülich GmbH, 52428 Jülich (Germany); Institut für Kristallographie, RWTH Aachen University, 52066 Aachen (Germany)

    2016-12-15

    Single crystals of triple acetates NaR[UO{sub 2}(CH{sub 3}COO){sub 3}]{sub 3}·6H{sub 2}O (R=Mg, Co, Ni, Zn), well-known for their use as reagents for sodium determination, were grown from aqueous solutions and their structural and spectroscopic properties were studied. Crystal structures of the mentioned phases are based upon (Na[UO{sub 2}(CH{sub 3}COO){sub 3}]{sub 3}){sup 2–} clusters and [R(H{sub 2}O){sub 6}]{sup 2+} aqua-complexes. The cooling of a single crystal of NaMg[UO{sub 2}(CH{sub 3}COO){sub 3}]{sub 3}·6H{sub 2}O from 300 to 100 K leads to a phase transition from trigonal to monoclinic crystal system. Intermolecular interactions between the structural units and their mutual packing were studied and compared from the point of view of the stereoatomic model of crystal structures based on Voronoi-Dirichlet tessellation. Using this method we compared the crystal structures of the triple acetates with Na[UO{sub 2}(CH{sub 3}COO){sub 3}] and [R(H{sub 2}O){sub 6}][UO{sub 2}(CH{sub 3}COO){sub 3}]{sub 2} and proposed reasons of triple acetates stability. Infrared and Raman spectra were collected and their bands were assigned. - Graphical abstract: Single crystals of uranium based triple acetates, analytical reagents for sodium determination, were synthesized and structurally, spectroscopically and topologically characterized. The structures were compared with the structures of compounds from preceding families [M(H{sub 2}O){sub 6})][UO{sub 2}(CH{sub 3}COO){sub 3}]{sub 2} (M = Mg, Co, Ni, Zn) and Na[UO{sub 2}(CH{sub 3}COO){sub 3}]. Analysis was performed with the method of molecular Voronoi-Dirichlet polyhedra to reveal a large contribution of the hydrogen bonds into intermolecular interactions which can be a reason of low solubility of studied complexes.

  4. Negative refraction angular characterization in one-dimensional photonic crystals.

    Directory of Open Access Journals (Sweden)

    Jesus Eduardo Lugo

    2011-04-01

    Full Text Available Photonic crystals are artificial structures that have periodic dielectric components with different refractive indices. Under certain conditions, they abnormally refract the light, a phenomenon called negative refraction. Here we experimentally characterize negative refraction in a one dimensional photonic crystal structure; near the low frequency edge of the fourth photonic bandgap. We compare the experimental results with current theory and a theory based on the group velocity developed here. We also analytically derived the negative refraction correctness condition that gives the angular region where negative refraction occurs.By using standard photonic techniques we experimentally determined the relationship between incidence and negative refraction angles and found the negative refraction range by applying the correctness condition. In order to compare both theories with experimental results an output refraction correction was utilized. The correction uses Snell's law and an effective refractive index based on two effective dielectric constants. We found good agreement between experiment and both theories in the negative refraction zone.Since both theories and the experimental observations agreed well in the negative refraction region, we can use both negative refraction theories plus the output correction to predict negative refraction angles. This can be very useful from a practical point of view for space filtering applications such as a photonic demultiplexer or for sensing applications.

  5. Negative refraction angular characterization in one-dimensional photonic crystals.

    Science.gov (United States)

    Lugo, Jesus Eduardo; Doti, Rafael; Faubert, Jocelyn

    2011-04-06

    Photonic crystals are artificial structures that have periodic dielectric components with different refractive indices. Under certain conditions, they abnormally refract the light, a phenomenon called negative refraction. Here we experimentally characterize negative refraction in a one dimensional photonic crystal structure; near the low frequency edge of the fourth photonic bandgap. We compare the experimental results with current theory and a theory based on the group velocity developed here. We also analytically derived the negative refraction correctness condition that gives the angular region where negative refraction occurs. By using standard photonic techniques we experimentally determined the relationship between incidence and negative refraction angles and found the negative refraction range by applying the correctness condition. In order to compare both theories with experimental results an output refraction correction was utilized. The correction uses Snell's law and an effective refractive index based on two effective dielectric constants. We found good agreement between experiment and both theories in the negative refraction zone. Since both theories and the experimental observations agreed well in the negative refraction region, we can use both negative refraction theories plus the output correction to predict negative refraction angles. This can be very useful from a practical point of view for space filtering applications such as a photonic demultiplexer or for sensing applications.

  6. Crystal structure, characterization and thermoelectric properties of the type-I clathrate Ba8-ySryAl14Si32 (0.6≤y≤1.3) prepared by aluminum flux

    International Nuclear Information System (INIS)

    Roudebush, John H.; Toberer, Eric S.; Hope, Hakon; Jeffrey Snyder, G.; Kauzlarich, Susan M.

    2011-01-01

    The title compound was prepared as single crystals using an aluminum flux technique. Single crystal and powder X-ray diffraction indicate that this composition crystallizes in the clathrate type-I structure, space group Pm3-bar n. Electron microprobe characterization indicates the composition to be Ba 8-y Sr y Al 14.2(2) Si 31.8(2) (0.77 1 =0.0233, wR 2 =0.0441) on a crystal of compositions Ba. The Sr atom preferentially occupies the 2a position; mixed Al/Si occupancy was found on all framework sites. These refinements are consistent with a fully occupied framework and nearly fully occupied cation guest sites as found by microprobe analysis. Temperature dependent electrical resistivity and thermal conductivity have been measured from room temperature to 1200 K on a hot-pressed pellet. Electrical resistivity reveals metallic behavior. The negative Seebeck coefficient indicates transport processes dominated by electrons as carriers. Thermal conductivity is between 22 and 25 mW/cm K. The sample shows n-type conductivity with a maximum figure of merit, zT of 0.3 at 1200 K. A single parabolic band model predicts a five-fold increase in zT at 800 K if carrier concentration is lowered. -- Graphical abstract: The inorganic type-I clathrate phase with nominal composition Ba 7 Sr 1 Al 14 Si 32 has been prepared by Al flux. Single crystal diffraction at 90 and 12 K reveal that the framework is fully occupied with the cation sites nearly fully occupied. The lattice thermal conductivity is low thereby suggesting further optimization of the carrier concentration will lead to a high zT. Display Omitted Highlights: → Ba 7 Sr 1 Al 14 Si 32 is a light element phase ideal for thermoelectric power generation. → Ba 7 Sr 1 Al 14 Si 32 is a high melting point cubic structure ideal for efficient power generation. → The framework is fully occupied with the cation sites nearly fully occupied. → Further optimization of the carrier concentration is expected to lead to a high zT.

  7. Structural and optical properties of WTe2 single crystals synthesized by DVT technique

    Science.gov (United States)

    Dixit, Vijay; Vyas, Chirag; Pathak, V. M.; Soalanki, G. K.; Patel, K. D.

    2018-05-01

    Layered transition metal di-chalcogenide (LTMDCs) crystals have attracted much attention due to their potential in optoelectronic device applications recently due to realization of their monolayer based structures. In the present investigation we report growth of WTe2 single crystals by direct vapor transport (DVT) technique. These crystals are then characterized by energy dispersive analysis of x-rays (EDAX) to study stoichiometric composition after growth. The structural properties are studied by x-ray diffraction (XRD) and selected area electron diffraction (SAED) is used to confirm orthorhombic structure of grown WTe2 crystal. Surface morphological properties of the crystals are also studied by scanning electron microscope (SEM). The optical properties of the grown crystals are studied by UV-Visible spectroscopy which gives direct band gap of 1.44 eV for grown WTe2 single crystals.

  8. Prediction and theoretical characterization of p-type organic semiconductor crystals for field-effect transistor applications.

    Science.gov (United States)

    Atahan-Evrenk, Sule; Aspuru-Guzik, Alán

    2014-01-01

    The theoretical prediction and characterization of the solid-state structure of organic semiconductors has tremendous potential for the discovery of new high performance materials. To date, the theoretical analysis mostly relied on the availability of crystal structures obtained through X-ray diffraction. However, the theoretical prediction of the crystal structures of organic semiconductor molecules remains a challenge. This review highlights some of the recent advances in the determination of structure-property relationships of the known organic semiconductor single-crystals and summarizes a few available studies on the prediction of the crystal structures of p-type organic semiconductors for transistor applications.

  9. Characterization of Crystals for Steering of Protons through Channelling in Hadronic Accelerators

    CERN Document Server

    Guidi, V; Boscolo-Marchi, E; Carnera, A; Chesnokov, Yu A; Della Mea, G; De Salvador, D; Fiorini, M; Ivanov, Y M; Martinelli, G; Mazzolari, A; Milan, E; Milan, R; Sambo, A; Scandale, Walter; Todros, S; Vomiero, A

    2006-01-01

    Channeling of relativistic particles through a crystal may be useful for many applications in accelerators, and particularly for collimation in hadronic colliders. Efficiency proved to be dependent on the state of the crystal surface and hence on the method used for preparation. We investigated the morphology and structure of the surface of the samples that have been used in accelerators with high efficiency. We found that crystal fabrication by only mechanical methods (dicing, lapping, and others) leads to a superficial damaged layer, which is correlated to performance limitation in accelerators. A planar chemical etching was studied and applied in order to remove the superficial damaged layer. RBS channeling analysis with low-energy protons and 4He+ highlighted better crystal perfection at surface, as a result of the etching. A protocol for preparation and characterization of crystal for channelling has been developed, which may be of interest for reliable operation with crystals in accelerators.

  10. Crystal structure of natural phaeosphaeride A

    Directory of Open Access Journals (Sweden)

    Victoria V. Abzianidze

    2015-08-01

    Full Text Available The asymmetric unit of the title compound, C15H23NO5, contains two independent molecules. Phaeosphaeride A contains two primary sections, an alkyl chain consisting of five C atoms and a cyclic system consisting of fused five- and six-membered rings with attached substituents. In the crystal, the molecules form layered structures. Nearly planar sheets, parallel to the (001 plane, form bilayers of two-dimensional hydrogen-bonded networks with the hydroxy groups located on the interior of the bilayer sheets. The network is constructed primarily of four O—H...O hydrogen bonds, which form a zigzag pattern in the (001 plane. The butyl chains interdigitate with the butyl chains on adjacent sheets. The crystal was twinned by a twofold rotation about the c axis, with refined major–minor occupancy fractions of 0.718 (6:0.282 (6.

  11. Synthesis and characterization of liquid crystals and their thermoset films

    International Nuclear Information System (INIS)

    Ahn, Yong-Ho; Jung, Myung-Sup; Chang, Jin-Hae

    2010-01-01

    We prepared a series of aromatic liquid crystals (LCs) based on aromatic ester units with the reactive end groups methyl-maleimide and nadimide, and the resulting LCs were thermally cross-linked to produce liquid crystalline thermoset (LCT) films by means of solution-casting and heat treatment. The synthesized LCs and LCTs were characterized with Fourier transform infrared (FT-IR) spectroscopy, 1 H nuclear magnetic resonance (NMR), differential scanning calorimetry (DSC), thermomechanical analysis (TMA), and polarizing optical microscopy with a hot stage. We found that all these LCs form nematic phases. The coefficients of thermal expansion (CTEs) of the LCT films are strongly affected by the reactive end group and the mesogen units in their main-chain structures. The methyl-maleimide-terminated biphenyl LCT was found to have the lowest CTE.

  12. Crystal structure of Cryptosporidium parvum pyruvate kinase.

    Directory of Open Access Journals (Sweden)

    William J Cook

    Full Text Available Pyruvate kinase plays a critical role in cellular metabolism of glucose by serving as a major regulator of glycolysis. This tetrameric enzyme is allosterically regulated by different effector molecules, mainly phosphosugars. In response to binding of effector molecules and substrates, significant structural changes have been identified in various pyruvate kinase structures. Pyruvate kinase of Cryptosporidium parvum is exceptional among known enzymes of protozoan origin in that it exhibits no allosteric property in the presence of commonly known effector molecules. The crystal structure of pyruvate kinase from C. parvum has been solved by molecular replacement techniques and refined to 2.5 Å resolution. In the active site a glycerol molecule is located near the γ-phosphate site of ATP, and the protein structure displays a partially closed active site. However, unlike other structures where the active site is closed, the α6' helix in C. parvum pyruvate kinase unwinds and assumes an extended conformation. In the crystal structure a sulfate ion is found at a site that is occupied by a phosphate of the effector molecule in many pyruvate kinase structures. A new feature of the C. parvum pyruvate kinase structure is the presence of a disulfide bond cross-linking the two monomers in the asymmetric unit. The disulfide bond is formed between cysteine residue 26 in the short N-helix of one monomer with cysteine residue 312 in a long helix (residues 303-320 of the second monomer at the interface of these monomers. Both cysteine residues are unique to C. parvum, and the disulfide bond remained intact in a reduced environment. However, the significance of this bond, if any, remains unknown at this time.

  13. One dimensional coordination polymers: Synthesis, crystal structures and spectroscopic properties

    Science.gov (United States)

    Karaağaç, Dursun; Kürkçüoğlu, Güneş Süheyla; Şenyel, Mustafa; Şahin, Onur

    2016-11-01

    Two new one dimensional (1D) cyanide complexes, namely [M(4-aepy)2(H2O)2][Pt(CN)4], (4-aepy = 4-(2-aminoethyl)pyridine M = Cu(II) (1) or Zn(II) (2)), have been synthesized and characterized by vibrational (FT-IR and Raman) spectroscopy, single crystal X-ray diffraction, thermal and elemental analyses techniques. The crystallographic analyses reveal that 1 and 2 are isomorphous and isostructural, and crystallize in the monoclinic system and C2 space group. The Pt(II) ions are coordinated by four cyanide-carbon atoms in the square-planar geometry and the [Pt(CN)4]2- ions act as a counter ion. The M(II) ions display an N4O2 coordination sphere with a distorted octahedral geometry, the nitrogen donors belonging to four molecules of the organic 4-aepy that act as unidentate ligands and two oxygen atoms from aqua ligands. The crystal structures of 1 and 2 are similar each other and linked via intermolecular hydrogen bonding, Pt⋯π interactions to form 3D supramolecular network. Vibration assignments of all the observed bands are given and the spectral features also supported to the crystal structures of the complexes.

  14. Crystal structure of MboIIA methyltransferase.

    Science.gov (United States)

    Osipiuk, Jerzy; Walsh, Martin A; Joachimiak, Andrzej

    2003-09-15

    DNA methyltransferases (MTases) are sequence-specific enzymes which transfer a methyl group from S-adenosyl-L-methionine (AdoMet) to the amino group of either cytosine or adenine within a recognized DNA sequence. Methylation of a base in a specific DNA sequence protects DNA from nucleolytic cleavage by restriction enzymes recognizing the same DNA sequence. We have determined at 1.74 A resolution the crystal structure of a beta-class DNA MTase MboIIA (M.MboIIA) from the bacterium Moraxella bovis, the smallest DNA MTase determined to date. M.MboIIA methylates the 3' adenine of the pentanucleotide sequence 5'-GAAGA-3'. The protein crystallizes with two molecules in the asymmetric unit which we propose to resemble the dimer when M.MboIIA is not bound to DNA. The overall structure of the enzyme closely resembles that of M.RsrI. However, the cofactor-binding pocket in M.MboIIA forms a closed structure which is in contrast to the open-form structures of other known MTases.

  15. Crystal Structure of the 30S Ribosomal Subunit from Thermus Thermophilus: Purification, Crystallization and Structure Determination

    International Nuclear Information System (INIS)

    Clemons, William M. Jr.; Brodersen, Ditlev E.; McCutcheonn, John P.; May, Joanna L.C.; Carter, Andrew P.; Morgan-Warren, Robert J.; Wimberly, Brian T.; Ramakrishnan, Venki

    2001-01-01

    We describe the crystallization and structure determination of the 30 S ribosomal subunit from Thermus thermophilus. Previous reports of crystals that diffracted to 10 (angstrom) resolution were used as a starting point to improve the quality of the diffraction. Eventually, ideas such as the addition of substrates or factors to eliminate conformational heterogeneity proved less important than attention to detail in yielding crystals that diffracted beyond 3 (angstrom) resolution. Despite improvements in technology and methodology in the last decade, the structure determination of the 30 S subunit presented some very challenging technical problems because of the size of the asymmetric unit, crystal variability and sensitivity to radiation damage. Some steps that were useful for determination of the atomic structure were: the use of anomalous scattering from the LIII edges of osmium and lutetium to obtain the necessary phasing signal; the use of tunable, third-generation synchrotron sources to obtain data of reasonable quality at high resolution; collection of derivative data precisely about a mirror plane to preserve small anomalous differences between Bijvoet mates despite extensive radiation damage and multi-crystal scaling; the pre-screening of crystals to ensure quality, isomorphism and the efficient use of scarce third-generation synchrotron time; pre-incubation of crystals in cobalt hexaammine to ensure isomorphism with other derivatives; and finally, the placement of proteins whose structures had been previously solved in isolation, in conjunction with biochemical data on protein-RNA interactions, to map out the architecture of the 30 S subunit prior to the construction of a detailed atomic-resolution model.

  16. Synthesis and spectral characterization of mono- and binuclear copper(II) complexes derived from 2-benzoylpyridine-N4-methyl-3-thiosemicarbazone: Crystal structure of a novel sulfur bridged copper(II) box-dimer

    Science.gov (United States)

    Jayakumar, K.; Sithambaresan, M.; Aiswarya, N.; Kurup, M. R. Prathapachandra

    2015-03-01

    Mononuclear and binuclear copper(II) complexes of 2-benzoylpyridine-N4-methyl thiosemicarbazone (HL) were prepared and characterized by a variety of spectroscopic techniques. Structural evidence for the novel sulfur bridged copper(II) iodo binuclear complex is obtained by single crystal X-ray diffraction analysis. The complex [Cu2L2I2], a non-centrosymmetric box dimer, crystallizes in monoclinic C2/c space group and it was found to have distorted square pyramidal geometry (Addison parameter, τ = 0.238) with the square basal plane occupied by the thiosemicarbazone moiety and iodine atom whereas the sulfur atom from the other coordinated thiosemicarbazone moiety occupies the apical position. This is the first crystallographically studied system having non-centrosymmetrical entities bridged via thiolate S atoms with Cu(II)sbnd I bond. The tridentate thiosemicarbazone coordinates in mono deprotonated thionic tautomeric form in all complexes except in sulfato complex, [Cu(HL)(SO4)]·H2O (1) where it binds to the metal centre in neutral form. The magnetic moment values and the EPR spectral studies reflect the binuclearity of some of the complexes. The spin Hamiltonian and bonding parameters are calculated based on EPR studies. In all the complexes g|| > g⊥ > 2.0023 and the g values in frozen DMF are consistent with the dx2-y2 ground state. The thermal stabilities of some of the complexes were also determined.

  17. Synthesis and spectral characterization of mono- and binuclear copper(II) complexes derived from 2-benzoylpyridine-N⁴-methyl-3-thiosemicarbazone: crystal structure of a novel sulfur bridged copper(II) box-dimer.

    Science.gov (United States)

    Jayakumar, K; Sithambaresan, M; Aiswarya, N; Kurup, M R Prathapachandra

    2015-03-15

    Mononuclear and binuclear copper(II) complexes of 2-benzoylpyridine-N(4)-methyl thiosemicarbazone (HL) were prepared and characterized by a variety of spectroscopic techniques. Structural evidence for the novel sulfur bridged copper(II) iodo binuclear complex is obtained by single crystal X-ray diffraction analysis. The complex [Cu2L2I2], a non-centrosymmetric box dimer, crystallizes in monoclinic C2/c space group and it was found to have distorted square pyramidal geometry (Addison parameter, τ=0.238) with the square basal plane occupied by the thiosemicarbazone moiety and iodine atom whereas the sulfur atom from the other coordinated thiosemicarbazone moiety occupies the apical position. This is the first crystallographically studied system having non-centrosymmetrical entities bridged via thiolate S atoms with Cu(II)I bond. The tridentate thiosemicarbazone coordinates in mono deprotonated thionic tautomeric form in all complexes except in sulfato complex, [Cu(HL)(SO4)]·H2O (1) where it binds to the metal centre in neutral form. The magnetic moment values and the EPR spectral studies reflect the binuclearity of some of the complexes. The spin Hamiltonian and bonding parameters are calculated based on EPR studies. In all the complexes g||>g⊥>2.0023 and the g values in frozen DMF are consistent with the d(x2-y2) ground state. The thermal stabilities of some of the complexes were also determined. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. Accuracy of crystal structure error estimates

    International Nuclear Information System (INIS)

    Taylor, R.; Kennard, O.

    1986-01-01

    A statistical analysis of 100 crystal structures retrieved from the Cambridge Structural Database is reported. Each structure has been determined independently by two different research groups. Comparison of the independent results leads to the following conclusions: (a) The e.s.d.'s of non-hydrogen-atom positional parameters are almost invariably too small. Typically, they are underestimated by a factor of 1.4-1.45. (b) The extent to which e.s.d.'s are underestimated varies significantly from structure to structure and from atom to atom within a structure. (c) Errors in the positional parameters of atoms belonging to the same chemical residue tend to be positively correlated. (d) The e.s.d.'s of heavy-atom positions are less reliable than those of light-atom positions. (e) Experimental errors in atomic positional parameters are normally, or approximately normally, distributed. (f) The e.s.d.'s of cell parameters are grossly underestimated, by an average factor of about 5 for cell lengths and 2.5 for cell angles. There is marginal evidence that the accuracy of atomic-coordinate e.s.d.'s also depends on diffractometer geometry, refinement procedure, whether or not the structure has a centre of symmetry, and the degree of precision attained in the structure determination. (orig.)

  19. The Crystal Structures of Potentially Tautomeric Compounds

    Science.gov (United States)

    Furmanova, Nina G.

    1981-08-01

    Data on the structures of potentially proto-, metallo-, and carbono-tropic compounds, obtained mainly by X-ray diffraction, are surveyed. The results of neutron and electron diffraction studies have also been partly used. It is shown that a characteristic feature of all the systems considered is the formation of hydrogen or secondary bonds ensuring the contribution of both possible tautomeric forms to the structure. Systematic consideration of the experimental data leads to the conclusion that there is a close relation between the crystal structure and the dynamic behaviour of the molecules in solution and that secondary and hydrogen bonds play a significant role in the tautomeric transition. The bibliography includes 152 references.

  20. Novel Crystal Structure C60 Nanowire

    Science.gov (United States)

    Mickelson, William; Aloni, Shaul; Han, Weiqiang; Cumings, John; Zettl, Alex

    2003-03-01

    We have created insulated C60 nanowire by packing C60 molecules into the interior of insulating boron nitride (BN) nanotubes. For small-diameter BN tubes, the wire consists of a linear chain of C60's. With increasing BN tube inner diameter, novel C60 stacking configurations are obtained (including helical, hollow core, and incommensurate) which are unknown for bulk or thin film forms of C60. C60 in BN nanotubes presents a model system for studying the properties of new dimensionally-constrained "silo" crystal structures.

  1. Crystal structure of MboIIA methyltransferase

    OpenAIRE

    Osipiuk, Jerzy; Walsh, Martin A.; Joachimiak, Andrzej

    2003-01-01

    DNA methyltransferases (MTases) are sequence-specific enzymes which transfer a methyl group from S-adenosyl-l-methionine (AdoMet) to the amino group of either cytosine or adenine within a recognized DNA sequence. Methylation of a base in a specific DNA sequence protects DNA from nucleolytic cleavage by restriction enzymes recognizing the same DNA sequence. We have determined at 1.74 Å resolution the crystal structure of a β-class DNA MTase MboIIA (M·MboIIA) from the bacterium Moraxella bovis,...

  2. Characterization of pure and copper-doped iron tartrate crystals

    Indian Academy of Sciences (India)

    Single crystal growth of pure and copper-doped iron tartrate crystals bearing composition Cu Fe(1−) C4H4O6 · H2O, where = 0, 0.07, 0.06, 0.05, 0.04, 0.03, is achieved using gel technique. The elemental analysis has been done using energy-dispersive X-ray analysis (EDAX) spectrum. The characterization studies ...

  3. Crystal and molecular structure of 2-thiouridine

    Energy Technology Data Exchange (ETDEWEB)

    Hawkinson, S W

    1977-01-01

    The ''minor'' nucleoside 2-thiouridine, C/sub 9/H/sub 12/O/sub 5/N/sub 2/S, crystallizes in a monoclinic cell, space group P2/sub 1/ with a = 5.049 (2), b = 7.526 (2), c = 14.050 (3) A, ..beta.. = 90.17 (2)/sup 0/, and d = 1.619 g cm/sup -3/ (for Z = 2) at 22 +- 2/sup 0/C. The structure was derived from 1334 unique intensities measured with an Oak Ridge computer-controlled diffractometer to a limit of sin theta/lambda = 0.65 A/sup -1/ with Nb-filtered Mo K..cap alpha.. radiation. Atomic parameters were obtained by a combination of Patterson and Fourier techniques and refined by full-matrix least squares to a final R(F) value of 0.023 for all data. The bond lengths and angles in the molecule agree well with those of other thiopyrimidines (C(2) - S = 1.677 A). The conformation of the sugar ring relative to the base is anti with a torsion angle chi(O(1')--C(1') ..-->.. N(1)--C(6)) of 17/sup 0/. The sugar exists in the 3'-endo conformation. The O(5')--C(5') bond is gauche to C(4) - O(1') and trans to C(4')--C(3') (torsion angles of 74 and -169/sup 0/ respectively). The molecules are linked together in the crystal by hydrogen bonds in an intricate network which is identical to that inferred by Kojic-Prodic, Liminga, Sljukic and Ruzic-Toros (Acta Cryst. (1974), B30, 1550-1555) for the crystal structure of 5,6-dihydro-2-thiouridine. 2 figures; 6 tables.

  4. Synthesis, FT–IR characterization and crystal structure of aqua(5,10,15,20-tetraphenylporphyrinato-κ4Nmanganese(III trifluoromethanesulfonate

    Directory of Open Access Journals (Sweden)

    Wafa Harhouri

    2016-05-01

    Full Text Available In the title salt, [Mn(C44H28N4(H2O](CF3SO3 or [MnIII(TPP(H2O](CF3SO3 (where TPP is the dianion of 5,10,15,20-tetraphenylporphyrin, the MnIII cation is chelated by the four pyrrole N atoms of the porphyrinate anion and additionally coordinated by an aqua ligand in an apical site, completing the distorted square-pyramidal coordination environment. The average Mn—N(pyrrole bond length is 1.998 (9 Å and the Mn—O(aqua bond length is 2.1057 (15 Å. The central MnIII ion is displaced by 0.1575 (5 Å from the N4C20 mean plane of the porphyrinate anion towards the apical aqua ligand. The porphyrinate macrocycle exhibits a moderate ruffling and strong saddle deformations. In the crystal lattice, the [MnIII(TPP(H2O]+ cation and the trifluoromethanesulfonate counter-ions are arranged in alternating planes packed along [001]. The components are linked together through O—H...O hydrogen bonds and much weaker C—H...O and C—H...F interactions. The crystal packing is further stabilized by weak C—H...π interactions involving the pyrrole and phenyl rings of the porphyrin moieties.

  5. Syntheses and Crystal Structures of Ferrocenoindenes

    Directory of Open Access Journals (Sweden)

    Gerhard Laus

    2013-02-01

    Full Text Available Ferrocenoindenes display planar chirality and thus represent valuable ligands for asymmetric catalysis. Here, we report on the synthesis of novel 3-(1,1-dibromomethyleneferroceno[1,2-a]indene, (Z-3-(1-bromomethylene-6-iodoferroceno[1,2-a]indene, and benzo[5,6-f]ferroceno[2,3,a]inden-1-one. Any application-oriented design of chiral catalysts requires fundamental knowledge about the ligands involved, not only in terms of atom-connectivity, but also in terms of their three-dimensional structure and steric demand. Therefore, the crystal structures of 2-ferrocenylbenzoic acid, ferroceno[1,2-a]indene, and (Z-3-(1-bromomethylene-6-iodoferroceno[1,2-a]indene have been determined. The bond-lengths that can be retrieved therefrom also allow for an estimation of the reactivity of the aryl-iodo, bromo-methylidene and dibromomethylidene moieties.

  6. The crystal structure of scandium dyhydrate triglycolate

    International Nuclear Information System (INIS)

    Dukareva, L.M.; Antishkina, A.S.; Porai-Koshits, M.A.; Ostrikova, V.N.; Arkhangel'skij, I.V.; Amanov, A.Z.

    1978-01-01

    The structure of colorless crystals of scandium glycolate dehydrate Sc(CH 2 OHCOO) 3 x2H 2 O, synthesized at the chemical department of MSU has been investigated. Parameters of the monoclinic lattice are determined according to roentgenograms of swing and Kforograms and are specified using the DRON-1 diffractor: a=14.624-+0.005 A; b=13.052-+0.003 A; c=5.730+-0.003 A; γ=96.26 deg+-0.01 deg; rhosub(exper.)=1.09 g/cm 3 ; Z=4; Sp.=P 2/b. Experimental photographic data are obtained using the KFOR chamber. Scannings of the layer lines h anti Ko-h anti K4, containing 742 independent reflexes are taken. Deciphering of the structure is carried out by means of analysis of the Paterson functions distribution and conventional and differential electron densities. Description of the system is presented

  7. Structure, thermodynamics, and crystallization of amorphous hafnia

    International Nuclear Information System (INIS)

    Luo, Xuhui; Demkov, Alexander A.

    2015-01-01

    We investigate theoretically amorphous hafnia using the first principles melt and quench method. We identify two types of amorphous structures of hafnia. Type I and type II are related to tetragonal and monoclinic hafnia, respectively. We find type II structure to show stronger disorder than type I. Using the phonon density of states, we calculate the specific heat capacity for type II amorphous hafnia. Using the nudged elastic band method, we show that the averaged transition barrier between the type II amorphous hafnia and monoclinic phase is approximately 0.09 eV/HfO 2 . The crystallization temperature is estimated to be 421 K. The calculations suggest an explanation for the low thermal stability of amorphous hafnia

  8. The Crystal Structures of Two Novel Cadmium-Picolinic Acid ...

    African Journals Online (AJOL)

    The crystal structures of two novel cadmium-picolinic acid complexes grown in aqueous solutions at selected pH values are reported. The structures are compared to expected solution species under the same conditions. The crystal structure of complex 1 exhibits a seven coordinate structure which contains a protonated ...

  9. Synthesis and Characterization of Tert-Butylgallium-Antimony Compounds; X-Ray Crystal Structures of t-Bu3Ga. Sb(SiMe3)3, T-Bu2GaSb(SiMe3)2, and t-Bu2GaSb(SiMe3)Ga(t-Bu)2Cl, The first Example of a Gallium-Antimony Mixed-Bridge Compound

    National Research Council Canada - National Science Library

    Wells, Richard

    1997-01-01

    ...:1 equilibration of t-Bu2GaCl with 2. These new gallium-antimony compounds have been characterized through multinuclear solution NMR spectroscopy, partial elemental analysis, and single-crystal X-ray structural analysis...

  10. Structural Transitions in Cholesteric Liquid Crystal Droplets

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Ye; Bukusoglu, Emre; Martínez-González, José A.; Rahimi, Mohammad; Roberts, Tyler F.; Zhang, Rui; Wang, Xiaoguang; Abbott, Nicholas L.; de Pablo, Juan J.

    2016-07-26

    Confinement of cholesteric liquid crystals (ChLC) into droplets leads to a delicate interplay between elasticity, chirality, and surface energy. In this work, we rely on a combination of theory and experiments to understand the rich morphological behavior that arises from that balance. More specifically, a systematic study of micrometer-sized ChLC droplets is presented as a function of chirality and surface energy (or anchoring). With increasing chirality, a continuous transition is observed from a twisted bipolar structure to a radial spherical structure, all within a narrow range of chirality. During such a transition, a bent structure is predicted by simulations and confirmed by experimental observations. Simulations are also able to capture the dynamics of the quenching process observed in experiments. Consistent with published work, it is found that nanoparticles are attracted to defect regions on the surface of the droplets. For weak anchoring conditions at the nanoparticle surface, ChLC droplets adopt a morphology similar to that of the equilibrium helical phase observed for ChLCs in the bulk. As the anchoring strength increases, a planar bipolar structure arises, followed by a morphological transition to a bent structure. The influence of chirality and surface interactions are discussed in the context of the potential use of ChLC droplets as stimuli-responsive materials for reporting molecular adsorbates.

  11. Crystal structure of strontium dinickel iron orthophosphate

    Directory of Open Access Journals (Sweden)

    Said Ouaatta

    2015-10-01

    Full Text Available The title compound, SrNi2Fe(PO43, synthesized by solid-state reaction, crystallizes in an ordered variant of the α-CrPO4 structure. In the asymmetric unit, two O atoms are in general positions, whereas all others atoms are in special positions of the space group Imma: the Sr cation and one P atom occupy the Wyckoff position 4e (mm2, Fe is on 4b (2/m, Ni and the other P atom are on 8g (2, one O atom is on 8h (m and the other on 8i (m. The three-dimensional framework of the crystal structure is built up by [PO4] tetrahedra, [FeO6] octahedra and [Ni2O10] dimers of edge-sharing octahedra, linked through common corners or edges. This structure comprises two types of layers stacked alternately along the [100] direction. The first layer is formed by edge-sharing octahedra ([Ni2O10] dimer linked to [PO4] tetrahedra via common edges while the second layer is built up from a strontium row followed by infinite chains of alternating [PO4] tetrahedra and FeO6 octahedra sharing apices. The layers are held together through vertices of [PO4] tetrahedra and [FeO6] octahedra, leading to the appearance of two types of tunnels parallel to the a- and b-axis directions in which the Sr cations are located. Each Sr cation is surrounded by eight O atoms.

  12. A HPMT based set-up to characterize scintillating crystals

    International Nuclear Information System (INIS)

    D'Ambrosio, C.; Ercoli, C.; Jaaskelainen, S.; Lecoeur, G.; Leutz, H.; Loos, R.; Piedigrossi, D.; Puertolas, D.; Rosso, E.; Schomaker, R.

    1999-01-01

    We have developed a fully automatic measurement set-up, capable of measuring light yields arising from scintillating crystals in a linear range of about four orders of magnitude. The photodetector is a hybrid photomultiplier tube specially developed to optimize linear range and photon detection. Crystal and photodetector are temperature controlled by a closed water circuit, as this is essential when measuring low light yield scintillating crystals with a marked temperature dependence of their light yield. Gamma sources can be placed either on top or on the side of the crystal. In this latter case, the source can be automatically moved by a computer-controlled step motor to provide a uniformity profile of the light yield along the crystal. Tagged and not-tagged operation modes are possible. The whole set-up is computer-controlled in an effort to provide fast and reliable measurements, to characterize many crystals per day. This is important for the quality control of the lead tungstate crystals that will be applied in the electromagnetic calorimeter of the CMS-detector at the LHC at CERN. (author)

  13. A HPMT based set-up to characterize scintillating crystals

    Energy Technology Data Exchange (ETDEWEB)

    D' Ambrosio, C.; Ercoli, C.; Jaaskelainen, S.; Lecoeur, G.; Leutz, H.; Loos, R.; Piedigrossi, D.; Puertolas, D.; Rosso, E.; Schomaker, R

    1999-09-21

    We have developed a fully automatic measurement set-up, capable of measuring light yields arising from scintillating crystals in a linear range of about four orders of magnitude. The photodetector is a hybrid photomultiplier tube specially developed to optimize linear range and photon detection. Crystal and photodetector are temperature controlled by a closed water circuit, as this is essential when measuring low light yield scintillating crystals with a marked temperature dependence of their light yield. Gamma sources can be placed either on top or on the side of the crystal. In this latter case, the source can be automatically moved by a computer-controlled step motor to provide a uniformity profile of the light yield along the crystal. Tagged and not-tagged operation modes are possible. The whole set-up is computer-controlled in an effort to provide fast and reliable measurements, to characterize many crystals per day. This is important for the quality control of the lead tungstate crystals that will be applied in the electromagnetic calorimeter of the CMS-detector at the LHC at CERN. (author)

  14. Facile synthesis of gold nanomaterials with unusual crystal structures.

    Science.gov (United States)

    Fan, Zhanxi; Huang, Xiao; Chen, Ye; Huang, Wei; Zhang, Hua

    2017-11-01

    Gold (Au) nanomaterials have attracted wide research attention, owing to their high chemical stability, promising catalytic properties, excellent biocompatibility, unique electronic structure and outstanding localized surface plasmon resonance (LSPR) absorption properties; all of which are closely related to their size and shape. Recently, crystal-phase-controlled synthesis of noble metal nanomaterials has emerged as a promising strategy to tune their physicochemical properties. This protocol describes the detailed experimental procedures for the crystal-phase-controlled syntheses of Au nanomaterials with unusual crystal structures under mild conditions. Briefly, pure hexagonal close-packed (hcp) Au square sheets (AuSSs) with a thickness of ∼2.4 nm are synthesized using a graphene-oxide-assisted method in which HAuCl 4 is reduced by oleylamine in a mixture of hexane and ethanol. By using pure hexane as the solvent, well-dispersed ultrathin hcp/face-centered cubic (fcc) Au nanowires with a diameter of ∼1.6 nm on graphene oxide can be obtained. Meanwhile, hcp/fcc Au square-like plates with a side length of 200-400 nm are prepared via the secondary growth of Au on the hcp AuSSs. Remarkably, hexagonal (4H) Au nanoribbons with a thickness of 2.0-6.0 nm can be synthesized with a one-pot colloidal method in which HAuCl 4 is reduced by oleylamine in a mixed solvent of hexane and 1,2-dichloropropane. It takes 17-37 h for the synthesis of these Au nanomaterials with unusual crystal structures. Transmission electron microscopy (TEM) and atomic force microscopy (AFM) are used to characterize the resultant Au nanomaterials, which could have many promising applications, such as biosensing, near-IR photothermal therapy, catalysis and surface-enhanced Raman scattering (SERS).

  15. Thienyl-containing $-Diketones: Synthesis, Characterization, Crystal ...

    African Journals Online (AJOL)

    NJD

    A synergistic interplay of resonance and hydrogen bond. (HB) formation ...... 18 Cambridge Structural Database (CSD), Version 5.27, August 2006 update. ... 21 P.W. Atkins, Physical Chemistry, 5th edn., Oxford University Press,. Oxford, UK ...

  16. Growth and characterization of β-Ga2O3 crystals

    Science.gov (United States)

    Nikolaev, V. I.; Maslov, V.; Stepanov, S. I.; Pechnikov, A. I.; Krymov, V.; Nikitina, I. P.; Guzilova, L. I.; Bougrov, V. E.; Romanov, A. E.

    2017-01-01

    Here we report on the growth and characterization of β-Ga2O3 bulk crystals and polycrystalline layer on different substrates. Bulk β-Ga2O3 crystals were produced by free crystallisation of gallium oxide melt in sapphire crucible. Transparent single crystals measuring up to 8 mm across were obtained. Good structural quality was confirmed by x-ray diffraction rocking curve FWHM values of 46″. Young's modulus, shear modulus and hardness of the β-Ga2O3 crystals were measured by nanoindentation and Vickers microindentation techniques. Polycrystalline β-Ga2O3 films were deposited on silicon and sapphire substrates by sublimation method. It was found that structure and morphology of the films were greatly influenced by the material and orientation of the substrates. The best results were achieved on a-plane sapphire substrates where predominantly (111) oriented films were obtained.

  17. Crystal structure of a snake venom cardiotoxin

    International Nuclear Information System (INIS)

    Rees, B.; Samama, J.P.; Thierry, J.C.; Gilibert, M.; Fischer, J.; Schweitz, H.; Lazdunski, M.; Moras, D.

    1987-01-01

    Cardiotoxin V/sup II/4 from Naja mossambica crystallizes in space group P6 1 (a = b = 73.9 A; c = 59.0 A) with two molecules of toxin (molecular mass = 6715 Da) in the asymmetric unit. The structure was solved by using a combination of multiple isomorphous replacement and density modification methods. Model building and least-squares refinement led to an agreement factor of 27% for a data set to 3-A resolution prior to any inclusion of solvent molecules. The topology of the molecule is similar to that found in short and long snake neurotoxins, which block the nicotinic acetylcholine receptor. Major differences occur in the conformation of the central loop, resulting in a change in the concavity of the molecule. Hydrophobic residues are clustered in two distinct areas. The existence of stable dimeric entities in the crystalline state, with the formation of a six-stranded antiparallel β sheet, may be functionally relevant

  18. Electronic structure of single crystal C60

    International Nuclear Information System (INIS)

    Wu, J.; Shen, Z.X.; Dessau, D.S.; Cao, R.; Marshall, D.S.; Pianetta, P.; Lindau, I.; Yang, X.; Terry, J.; King, D.M.; Wells, B.O.; Elloway, D.; Wendt, H.R.; Brown, C.A.; Hunziker, H.; Vries, M.S. de

    1992-01-01

    We report angle-resolved photoemission data from single crystals of C 60 cleaved in UHV. Unlike the other forms of pure carbon, the valence band spectrum of C 60 consists of many sharp features that can be essentially accounted for by the quantum chemical calculations describing individual molecules. This suggests that the electronic structure of solid C 60 is mainly determined by the bonding interactions within the individual molecules. We also observe remarkable intensity modulations of the photoemission features as a function of photon energy, suggesting strong final state effects. Finally, we address the issue of the band width of the HOMO state of C 60 . We assert that the width of the photoemission peak of C 60 does not reflect the intrinsic band width because it is broadened by the non 0-0 transitions via the Franck-Condon principle. Our view point provides a possible reconciliation between these photoemission data and those measured by other techniques. (orig.)

  19. Crystal structure of Homo sapiens protein LOC79017

    Energy Technology Data Exchange (ETDEWEB)

    Bae, Euiyoung; Bingman, Craig A.; Aceti, David J.; Phillips, Jr., George N. (UW)

    2010-02-08

    LOC79017 (MW 21.0 kDa, residues 1-188) was annotated as a hypothetical protein encoded by Homo sapiens chromosome 7 open reading frame 24. It was selected as a target by the Center for Eukaryotic Structural Genomics (CESG) because it did not share more than 30% sequence identity with any protein for which the three-dimensional structure is known. The biological function of the protein has not been established yet. Parts of LOC79017 were identified as members of uncharacterized Pfam families (residues 1-95 as PB006073 and residues 104-180 as PB031696). BLAST searches revealed homologues of LOC79017 in many eukaryotes, but none of them have been functionally characterized. Here, we report the crystal structure of H. sapiens protein LOC79017 (UniGene code Hs.530024, UniProt code O75223, CESG target number go.35223).

  20. Crystal chemical characterization of mullite-type aluminum borate compounds

    Energy Technology Data Exchange (ETDEWEB)

    Hoffmann, K., E-mail: Kristin.Hoffmann@uni-bremen.de [Kristallographie, FB05, Klagenfurter Straße / GEO, Universität Bremen, D-28359 Bremen (Germany); Institut für Anorganische Chemie und Kristallographie, FB02, Leobener Straße / NW2, Universität Bremen, D-28359 Bremen (Germany); Hooper, T.J.N. [Department of Physics, University of Warwick, Coventry CV4 7AL (United Kingdom); Zhao, H.; Kolb, U. [Institut für Anorganische Chemie und Analytische Chemie, Jakob-Welder-WegJakob-Welder-Weg 11, Johannes Gutenberg-University Mainz, D-55128 Mainz (Germany); Murshed, M.M. [Institut für Anorganische Chemie und Kristallographie, FB02, Leobener Straße / NW2, Universität Bremen, D-28359 Bremen (Germany); MAPEX Center for Materials and Processes, Bibliothekstraße 1, Universität Bremen, D-28359 Bremen (Germany); Fischer, M.; Lührs, H. [Kristallographie, FB05, Klagenfurter Straße / GEO, Universität Bremen, D-28359 Bremen (Germany); MAPEX Center for Materials and Processes, Bibliothekstraße 1, Universität Bremen, D-28359 Bremen (Germany); Nénert, G. [Institut Laue-Langevin, 6 Rue Jules Horowitz, 38042 Grenoble Cedex 9 (France); Kudějová, P.; Senyshyn, A. [Heinz Maier-Leibnitz Zentrum (MLZ), Technische Universität München, Lichtenbergstr. 1, D-85748 Garching (Germany); and others

    2017-03-15

    Al-rich aluminum borates were prepared by different synthesis routes using various Al/B ratios, characterized by diffraction methods, spectroscopy and prompt gamma activation analysis. The {sup 11}B NMR data show a small amount of BO{sub 4} species in all samples. The chemical analysis indicates a trend in the Al/B ratio instead of a fixed composition. Both methods indicate a solid solution Al{sub 5−x}B{sub 1+x}O{sub 9} where Al is substituted by B in the range of 1–3%. The structure of B-rich Al{sub 4}B{sub 2}O{sub 9} (C2/m, a=1488 pm, b=553 pm, c=1502 pm, ß=90.6°), was re-investigated by electron diffraction methods, showing that structural details vary within a crystallite. In most of the domains the atoms are orderly distributed, showing no signal for the postulated channel oxygen atom O5. The absence of O5 is supported by density functional theory calculations. Other domains show a probable disordered configuration of O5 and O10, indicated by diffuse scattering along the b direction. - Graphical abstract: Projections of three-dimensional electron diffraction space of Al{sub 4}B{sub 2}O{sub 9} along the main directions. - Highlights: • The crystal structure of Al{sub 4}B{sub 2}O{sub 9} was re-evaluated. • Structural details vary among different crystals and inside Al{sub 4}B{sub 2}O{sub 9} crystallites. • Diffuse scattering indicate a probable disordered configuration of O5 and O10. • A solid solution series for Al{sub 5−x}B{sub x}O{sub 9} is indicated by PGAA and NMR spectroscopy. • The presence of BO{sub 4} groups is confirmed by {sup 11}B MAS NMR spectroscopy for Al{sub 5−x}B{sub 1+x}O{sub 9}.

  1. New μ-OAC bridged dinuclear copper(II) complex with tridentate Schiff base ligand: synthesis, characterization, crystal structure, and CuO nano-particles formation

    Czech Academy of Sciences Publication Activity Database

    Grivani, G.; Eigner, Václav; Dušek, Michal; Sadeghi, B.; Khalaji, A.D.

    2015-01-01

    Roč. 41, č. 7 (2015), s. 456-461 ISSN 1070-3284 R&D Projects: GA ČR(CZ) GA14-03276S Institutional support: RVO:68378271 Keywords : Schiff base * complex structure * x-ray crystallography * Jana2006 Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.516, year: 2015

  2. 2.2.1. Synthesis, spectroscopic characterization and crystal structure of [ReV(O2(pyz4][ReII(NOBr4(pyz] (pyz = pyrazine

    Directory of Open Access Journals (Sweden)

    Mario Pacheco, Alicia Cuevas, Javier González-Platas, Carlos Kremer*

    2015-03-01

    Full Text Available Abstract: A novel Re(V-Re(II nitrosyl complex, [Re(O2(pyz 4][Re(NOBr4(pyz] (pyz = pyrazine was prepared and characterized by X-ray diffraction, elemental analysis, infrared and ultraviolet-visible absorption spectra. This product is obtained in the initial steps of the reaction of (NBu4[Re(NOBr4(EtOH] with pyrazine. Both, the cation and the anion are mononuclear complexes. The Re(V atom in the cation is six-coordinate with four nitrogen atoms from pyrazine ligands, and two oxo ligands. The Re(II anion is also six-coordinate, with four bromide ligands, a linear nitrosyl group and one nitrogen from pyrazine. The spectroscopic studies are discussed and compared with those already reported separately for the cation and the anion. Supporting information: X-Ray (CIF file

  3. Crystal growth, characterization and theoretical studies of 4-aminopyridinium picrate

    Science.gov (United States)

    Aditya Prasad, A.; Muthu, K.; Rajasekar, M.; Meenatchi, V.; Meenakshisundaram, S. P.

    2015-01-01

    Single crystals of 4-aminopyridinium picrate (APP) were grown by slow evaporation of a mixed solvent system methanol-acetone (1:1, v/v) containing equimolar quantities of 4-aminopyridine and picric acid. Structure is elucidated by single crystal XRD analysis and the crystal belongs to monoclinic system with four molecules in the unit cell (space group P21/c) and the cell parameter values are, a = 8.513 Å (±0.015), b = 11.33 Å (±0.02), c = 14.33 Å (±0.03) and β = 104.15° (±0.019), V = 1340 A3 (±6) with refined R factors R1 = 0.0053 and wR2 = 0.0126. The electron density mapping is interpreted to find coordinates for each atom in the crystallized molecules. The various functional groups present in the molecule are confirmed by FT-IR analysis. UV-visible spectral analysis was used to determine the band gap energy of 4-aminopyridinium picrate. Powder X-ray diffraction pattern reveals the crystallinity of the as-grown crystal and it closely resembles the simulated XRD from the single crystal XRD analysis. Scanning electron microscopy reveals the surface morphology of the grown crystal. Optimized geometry is derived by Hartree-Fock theory calculations and the first-order molecular hyperpolarizability (β), theoretically calculated bond length, bond angles and excited state energy from theoretical UV-vis spectrum were estimated.

  4. Crystallization and preliminary characterization of dihydropteridine reductase from Dictyostelium discoideum

    International Nuclear Information System (INIS)

    Chen, Cong; Seo, Kyung Hye; Kim, Hye Lim; Zhuang, Ningning; Park, Young Shik; Lee, Kon Ho

    2008-01-01

    The dihydropteridine reductase from D. discoideum has been crystallized. Diffraction data were collected from a rectangular-shaped crystal to 2.16 Å resolution. Dihydropteridine reductase from Dictyostelium discoideum (dicDHPR) can produce d-threo-BH 4 [6R-(1′R,2′R)-5,6,7,8-tetrahydrobiopterin], a stereoisomer of l-erythro-BH 4 , in the last step of tetrahydrobiopterin (BH 4 ) recycling. In this reaction, DHPR uses NADH as a cofactor to reduce quinonoid dihydrobiopterin back to BH 4 . To date, the enzyme has been purified to homogeneity from many sources. In this report, the dicDHPR–NAD complex has been crystallized using the hanging-drop vapour-diffusion method with PEG 3350 as a precipitant. Rectangular-shaped crystals were obtained. Crystals grew to maximum dimensions of 0.4 × 0.6 × 0.1 mm. The crystal belonged to space group P2 1 , with unit-cell parameters a = 49.81, b = 129.90, c = 78.76 Å, β = 100.00°, and contained four molecules in the asymmetric unit, forming two closely interacting dicDHPR–NAD dimers. Diffraction data were collected to 2.16 Å resolution using synchrotron radiation. The crystal structure has been determined using the molecular-replacement method

  5. Characterization of gypsum crystals exposed to a high CO2 concentration fog using x-ray

    International Nuclear Information System (INIS)

    Carreño-Márquez, I. J. A.; Castillo-Sandoval, I.; Esparza-Ponce, H. E.; Fuentes-Cobas, L.; Montero-Cabrera, M. E.

    2015-01-01

    In Chihuahua State, a little town called Naica has the largest gypsum single crystals in the world. The growth of these structures has been described as a long and stable process developed over thousands of years. Due to the change in the environmental conditions, these crystals could suffer alterations on their surface. In this project we study the cause of possible deterioration of the giant crystals and intend to suggest measures for their preservation. For this sake, our first experiment consists on several gypsum crystals that have been subjected in a climate chamber to a fog at high CO 2 concentration and 51 °C for a period of time of six months, extracting two crystals every 15 days. Then the crystals have been characterized through Grazing Incidence X-Ray Diffraction using a diffractometer PanAlytical X’PertPro with two different detectors; Xe-filled proportional detector and a Pixel 3D detector. The results were compared to determine which technique is the most suitable to study the degradation of gypsum single crystals. In the two cases, we have identified only the gypsum phase, but with different crystal plane orientations

  6. Crystal structure and pharmacological characterization of a novel N-methyl-D-aspartate (NMDA) receptor antagonist at the GluN1 glycine binding site

    DEFF Research Database (Denmark)

    Kvist, Trine; Steffensen, Thomas Bielefeldt; Greenwood, Jeremy R

    2013-01-01

    NMDA receptors are ligand-gated ion channels that mediate excitatory neurotransmission in the brain. They are tetrameric complexes composed of glycine-binding GluN1 and GluN3 subunits together with glutamate-binding GluN2 subunits. Subunit-selective antagonists that discriminate between the glyci...... screening. Furthermore, the structure reveals that the imino acetamido group of TK40 acts as an α-amino acid bioisostere, which could be of importance in bioisosteric replacement strategies for future ligand design....

  7. Formamidinium iodide: crystal structure and phase transitions

    Directory of Open Access Journals (Sweden)

    Andrey A. Petrov

    2017-04-01

    Full Text Available At a temperature of 100 K, CH5N2+·I− (I, crystallizes in the monoclinic space group P21/c. The formamidinium cation adopts a planar symmetrical structure [the r.m.s. deviation is 0.002 Å, and the C—N bond lengths are 1.301 (7 and 1.309 (8 Å]. The iodide anion does not lie within the cation plane, but deviates from it by 0.643 (10 Å. The cation and anion of I form a tight ionic pair by a strong N—H...I hydrogen bond. In the crystal of I, the tight ionic pairs form hydrogen-bonded zigzag-like chains propagating toward [20-1] via strong N—H...I hydrogen bonds. The hydrogen-bonded chains are further packed in stacks along [100]. The thermal behaviour of I was studied by different physicochemical methods (thermogravimetry, differential scanning calorimetry and powder diffraction. Differential scanning calorimetry revealed three narrow endothermic peaks at 346, 387 and 525 K, and one broad endothermic peak at ∼605 K. The first and second peaks are related to solid–solid phase transitions, while the third and fourth peaks are attributed to the melting and decomposition of I. The enthalpies of the phase transitions at 346 and 387 K are estimated as 2.60 and 2.75 kJ mol−1, respectively. The X-ray powder diffraction data collected at different temperatures indicate the existence of I as the monoclinic (100–346 K, orthorhombic (346–387 K and cubic (387–525 K polymorphic modifications.

  8. Synthesis and crystal structure of two lead (II) complexes with 1,10-phenanthroline ligand

    International Nuclear Information System (INIS)

    Olivera, Fiorella L.; Santillan, Guillermo A.

    2012-01-01

    Two coordination complexes have been synthesized by the reaction of lead nitrate (II) with 1,10-phenanthroline in methanol/water. The crystals of these complexes were obtained by using the diffusion method and structurally characterized by X-ray single crystal diffraction. Both complexes crystallized in the monoclinic space group P2 1 /c. The analysis by crystal X-ray diffraction reveals that in both complexes the coordination around the lead (II) ion is a distorted octahedral structure where the ion is bonded to the heterocyclic nitrogen atoms of chelating ligand 1,10-phenanthroline, three oxygen atoms of three nitrate groups and one oxygen from the water molecule. The difference between the complexes lies in the way of nitrate ion in presence of carboxylic acid aromatics. In addition, the crystal structure of complexes can be regarded as a 3D coordination polymer through Pb-O weak interactions, hydrogen bonds and π-π stacking interactions. (author).

  9. Crystal Structures and Characterizations of Bis(1-benzoyl methyl-benzotriazole-N3)dichoro Metal(II) Complex:[MCl2-(C6H4N3CH2COPh)2] [M=Zn(II), Co(II)

    Institute of Scientific and Technical Information of China (English)

    JIAN,Fang-Fang(建方方); SUN,Ping-Ping(孙萍萍); XIAO,Hai-Lian(肖海连); JIAO,Kui(焦奎)

    2004-01-01

    The structures of [MCl2(C6H4N3CH2COPh)2] [M=Zn(II) (1), Co(II) (2)] have been determined by X-ray crystallography. They were characterized by elemental analysis, IR spectrum, electronic spectrum and thermogravimetric-differential thermal analysis. They all crystallize in the triclinic system, space group Pī, with lattice parameters a=0.9449(2) nm, b=1.1291(2) nm, c=1.3637(3) nm, α=111.70(3)°, β=94.33(3)°, γ=90.97(3), Z=2 for compound 1; a=0.9437(2) nm, b=1.1277(2) nm, c=1.3650(3) nm, α=111.76(3)°, β=94.50(3)°, γ=90.80(3)°, Z=2 for compound 2. The metal ions are all coordinated by two Cl- anions and two nitrogen atoms of 1-benzoylmethyl-benzotriazole ligands, forming the distorted tetrahedral geometry. The Zn-Cl and Zn-N bond lengths are 0.2209(2), 0.2210(2) nm and 0.2059(4), 0.2067(4) nm, respectively. The Co-Cl and Co-N bond lengths are 0.2215(2), 0.2222(2) nm and 0.2028(5), 0.2045(5) nm, respectively. The thermogravimetric (TG) data indicate that they are nearly similar in TG curve, and there are not structural transitions in the two compounds. They all have a high thermal stability. But, there is little difference in DTG (differential thermogravimetric) curves of those two compounds. Elemental analysis, electronic and IR spectra are in agreement with the structural data.

  10. Syntheses, crystal structures and characterizations of BaZn(SeO3)2 and BaZn(TeO3)Cl2

    International Nuclear Information System (INIS)

    Jiang Hailong; Feng Meiling; Mao Jianggao

    2006-01-01

    Two new barium zinc selenite and tellurite, namely, BaZn(SeO 3 ) 2 and BaZn(TeO 3 )Cl 2 , have been synthesized by the solid state reaction. The structure of BaZn(SeO 3 ) 2 features double chains of [Zn(SeO 3 ) 2 ] 2- anions composed of four- and eight-member rings which are alternatively along a-axis. The double chains of [Zn 2 (TeO 3 ) 2 Cl 3 ] 3- anions in BaZn(TeO 3 )Cl 2 are formed by Zn 3 Te 3 rings in which each tellurite group connects with three ZnO 3 Cl tetrahedra. BaZn(SeO 3 ) 2 and BaZn(TeO 3 )Cl 2 are wide bandgap semiconductors based on optical diffuse reflectance spectrum measurements. -- Graphical abstract: Two new barium zinc selenite and tellurite, namely, BaZn(SeO 3 ) 2 and BaZn(TeO 3 )Cl 2 , have been synthesized by solid state reaction. The structure of BaZn(SeO 3 ) 2 features 1D double chains of [Zn(SeO 3 ) 2 ] 2- anions composed of four- and eight-member rings which are alternatively along a-axis. The 1D double chains of [Zn 2 (TeO 3 ) 2 Cl 3 ] 3- anions in BaZn(TeO 3 )Cl 2 are formed by Zn 3 Te 3 rings in which each tellurite group connects with one ZnO 3 Cl and two ZnO 2 Cl 2 tetrahedra. BaZn(SeO 3 ) 2 and BaZn(TeO 3 )Cl 2 are wide bandgap semiconductors based on optical diffuse reflectance spectrum measurements

  11. Fully automatic characterization and data collection from crystals of biological macromolecules

    International Nuclear Information System (INIS)

    Svensson, Olof; Malbet-Monaco, Stéphanie; Popov, Alexander; Nurizzo, Didier; Bowler, Matthew W.

    2015-01-01

    A fully automatic system has been developed that performs X-ray centring and characterization of, and data collection from, large numbers of cryocooled crystals without human intervention. Considerable effort is dedicated to evaluating macromolecular crystals at synchrotron sources, even for well established and robust systems. Much of this work is repetitive, and the time spent could be better invested in the interpretation of the results. In order to decrease the need for manual intervention in the most repetitive steps of structural biology projects, initial screening and data collection, a fully automatic system has been developed to mount, locate, centre to the optimal diffraction volume, characterize and, if possible, collect data from multiple cryocooled crystals. Using the capabilities of pixel-array detectors, the system is as fast as a human operator, taking an average of 6 min per sample depending on the sample size and the level of characterization required. Using a fast X-ray-based routine, samples are located and centred systematically at the position of highest diffraction signal and important parameters for sample characterization, such as flux, beam size and crystal volume, are automatically taken into account, ensuring the calculation of optimal data-collection strategies. The system is now in operation at the new ESRF beamline MASSIF-1 and has been used by both industrial and academic users for many different sample types, including crystals of less than 20 µm in the smallest dimension. To date, over 8000 samples have been evaluated on MASSIF-1 without any human intervention

  12. Fully automatic characterization and data collection from crystals of biological macromolecules

    Energy Technology Data Exchange (ETDEWEB)

    Svensson, Olof; Malbet-Monaco, Stéphanie; Popov, Alexander; Nurizzo, Didier, E-mail: nurizzo@esrf.fr [European Synchrotron Radiation Facility, 71 Avenue des Martyrs, CS 40220, 38043 Grenoble (France); Bowler, Matthew W., E-mail: nurizzo@esrf.fr [European Molecular Biology Laboratory, Grenoble Outstation, 71 Avenue des Martyrs, CS 90181, 38042 Grenoble (France); Université Grenoble Alpes–EMBL–CNRS, Grenoble Outstation, 71 Avenue des Martyrs, CS 90181, 38042 Grenoble (France); European Synchrotron Radiation Facility, 71 Avenue des Martyrs, CS 40220, 38043 Grenoble (France)

    2015-07-31

    A fully automatic system has been developed that performs X-ray centring and characterization of, and data collection from, large numbers of cryocooled crystals without human intervention. Considerable effort is dedicated to evaluating macromolecular crystals at synchrotron sources, even for well established and robust systems. Much of this work is repetitive, and the time spent could be better invested in the interpretation of the results. In order to decrease the need for manual intervention in the most repetitive steps of structural biology projects, initial screening and data collection, a fully automatic system has been developed to mount, locate, centre to the optimal diffraction volume, characterize and, if possible, collect data from multiple cryocooled crystals. Using the capabilities of pixel-array detectors, the system is as fast as a human operator, taking an average of 6 min per sample depending on the sample size and the level of characterization required. Using a fast X-ray-based routine, samples are located and centred systematically at the position of highest diffraction signal and important parameters for sample characterization, such as flux, beam size and crystal volume, are automatically taken into account, ensuring the calculation of optimal data-collection strategies. The system is now in operation at the new ESRF beamline MASSIF-1 and has been used by both industrial and academic users for many different sample types, including crystals of less than 20 µm in the smallest dimension. To date, over 8000 samples have been evaluated on MASSIF-1 without any human intervention.

  13. Crystal structure of the Al2CuIr phase

    International Nuclear Information System (INIS)

    Meshi, L.; Ezersky, V.; Kapush, D.; Grushko, B.

    2010-01-01

    A new ternary Al 2 CuIr phase was revealed in the Al-Cu-Ir system. It is formed below 1063 o C from the β-phase (CsCl-type structure) extending at elevated temperatures from AlIr. The crystal structure of the Al 2 CuIr phase was determined using a combination of precession electron diffraction and X-ray powder diffraction techniques. The phase has an orthorhombic C-centered unit cell with lattice parameters a = 8.1196(7) A, b = 5.0646(2) A and c = 5.18513(3) A; its crystal symmetry can be described by the Cmme (no. 67) space group (Pearson symbol oC16). The unit cell of the new phase contains 8 Al, 4 Cu and 4 Ir atoms and exhibits a new structure type. The reliability factors characterizing the Rietveld refinement procedure are: R p = 4.45%, R wp = 6.45%, R B = 3.69% and R f = 2.41%.

  14. Synthesis, crystal structure determination of two-dimensional ...

    Indian Academy of Sciences (India)

    Abstract. The 2-D polymeric complex (I) has the formula [Ag(phSE)(NO3)]n, which has been crystallized from methanol-acetonitrile mixture and characterized by elemental analysis and single-crystal X-ray diffraction analysis. In this polymer, each Ag(I) ion occupies distorted trigonal pyramidal geometry coordinating with two.

  15. CCDC 1408042: Experimental Crystal Structure Determination : 6,13-dimesitylpentacene

    KAUST Repository

    Shi, Xueliang

    2015-01-01

    An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

  16. CCDC 1416891: Experimental Crystal Structure Determination : Methyl-triphenyl-germanium

    KAUST Repository

    Bernatowicz, Piotr

    2015-01-01

    An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

  17. Synthesis, Physico-chemical Characterization, Crystal Structure and Influence on Microbial and Tumor Cells of Some Co(II Complexes with 5,7-Dimethyl-1,2,4-triazolo[1,5-a]pyrimidine

    Directory of Open Access Journals (Sweden)

    Luminiţa Măruţescu

    2017-07-01

    Full Text Available Three complexes, namely [Co(dmtp2(OH24][CoCl4] (1, [Co(dmtp2Cl2] (2 and [Co(dmtp2(OH24]Cl2∙2H2O (3 (dmtp: 5,7-dimethyl-1,2,4-triazolo[1,5-a]pyrimidine, were synthesized and characterized by spectral (IR, UV-Vis-NIR, and magnetic measurements at room temperature, as well as single crystal X-ray diffraction. Complex (1 crystallizes in monoclinic system (space group C2/c, complex (2 adopts an orthorhombic system (space group Pbca, and complex (3 crystallizes in triclinic system (space group P1. Various types of extended hydrogen bonds and π–π interactions provide a supramolecular architecture for all complexes. All species were evaluated for antimicrobial activity towards planktonic and biofilm-embedded microbial cells and influence on HEp-2 cell viability, cellular cycle and gene expression.

  18. Growth and structural characterization of single crystals of the magnetic superconductor Ru1-xSr2-yGd1+yCu2+xO8-δ (RuGd-1212) obtained by the partial melting technique

    Science.gov (United States)

    Yamaki, K.; Bamba, Y.; Mochiku, T.; Funahashi, S.; Matsushita, Y.; Irie, A.

    2018-05-01

    In this study, cubic single crystals of the magnetic superconductor Ru1-xSr2-yGd1+yCu2+xO8-δ (RuGd-1212) with typical dimensions of 100-150 μm in length were grown by the partial melting technique. Multiple 00l reflections were first observed by XRD measurements of the bulk RuGd-1212 single crystals. The resistivity of the obtained crystals was roughly estimated to be ∼24-80 mΩ cm and no superconducting transition was observed down to 4.2 K. From the XRD measurements and refinement of the crystal structure, it was apparent that the Ru and Sr sites of the single-crystal RuGd-1212 were partially substituted by Cu and Gd, respectively. Oxygen defects were found to be minor (δ ≈ 0.1). The lattice parameters a and c of the single crystals were found to be larger and smaller, respectively, than those of a polycrystalline sample.

  19. Purification, characterization and crystallization of the F-ATPase from Paracoccus denitrificans.

    Science.gov (United States)

    Morales-Rios, Edgar; Watt, Ian N; Zhang, Qifeng; Ding, Shujing; Fearnley, Ian M; Montgomery, Martin G; Wakelam, Michael J O; Walker, John E

    2015-09-01

    The structures of F-ATPases have been determined predominantly with mitochondrial enzymes, but hitherto no F-ATPase has been crystallized intact. A high-resolution model of the bovine enzyme built up from separate sub-structures determined by X-ray crystallography contains about 85% of the entire complex, but it lacks a crucial region that provides a transmembrane proton pathway involved in the generation of the rotary mechanism that drives the synthesis of ATP. Here the isolation, characterization and crystallization of an integral F-ATPase complex from the α-proteobacterium Paracoccus denitrificans are described. Unlike many eubacterial F-ATPases, which can both synthesize and hydrolyse ATP, the P. denitrificans enzyme can only carry out the synthetic reaction. The mechanism of inhibition of its ATP hydrolytic activity involves a ζ inhibitor protein, which binds to the catalytic F₁-domain of the enzyme. The complex that has been crystallized, and the crystals themselves, contain the nine core proteins of the complete F-ATPase complex plus the ζ inhibitor protein. The formation of crystals depends upon the presence of bound bacterial cardiolipin and phospholipid molecules; when they were removed, the complex failed to crystallize. The experiments open the way to an atomic structure of an F-ATPase complex. © 2015 The Authors.

  20. Polymorphism in phenobarbital: discovery of a new polymorph and crystal structure of elusive form V.

    Science.gov (United States)

    Roy, Saikat; Goud, N Rajesh; Matzger, Adam J

    2016-03-21

    This report highlights the discovery of a new polymorph of the anticonvulsant drug phenobarbital (PB) using polymer-induced heteronucleation (PIHn) and unravelling the crystal structure of the elusive form V. Both forms are characterized by structural, thermal and VT-Raman spectroscopy methods to elucidate phase transformation behavior and shed light on stability relationships.

  1. Synthesis, crystal structure, and spectroscopic characterization of two new binuclear complexes of manganese(II) and vanadium(V) with dipicolinate ligands containing 2-aminopyrimidinium as a counter cation

    Czech Academy of Sciences Publication Activity Database

    Tabatabaee, M.; Mahmoodikhah, H.; Ahadiat, G.; Dušek, Michal; Pojarová, Michaela

    2013-01-01

    Roč. 144, č. 5 (2013), s. 621-626 ISSN 0026-9247 R&D Projects: GA ČR(CZ) GAP204/11/0809 Institutional support: RVO:68378271 Keywords : manganese complex * vanadium complex * dipicolinic ligand * crystal structure Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.347, year: 2013

  2. Synthesis, characterization and crystal structure determination of a new vanadium(IV) Schiff base complex (VOL.sub.2./sub.) and investigation of its catalytic activity in the epoxidation of cyclooctene

    Czech Academy of Sciences Publication Activity Database

    Grivani, G.; Tahmasebi, V.; Khalaji, A.D.; Fejfarová, Karla; Dušek, Michal

    2013-01-01

    Roč. 51, č. 1 (2013), s. 54-60 ISSN 0277-5387 R&D Projects: GA ČR(CZ) GAP204/11/0809 Institutional support: RVO:68378271 Keywords : vanadium (IV) * Schiff base * single crystal * structure determination * catalysis * epoxidation Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.047, year: 2013

  3. Crystal structure of Clostridium difficile toxin A

    Energy Technology Data Exchange (ETDEWEB)

    Chumbler, Nicole M.; Rutherford, Stacey A.; Zhang, Zhifen; Farrow, Melissa A.; Lisher, John P.; Farquhar, Erik; Giedroc, David P.; Spiller, Benjamin W.; Melnyk, Roman A.; Lacy, D. Borden

    2016-01-11

    Clostridium difficile infection is the leading cause of hospital-acquired diarrhoea and pseudomembranous colitis. Disease is mediated by the actions of two toxins, TcdA and TcdB, which cause the diarrhoea, as well as inflammation and necrosis within the colon. The toxins are large (308 and 270 kDa, respectively), homologous (47% amino acid identity) glucosyltransferases that target small GTPases within the host. The multidomain toxins enter cells by receptor-mediated endocytosis and, upon exposure to the low pH of the endosome, insert into and deliver two enzymatic domains across the membrane. Eukaryotic inositol-hexakisphosphate (InsP6) binds an autoprocessing domain to activate a proteolysis event that releases the N-terminal glucosyltransferase domain into the cytosol. Here, we report the crystal structure of a 1,832-amino-acid fragment of TcdA (TcdA1832), which reveals a requirement for zinc in the mechanism of toxin autoprocessing and an extended delivery domain that serves as a scaffold for the hydrophobic α-helices involved in pH-dependent pore formation. A surface loop of the delivery domain whose sequence is strictly conserved among all large clostridial toxins is shown to be functionally important, and is highlighted for future efforts in the development of vaccines and novel therapeutics.

  4. Crystal structure study of new lanthanide silicates with silico-carnotite structure

    International Nuclear Information System (INIS)

    Piccinelli, F.; Lausi, A.; Speghini, A.; Bettinelli, M.

    2012-01-01

    The crystal structures of new rare earth-based silicate compounds (Ca 3 Eu 2 Si 3 O 12 , Ca 3 Gd 2 Si 3 O 12 , Ca 3 Dy 2 Si 3 O 12 , Ca 3 Er 2 Si 3 O 12 and Ca 3 Lu 2 Si 3 O 12 ) have been determined using powder X-ray diffraction. From Rietveld refinement calculations on the collected powder patterns we observe a different distribution of the rare earth ions on the three available crystal sites characterized by different coordination numbers, depending on the ionic radius of the rare earth ion. The reasons of the instability of the silico-carnotite structure for lanthanide ions larger than Eu 3+ have been deduced. In addition, in order to detect crystal phase transitions, the powder patterns of Ca 3 Eu 2 Si 3 O 12 and Ca 3 Sm 2 Si 3 O 12 samples have been collected as a function of the temperature (RT-1000 °C range), but no phase transitions have been observed. - Graphical abstract: Synchrotron X-ray diffraction allows us the accurate determination of the RE 3+ ions distribution on the three available crystal sites of the silico-carnotite structure. Highlights: ► The structure of the Ca 3 M 2 Si 3 O 12 (M=Eu, Gd, Dy, Er and Lu) was determined. ► Different distribution of RE 3+ ions on the three available crystal sites was observed. ► The instability of the silico-carnotite structure for RE=La→Sm was discussed.

  5. Characterization of Crystal Chirality in Amino Acids Using Low-Frequency Raman Spectroscopy.

    Science.gov (United States)

    Aviv, Hagit; Nemtsov, Irena; Mastai, Yitzhak; Tischler, Yaakov R

    2017-10-19

    We present a new method for differentiating racemic crystals from enantiopure crystals. Recently, developments in optical filters have enabled the facile use of Raman spectroscopy to detect low-frequency vibrational (LFV) modes. Here, for the first time, we use Raman spectroscopy to characterize the LFV modes for crystalline organic materials composed of chiral molecules. The LF-Raman spectra of racemic and enantiopure crystals exhibit a significant variation, which we attribute to different hydrogen-bond networks in the chiral crystal structures. Across a representative set of amino acids, we observed that when comparing racemic versus enantiopure crystals, the available LFV modes and their relative scattering intensity are strong functions of side chain polarity. Thus, LF-Raman can be used as a method that is complementary to the currently used methods for characterizing crystal chirality due to simpler, faster, and more sensitive measurements, along with the small sample size required, which is limited by the laser-beam diameter in the focus.

  6. Band structures in fractal grading porous phononic crystals

    Science.gov (United States)

    Wang, Kai; Liu, Ying; Liang, Tianshu; Wang, Bin

    2018-05-01

    In this paper, a new grading porous structure is introduced based on a Sierpinski triangle routine, and wave propagation in this fractal grading porous phononic crystal is investigated. The influences of fractal hierarchy and porosity on the band structures in fractal graidng porous phononic crystals are clarified. Vibration modes of unit cell at absolute band gap edges are given to manifest formation mechanism of absolute band gaps. The results show that absolute band gaps are easy to form in fractal structures comparatively to the normal ones with the same porosity. Structures with higher fractal hierarchies benefit multiple wider absolute band gaps. This work provides useful guidance in design of fractal porous phononic crystals.

  7. Crystal and source characterization for the Crystal Backlighter Imager capability at the National Ignition Facility

    Science.gov (United States)

    Krauland, C. M.; Hall, G. N.; Buscho, J. G.; Hibbard, R.; McCarville, T. J.; Lowe-Webb, R.; Ayers, S. L.; Kalantar, D.; Kohut, T.; Kemp, G. E.; Bradley, D. K.; Bell, P.; Landen, O. L.; Brewster, T. N.; Piston, K.

    2017-10-01

    The Crystal Backlighter Imager (CBI) is a very narrow bandwidth ( 10 eV) x-ray radiography system that uses Bragg reflection from a spherically-curved crystal at near normal incidence. This diagnostic has the capability to image late in an ICF implosion because it only requires the brightness of the backlighter to be larger than the capsule self-emission in that narrow bandwidth. While the limited bandwidth is advantageous for this reason, it also requires that the effective energy of the backlighter atomic line is known to 1 eV accuracy for proper crystal alignment. Any Doppler shift in the line energy must be understood for the imaging system to work. The work presented details characterization experiments done at the Jupiter Laser Facility with a Si (8 6 2) crystal that will be used with a Selenium backlighter in the NIF CBI diagnostic. We used the spherically-bent crystals to image a small ( 200 µm) He α source generated by the Janus laser on a Se foil. Scanning Bragg angles over multiple shots allowed us to map out the spectral line intensity distribution for optimal alignment in NIF. A subsequent Doppler shift measurement using CBI on NIF will also be presented with complementary HYDRA modeling for both experiments. Prepared by LLNL under Contract DE-AC52-07NA27344 and by General Atomics under Contract DE-NA0001808.

  8. Single Crystals of Organolead Halide Perovskites: Growth, Characterization, and Applications

    KAUST Repository

    Peng, Wei

    2017-04-01

    With the soaring advancement of organolead halide perovskite solar cells rising from a power conversion efficiency of merely 3% to more than 22% shortly in five years, researchers’ interests on this big material family have been greatly spurred. So far, both in-depth studies on the fundamental properties of organolead halide perovskites and their extended applications such as photodetectors, light emitting diodes, and lasing have been intensively reported. The great successes have been ascribed to various superior properties of organolead halide hybrid perovskites such as long carrier lifetimes, high carrier mobility, and solution-processable high quality thin films, as will be discussed in Chapter 1. Notably, most of these studies have been limited to their polycrystalline thin films. Single crystals, as a counter form of polycrystals, have no grain boundaries and higher crystallinity, and thus less defects. These characteristics gift single crystals with superior optical, electrical, and mechanical properties, which will be discussed in Chapter 2. For example, organolead halide perovskite single crystals have been reported with much longer carrier lifetimes and higher carrier mobilities, which are especially intriguing for optoelectronic applications. Besides their superior optoelectronic properties, organolead halide perovskites have shown large composition versatility, especially their organic components, which can be controlled to effectively adjust their crystal structures and further fundamental properties. Single crystals are an ideal platform for such composition-structure-property study since a uniform structure with homogeneous compositions and without distraction from grain boundaries as well as excess defects can provide unambiguously information of material properties. As a major part of work of this dissertation, explorative work on the composition-structure-property study of organic-cation-alloyed organolead halide perovskites using their single

  9. Structural Color Patterns by Electrohydrodynamic Jet Printed Photonic Crystals.

    Science.gov (United States)

    Ding, Haibo; Zhu, Cun; Tian, Lei; Liu, Cihui; Fu, Guangbin; Shang, Luoran; Gu, Zhongze

    2017-04-05

    In this work, we demonstrate the fabrication of photonic crystal patterns with controllable morphologies and structural colors utilizing electrohydrodynamic jet (E-jet) printing with colloidal crystal inks. The final shape of photonic crystal units is controlled by the applied voltage signal and wettability of the substrate. Optical properties of the structural color patterns are tuned by the self-assembly of the silica nanoparticle building blocks. Using this direct printing technique, it is feasible to print customized functional patterns composed of photonic crystal dots or photonic crystal lines according to relevant printing mode and predesigned tracks. This is the first report for E-jet printing with colloidal crystal inks. Our results exhibit promising applications in displays, biosensors, and other functional devices.

  10. Synthesis, crystal structures, spectroscopic characterization and in ...

    Indian Academy of Sciences (India)

    cDepartment of Biotechnology, School of Bio-Sciences and Technology, VIT University, Vellore,. Tamil Nadu .... M. The lower molar conductivity values of 3 and 3.5. −1 cm2mol. −1 ..... the tolerance of pancreatic β-cells against oxida- tive stress ...

  11. Physicochemical and crystal structure analyses of the antidiabetic agent troglitazone.

    Science.gov (United States)

    Kobayashi, Katsuhiro; Fukuhara, Hiroshi; Hata, Tadashi; Sekine, Akiko; Uekusa, Hidehiro; Ohashi, Yuji

    2003-07-01

    The antidiabetic agent troglitazone has two asymmetric carbons located at the chroman ring and the thiazolidine ring and is produced as a mixture of equal amounts of four optical isomers, 2R-5S, 2S-5R, 2R-5R, and 2S-5S. The crystalline powdered drug substance consists of two diastereomer pairs, 2R-5R/2S-5S and 2R-5S/2S-5R. There are many types of crystals obtained from various crystallization conditions. The X-ray structure analysis and the physicochemical analyses of troglitazone were performed. The solvated crystals of the 2R-5R/2S-5S pair were crystallized from several solutions: methanol, ethanol, acetonitrile, and dichloromethane. The ratio of solvent and troglitazone was 1 : 2 (L1/2-form). The monohydrate crystals were obtained from aqueous acetone solution (L1-form). On the other hand, only an anhydrate crystal of the 2R-5S/2S-5R pair was crystallized from various solutions (H0-form). The dihydrous mixed crystal (MA2-form) was obtained from a mixture of the two diastereomer pairs of 2R-5R/2S-5S and 2R-5S/2S-5R in equal amounts by the slow evaporation of aqueous acetone solution. The crystal structure of the MA2-form is similar to the H0-form. When the MA2 crystal was kept under low humidity, it was converted into the dehydrated form (MA0-form) with retention of the single crystal form. The structure of the MA0-form is isomorphous to the H0-form. The MA2-form was converted into the MA0-form and vice versa with retention of the single crystal under low and high humidity, respectively. The crystallization and storage conditions of the drug substances were successfully analyzed.

  12. 1-Hydroxyethyl-2-Substituted Phenoxymethyl Benzimidazoles: Synthesis and Crystal Structures

    International Nuclear Information System (INIS)

    Wu, J.; Wang, Z.; Gu, H.; Chen, W.; Zhao, L.; Zhao, C.

    2016-01-01

    Five novel 1-hydroxyethyl-2-substituted phenoxymethyl benzimidazoles c1-c5 were successfully synthesized by a three-step route. Firstly, five substituted phenoxymethyl acids a1-a5 were prepared by the O-carboxymethylation reaction of the starting substituted phenols under microwave irradiation. Then, these compounds reacted with o-phenylendiamine to get the key intermediates 2-substituted phenoxymethyl benzimidazoles b1-b5. At last, the target compounds were synthesized by the N-hydroxyethylation reaction of b1-b5 with 2-chloroethyl alcohol through the solid-liquid phase transfer catalysis method, where tetrabutyl ammonium bromide (TBAB) was used as the catalyst. The structures of the target compounds were well characterized and verified by elemental analysis, MS, IR, 1H NMR, 13C NMR and single crystal X-ray diffraction analysis. (author)

  13. Crystal structure of arginine methyltransferase 6 from Trypanosoma brucei.

    Directory of Open Access Journals (Sweden)

    Chongyuan Wang

    Full Text Available Arginine methylation plays vital roles in the cellular functions of the protozoan Trypanosoma brucei. The T. brucei arginine methyltransferase 6 (TbPRMT6 is a type I arginine methyltransferase homologous to human PRMT6. In this study, we report the crystal structures of apo-TbPRMT6 and its complex with the reaction product S-adenosyl-homocysteine (SAH. The structure of apo-TbPRMT6 displays several features that are different from those of type I PRMTs that were structurally characterized previously, including four stretches of insertion, the absence of strand β15, and a distinct dimerization arm. The comparison of the apo-TbPRMT6 and SAH-TbPRMT6 structures revealed the fine rearrangements in the active site upon SAH binding. The isothermal titration calorimetry results demonstrated that SAH binding greatly increases the affinity of TbPRMT6 to a substrate peptide derived from bovine histone H4. The western blotting and mass spectrometry results revealed that TbPRMT6 methylates bovine histone H4 tail at arginine 3 but cannot methylate several T. brucei histone tails. In summary, our results highlight the structural differences between TbPRMT6 and other type I PRMTs and reveal that the active site rearrangement upon SAH binding is important for the substrate binding of TbPRMT6.

  14. Photonic Crystal Structures with Tunable Structure Color as Colorimetric Sensors

    Science.gov (United States)

    Wang, Hui; Zhang, Ke-Qin

    2013-01-01

    Colorimetric sensing, which transduces environmental changes into visible color changes, provides a simple yet powerful detection mechanism that is well-suited to the development of low-cost and low-power sensors. A new approach in colorimetric sensing exploits the structural color of photonic crystals (PCs) to create environmentally-influenced color-changeable materials. PCs are composed of periodic dielectrics or metallo-dielectric nanostructures that affect the propagation of electromagnetic waves (EM) by defining the allowed and forbidden photonic bands. Simultaneously, an amazing variety of naturally occurring biological systems exhibit iridescent color due to the presence of PC structures throughout multi-dimensional space. In particular, some kinds of the structural colors in living organisms can be reversibly changed in reaction to external stimuli. Based on the lessons learned from natural photonic structures, some specific examples of PCs-based colorimetric sensors are presented in detail to demonstrate their unprecedented potential in practical applications, such as the detections of temperature, pH, ionic species, solvents, vapor, humidity, pressure and biomolecules. The combination of the nanofabrication technique, useful design methodologies inspired by biological systems and colorimetric sensing will lead to substantial developments in low-cost, miniaturized and widely deployable optical sensors. PMID:23539027

  15. Photonic Crystal Structures with Tunable Structure Color as Colorimetric Sensors

    Directory of Open Access Journals (Sweden)

    Ke-Qin Zhang

    2013-03-01

    Full Text Available Colorimetric sensing, which transduces environmental changes into visible color changes, provides a simple yet powerful detection mechanism that is well-suited to the development of low-cost and low-power sensors. A new approach in colorimetric sensing exploits the structural color of photonic crystals (PCs to create environmentally-influenced color-changeable materials. PCs are composed of periodic dielectrics or metallo-dielectric nanostructures that affect the propagation of electromagnetic waves (EM by defining the allowed and forbidden photonic bands. Simultaneously, an amazing variety of naturally occurring biological systems exhibit iridescent color due to the presence of PC structures throughout multi-dimensional space. In particular, some kinds of the structural colors in living organisms can be reversibly changed in reaction to external stimuli. Based on the lessons learned from natural photonic structures, some specific examples of PCs-based colorimetric sensors are presented in detail to demonstrate their unprecedented potential in practical applications, such as the detections of temperature, pH, ionic species, solvents, vapor, humidity, pressure and biomolecules. The combination of the nanofabrication technique, useful design methodologies inspired by biological systems and colorimetric sensing will lead to substantial developments in low-cost, miniaturized and widely deployable optical sensors.

  16. Elastic properties of Ti-24Nb-4Zr-8Sn single crystals with bcc crystal structure

    International Nuclear Information System (INIS)

    Zhang, Y.W.; Li, S.J.; Obbard, E.G.; Wang, H.; Wang, S.C.; Hao, Y.L.; Yang, R.

    2011-01-01

    Research highlights: → The single crystals of Ti2448 alloy with the bcc crystal structure were prepared. → The elastic moduli and constants were measured by several resonant methods. → The crystal shows significant elastic asymmetry in tension and compression. → The crystal exhibits weak nonlinear elasticity with large elastic strain ∼2.5%. → The crystal has weak atomic interactions against crystal distortion to low symmetry. - Abstract: Single crystals of Ti2448 alloy (Ti-24Nb-4Zr-8Sn in wt.%) were grown successfully using an optical floating-zone furnace. Several kinds of resonant methods gave consistent Young's moduli of 27.1, 56.3 and 88.1 GPa and shear moduli of 34.8, 11.0 and 14.6 GPa for the , and oriented single crystals, and C 11 , C 12 and C 44 of 57.2, 36.1 and 35.9 GPa respectively. Uniaxial testing revealed asymmetrical elastic behaviors of the crystals: tension caused elastic softening with a large reversible strain of ∼4% and a stress plateau of ∼250 MPa, whereas compression resulted in gradual elastic stiffening with much smaller reversible strain. The crystals exhibited weak nonlinear elasticity with a large elastic strain of ∼2.5% and a high strength, approaching ∼20% and ∼30% of its ideal shear and ideal tensile strength respectively. The crystals showed linear elasticity with a small elastic strain of ∼1%. These elastic deformation characteristics have been interpreted in terms of weakened atomic interactions against crystal distortion to low crystal symmetry under external applied stresses. These results are consistent with the properties of polycrystalline Ti2448, including high strength, low elastic modulus, large recoverable strain and weak strengthening effect due to grain refinement.

  17. New Mn(II, Ni(II, Cd(II, Pb(II complexes with 2-methylbenzimidazole and other ligands. Synthesis, spectroscopic characterization, crystal structure, magnetic susceptibility and biological activity studies

    Directory of Open Access Journals (Sweden)

    Shayma A. Shaker

    2016-11-01

    Full Text Available Synthesis and characterization of Mn(II, Ni(II, Cd(II and Pb(II mixed ligand complexes of 2-methylbenzimidazole with other ligands have been reported. The structure of the ligands and their complexes was investigated using elemental analysis, IR, UV–Vis, (1H, 13C NMR spectroscopy, molar conductivity and magnetic susceptibility measurements. In all the studies of complexes, the 2-methylbenzimidazole behaves as a neutral monodentate ligand which is coordinated with the metal ions through the N atom. While benzotriazole behaves as a neutral bidentate ligand which is coordinated with the Ni(II ion through the two N atoms. Moreover, the N-acetylglycine behaves as a bidentate ligand which is coordinated with the Mn(II, Ni(II and Pb(II ions through the N atom and the terminal carboxyl oxygen atom. The magnetic and spectral data indicate the tetrahedral geometry for Mn(II complex, irregular tetrahedral geometry for Pb(II complex and octahedral geometry for Ni(II complex. The X-ray single crystal diffraction method was used to confirm a centrosymmetric dinuclear Cd(II complex as each two metal ions are linked by a pair of thiocyanate N = S bridge. Two 2-methylbenzimidazole N-atom donors and one terminal thiocyanate N atom complete a highly distorted square pyramid geometry around the Cd atom. Besides, different cell types were used to determine the inhibitory effect of Mn(II, Ni(II, Cd(II and Pb(II complexes on cell growth using MTT assay. Cd(II complex showed cytotoxic effect on various types of cancer cell lines with different EC50 values.

  18. The crystal structure and twinning of neodymium gallium perovskite single crystals

    International Nuclear Information System (INIS)

    Ubizskii, S.B.; Vasylechko, L.O.; Savytskii, D.I.; Matkovskii, A.O.; Syvorotka, I.M.

    1994-01-01

    By means of X-ray structure analysis, the crystal structure of neodymium gallium perovskite (NGP) single crystals (NdGaO 3 ) being used as a substrate for HTSC film epitaxy has been refined and the position of atoms has been determined. The possibility of YBa 2 Cu 3 O 7-x film epitaxy on the plane (110) of NGP crystal as well as its advantages and pitfalls are analysed from structural data. The twinning types in the NGP crystal were established. The twinning structure of NGP substrates is found to be stable up to a temperature of 1173 K, as differentiated from the LaGaO 3 and LaAlO 3 substrates. It is intimated that the twinning in the NGP substrates oriented as (001) can result in creation of 90 degrees twin bonds in a film, and in the case of (110)-oriented plates it is possible to ignore the twinning presence in substrate completely. (author)

  19. Preparation and crystal structure of Ca4Sb2O

    International Nuclear Information System (INIS)

    Eisenmann, B.; Limartha, H.; Schaefer, H.

    1980-01-01

    The formerly described compound Ca 2 Sb is to be corrected to Ca 4 Sb 2 O as shown by X-ray diffractometer data of single crystals and neutron diffraction diagrams of powders. The compound crystallizes in the K 2 NiF 4 structure type. (orig.)

  20. Crystal structure of vanadite: Refinement of anisotropic displacement parameters

    Czech Academy of Sciences Publication Activity Database

    Laufek, F.; Skála, Roman; Haloda, J.; Císařová, I.

    2006-01-01

    Roč. 51, 3-4 (2006), s. 271-275 ISSN 1210-8197 Institutional research plan: CEZ:AV0Z30130516 Keywords : anisotropic displacement parameter * crystal structure * single-crystal X-ray refinement * vanadinite Subject RIV: DB - Geology ; Mineralogy

  1. Nucleation of colloidal crystals on configurable seed structures

    NARCIS (Netherlands)

    Hermes, M; Vermolen, E.C.M.; Leunissen, M.E.; Vossen, D.L.J.; van Oostrum, P.D.J.; Dijkstra, M.; van Blaaderen, A.

    2011-01-01

    Nucleation is an important stage in the growth of crystals. During this stage, the structure and orientation of a crystal are determined. However, short time- and length-scales make nucleation poorly understood. Micrometer-sized colloidal particles form an ideal model system to study nucleation due

  2. Structural characterization of electrodeposited boron

    Indian Academy of Sciences (India)

    Structural characterization of electrodeposited boron was carried out by using transmission electron microscopy and Raman spectroscopy. Electron diffraction and phase contrast imaging were carried out by using transmission electron microscopy. Phase identification was done based on the analysis of electron diffraction ...

  3. Characterization of Injection Molded Structures

    DEFF Research Database (Denmark)

    Sun, Ling; Søgaard, Emil; Andersen, Nis Korsgaard

    for different applications. We show how to correlate the structures of the polymer replicas with respect to their functionalities. Furthermore, we introduce how we coordinate with all partners in the “Nanoplast” project, and how we utilize the existing facilities of each method to understand structure......Microscopy has been widely applied to understand surface structures of solid samples. According to the instrumental methodology, there are different microscopy methods: optical microscopy, electron microscopy, and scanning probe microscopy (SPM). These microscopy methods have individual advantages...... and limitations. Therefore, it would be difficult to characterize complex, especially hierarchical structures by using only one method. Here we present a combined optical microscopy, scanning electron microscopy (SEM), and scanning probe microscopy study on injection molded structures. These structures are used...

  4. Structure of cleaved (001) USb2 single crystal

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Shao-ping [Los Alamos National Laboratory; Hawley, Marilyn [Los Alamos National Laboratory; Bauer, Eric D [Los Alamos National Laboratory; Stockum, Phil B [STANFORD UNIV.; Manoharan, Hari C [STANFORD UNIV

    2009-01-01

    We have achieved what we believe to be the first atomic resolution STM images for a uranium compound taken at room temperature. The a, b, and c lattice parameters in the images confirm that the USb{sub 2} crystals cleave on the (001) basal plane as expected. The a and b dimensions were equal, with the atoms arranged in a cubic pattern. Our calculations indicate a symmetric cut between Sb planes to be the most favorable cleavage plane and U atoms to be responsible for most of the DOS measured by STM. Some strange features observed in the STM will be discussed in conjunction with ab initio calculations. The purpose of this work is to demonstrate the power of scanning tunneling microscopy (STM) techniques combined with a theoretical underpinning to determine the surface atomic structure and properties of actinide materials, such as the quasi 2-dimensional uranium dipnictide USb{sub 2} single crystal, thereby contributing to the understanding of their surface structural and electronic properties. The members of this interesting UX{sub 2} (X=P, As, Sb, Bi) series of compounds display dual localized and itinerant 5f electron behavior within the same compound due to the hybridization of the 5f orbitals with the conduction band. With the exception of UO{sub 2}, which has to be studied at elevated temperature to generate enough carriers for STM imaging, STM techniques have not been applied successfully to the characterization of the surface atomic structure of any other single crystal actinide compound, to the best of our knowledge. However, STM has been used to a limited extent for the study of some cerium compounds. STM probes electronic properties at the atomic level and can directly provide information about the local density of filled and empty states (LDOS) states simultaneously. A STM topograph provides the local atomic arrangement and spacing of the atoms on the surface, local defect structures (e.g. steps, vacancies, and kink sites) and the presence of contaminants

  5. Ultrasonic characterization of pork fat crystallization during cold storage.

    Science.gov (United States)

    Corona, Edith; García-Pérez, José V; Santacatalina, Juan V; Ventanas, Sonia; Benedito, José

    2014-05-01

    In this work, the feasibility of using ultrasonic velocity measurements for characterizing and differentiating the crystallization pattern in 2 pork backfats (Montanera and Cebo Iberian fats) during cold storage (0 °C, 2 °C, 5 °C, 7 °C, and 10 °C) was evaluated. The fatty acid profile, thermal behavior, and textural properties (hardness) of fat were also determined. Both fats became harder during cold storage (average hardness increase for both fats, 11.5 N, 8 N, and 1.8 N at 0, °C 2 °C, and 5 °C , respectively), showing a 2-step pattern related with the separate crystallization of the different existing triacylglycerols, which was well described using a modified Avrami equation (explained variance > 99%). Due to a greater content of saturated triacylglycerols, Cebo fat (45.1%) was harder than Montanera (41.8%). The ultrasonic velocity followed a similar 2-step pattern to hardness during cold storage, being found an average increase for both fats of 184, 161, and 150 m/s at 0 °C 2 °C, and 5 °C, respectively. Thus, ultrasonic measurements were useful both to characterize the textural changes taking place during cold storage and to differentiate between fats with different composition. The cold storage of dry-cured meat products during their distribution and retail sale exert an important effect on their textural properties and consumers' acceptance due to the crystallization of the fat fraction, which is greatly influenced by the type of fat. In this work, a nondestructive ultrasonic technique was used to identify the textural changes provoked by the crystallization during cold storage, and to differentiate between fats, which could be used for quality control purposes. © 2014 Institute of Food Technologists®

  6. Synthesis and Characterization of Photo-Responsive Thermotropic Liquid Crystals Based on Azobenzene

    Directory of Open Access Journals (Sweden)

    Runmiao Yang

    2018-03-01

    Full Text Available A series of new thermotropic liquid crystals (LCs containing azobenzene units was synthesized. The structures of the compounds were characterized by means of NMR and FTIR spectroscopy. Their mesomorphic behaviors were investigated via differential scanning calorimetry (DSC and polarizing optical microscopy (POM. Based on the POM and DSC measurements, the optical properties of the Razo-ester were tested using UV-vis spectroscopy. The azobenzene side chain displayed a strong ability to influence the formation of thermotropic LCs.

  7. Engineering and Characterizing Light-Matter Interactions in Photonic Crystals

    Science.gov (United States)

    2010-01-01

    SU8 monomer has, on average, eight epoxy groups, that under go a ring-opening polymerization in the presence of an acid catalyst. SU8 falls into...copper oxide [49] into colloidal and SU8 polymer photonic crystal templates, respectively. 1.5.2 Gas-Phase Infilling Gas-phase deposition typically...resist using direct laser writing. 78 Figure 2. Scanning electron micrograph of an over- polymerized woodpile structure fabricated in SU8 photo-resist

  8. Acquisition of Single Crystal Growth and Characterization Equipment. Final report

    International Nuclear Information System (INIS)

    Maple, M. Brian; Zocco, Diego A.

    2008-01-01

    Final Report for DOE Grant No. DE-FG02-04ER46178 'Acquisition of Single Crystal Growth and Characterization Equipment'. There is growing concern in the condensed matter community that the need for quality crystal growth and materials preparation laboratories is not being met in the United States. It has been suggested that there are too many researchers performing measurements on too few materials. As a result, many user facilities are not being used optimally. The number of proficient crystal growers is too small. In addition, insufficient attention is being paid to the enterprise of finding new and interesting materials, which is the driving force behind much of condensed matter research and, ultimately, technology. While a detailed assessment of this situation is clearly needed, enough evidence of a problem already exists to compel a general consensus that the situation must be addressed promptly. This final report describes the work carried out during the last four years in our group, in which a state-of-the-art single crystal growth and characterization facility was established for the study of novel oxides and intermetallic compounds of rare earth, actinide and transition metal elements. Research emphasis is on the physics of superconducting (SC), magnetic, heavy fermion (HF), non-Fermi liquid (NFL) and other types of strongly correlated electron phenomena in bulk single crystals. Properties of these materials are being studied as a function of concentration of chemical constituents, temperature, pressure, and magnetic field, which provide information about the electronic, lattice, and magnetic excitations at the root of various strongly correlated electron phenomena. Most importantly, the facility makes possible the investigation of material properties that can only be achieved in high quality bulk single crystals, including magnetic and transport phenomena, studies of the effects of disorder, properties in the clean limit, and spectroscopic and scattering

  9. Crystal structure and crystal growth of the polar ferrimagnet CaBaFe4O7

    Science.gov (United States)

    Perry, R. S.; Kurebayashi, H.; Gibbs, A.; Gutmann, M. J.

    2018-05-01

    Magnetic materials are a cornerstone for developing spintronic devices for the transport of information via magnetic excitations. To date, relatively few materials have been investigated for the purpose of spin transport, mostly due to the paucity of suitable candidates as these materials are often chemically complex and difficult to synthesize. We present the crystal growth and a structure solution on the high-temperature crystal structure of the layered, polar ferrimagnet CaBaFe4O7 , which is a possible new contender for spintronics research. The space group is identified as P 3 by refinement of single crystal and powder neutron diffraction data. At 400 K, the trigonal lattice parameters are a =11.0114 (11 )Å and c =10.330 (3 )Å . The structure is similar to the low-temperature phase with alternating layers of triangular and Kagome-arranged Fe-O tetrahedra. We also present details of the crystal growth by traveling solvent method.

  10. Synthesis, crystal structure and Thermogravimetry of ortho-phthalic ...

    Indian Academy of Sciences (India)

    satisfied by two chelated carboxylates while fifth and sixth co-ordination positions are satisfied by monodentate ... Keywords. o-Phthalic acid; coordination polymer; X-ray crystal structure; Copper(II); EPR; TGA. 1. .... Absorption coefficient.

  11. Crystal structure and pair potentials: A molecular-dynamics study

    Energy Technology Data Exchange (ETDEWEB)

    Parrinello, M.; Rahman, A.

    1980-10-06

    With use of a Lagrangian which allows for the variation of the shape and size of the periodically repeating molecular-dynamics cell, it is shown that different pair potentials lead to different crystal structures.

  12. Phase relations, crystal structures and physical properties of nuclear fuels

    International Nuclear Information System (INIS)

    Tagawa, Hiroaki; Fujino, Takeo; Tateno, Jun

    1975-07-01

    Phase relations, crystal structures and physical properties of the compounds for nuclear fuels are presented, including melting point, thermal expansion, diffusion and magnetic and electric properties. Emphasis is on oxides, carbides and nitrides of thorium, uranium and plutonium. (auth.)

  13. Growth and characterization of calcium hydrogen phosphate dihydrate crystals from single diffusion gel technique

    Energy Technology Data Exchange (ETDEWEB)

    Rajendran, K.; Dale Keefe, C. [Department of Chemistry, Cape Breton University, Sydney, Nova Scotia (Canada)

    2010-09-15

    Calcium hydrogen phosphate dihydrate (CaHPO{sub 4}.2H{sub 2}O, CHPD) a dissolved mineral in urine is known to cause renal or bladder stones in both human and animals. Growth of CHPD or brushite using sodium metasilicate gel techniques followed by light and polarizing microscopic studies revealed its structural and morphological details. Crystal identity by powder x-ray diffraction confirmed the FT-IR and FT-Raman spectroscopic techniques as alternate methods for fast analysis of brushite crystals which could form as one type of renal stones. P-O-P asymmetric stretchings in both FT-IR (987.2, 874.1 and 792 cm{sup -1}) and FT-Raman (986.3 cm{sup -1}, 1057.6 cm{sup -1} and 875.2 cm{sup -1}) were found as characteristics of brushite crystals. Differential Scanning Calorimetry (DSC) analysis revealed brushite crystallization purity using gel method by studying their endothermic peaks. This study incorporated a multidisciplinary approach in characterizing CHPD crystals grown in vitro to help formulate prevention or dissolution strategy in controlling urinary stone growth. Initial studies with 0.2 M citric acid ions as controlling agent in the nucleation of brushite crystals further support the presented approach. (copyright 2010 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  14. Crystal structure, thermal behavior, vibrational spectroscopy and ...

    Indian Academy of Sciences (India)

    64

    A single crystal was carefully selected under polarizing microscope and .... properties of our compound using infrared absorption and Raman scattering. ... pics in Raman at 1762 and 1782 cm-1 are assigned to the δ(HOH) mode of the water ...

  15. Formation of structured nanophases in halide crystals

    Czech Academy of Sciences Publication Activity Database

    Kulveit, Jan; Demo, Pavel; Polák, Karel; Sveshnikov, Alexey; Kožíšek, Zdeněk

    2013-01-01

    Roč. 5, č. 6 (2013), s. 561-564 ISSN 2164-6627 R&D Projects: GA ČR GAP108/12/0891 Institutional support: RVO:68378271 Keywords : halide crystals * nucleation Subject RIV: BM - Solid Matter Physics ; Magnetism http://www.aspbs.com/asem.html#v5n6

  16. Solvothermal syntheses, crystal structures, optical and thermal ...

    Indian Academy of Sciences (India)

    compounds 1–3 exhibit optical band gaps between 2.06 and 2.35 eV. Keywords. .... under a nitrogen stream of 100 mL min. −1 . 2.3 X-ray diffraction. Single-crystal ..... Liu G N, Guo G C, Wang M S, Cai L Z and Huang J S. 2010 Five dimeric ...

  17. The crystal structure of tRNA

    Indian Academy of Sciences (India)

    Madhu

    of yeast alanine tRNA by Robert Holley's group at Cornell. University ... decode nonsense codons) with John Smith and Brenner. However, my ... tRNA from 10 g of unfractionated tRNA. ... tRNA crystals were, in fact, protein (Hendrikson et al.

  18. Hydrothermal syntheses and single crystal structural ...

    Indian Academy of Sciences (India)

    Unknown

    Colourless. 84 lined stainless steel bomb. After heating in a pro- grammable oven at the respective temperatures and autogenous pressures for the notified time scale, cooling was carried out on a ramp of 10°C/h to room temperature. The crystals were collected by filtration, washed with, deionized water followed by diethyl-.

  19. Construction of crystal structure prototype database: methods and applications

    International Nuclear Information System (INIS)

    Su, Chuanxun; Lv, Jian; Wang, Hui; Wang, Yanchao; Ma, Yanming; Li, Quan; Zhang, Lijun

    2017-01-01

    Crystal structure prototype data have become a useful source of information for materials discovery in the fields of crystallography, chemistry, physics, and materials science. This work reports the development of a robust and efficient method for assessing the similarity of structures on the basis of their interatomic distances. Using this method, we proposed a simple and unambiguous definition of crystal structure prototype based on hierarchical clustering theory, and constructed the crystal structure prototype database (CSPD) by filtering the known crystallographic structures in a database. With similar method, a program structure prototype analysis package (SPAP) was developed to remove similar structures in CALYPSO prediction results and extract predicted low energy structures for a separate theoretical structure database. A series of statistics describing the distribution of crystal structure prototypes in the CSPD was compiled to provide an important insight for structure prediction and high-throughput calculations. Illustrative examples of the application of the proposed database are given, including the generation of initial structures for structure prediction and determination of the prototype structure in databases. These examples demonstrate the CSPD to be a generally applicable and useful tool for materials discovery. (paper)

  20. Construction of crystal structure prototype database: methods and applications.

    Science.gov (United States)

    Su, Chuanxun; Lv, Jian; Li, Quan; Wang, Hui; Zhang, Lijun; Wang, Yanchao; Ma, Yanming

    2017-04-26

    Crystal structure prototype data have become a useful source of information for materials discovery in the fields of crystallography, chemistry, physics, and materials science. This work reports the development of a robust and efficient method for assessing the similarity of structures on the basis of their interatomic distances. Using this method, we proposed a simple and unambiguous definition of crystal structure prototype based on hierarchical clustering theory, and constructed the crystal structure prototype database (CSPD) by filtering the known crystallographic structures in a database. With similar method, a program structure prototype analysis package (SPAP) was developed to remove similar structures in CALYPSO prediction results and extract predicted low energy structures for a separate theoretical structure database. A series of statistics describing the distribution of crystal structure prototypes in the CSPD was compiled to provide an important insight for structure prediction and high-throughput calculations. Illustrative examples of the application of the proposed database are given, including the generation of initial structures for structure prediction and determination of the prototype structure in databases. These examples demonstrate the CSPD to be a generally applicable and useful tool for materials discovery.

  1. Crystal habit, characterization and pharmacological activity of various crystal forms of arteether

    Directory of Open Access Journals (Sweden)

    Renu Chadha

    2011-08-01

    Full Text Available The aim of this study was to investigate and characterize different crystal forms of arteether, a rapidly acting, highly potent antimalarial drug for the treatment of acute Plasmodium falciparum malaria. Six different crystal forms were prepared utilizing various polar and non-polar solvents. Scanning electron microscopy (SEM revealed differences in the surface characteristics of the six forms from those of a commercial sample. Differential scanning calorimetry (DSC revealed the absence of a desolvation endotherm indicating that the forms were neither hydrates nor solvates. Powder X-ray diffraction (PXRD patterns of the forms showed much weaker major peaks than in the commercial sample indicating them to be less crystalline. Solubility and dissolution studies showed that the most amorphous form was the most soluble and possessed the highest antimalarial activity.

  2. Electroerosion impulse effect on W single crystal structure

    International Nuclear Information System (INIS)

    Aleshina, S.A.; Khvostikova, V.D.; Zolotykh, B.N.; Marchuk, A.I.

    1977-01-01

    The mechanism has been studied of brittle failure of single crystal tungsten on planes of crystallographic orientations [100], [110]; [111] in the process of electro-erosion machining by pulses of energies ranging from 1200 to 5000 μJ and of duration of 1 μs. It is shown that the electro-erosion machining of single crystal tungsten is characterized by the formation of a defect layer with a grid of microcracks which lie at a depth of approximately 80 μm. The appearance and the distribution of cracks on the surface of single crystals depends on the crystallogrpahic orientation

  3. Fully automatic characterization and data collection from crystals of biological macromolecules.

    Science.gov (United States)

    Svensson, Olof; Malbet-Monaco, Stéphanie; Popov, Alexander; Nurizzo, Didier; Bowler, Matthew W

    2015-08-01

    Considerable effort is dedicated to evaluating macromolecular crystals at synchrotron sources, even for well established and robust systems. Much of this work is repetitive, and the time spent could be better invested in the interpretation of the results. In order to decrease the need for manual intervention in the most repetitive steps of structural biology projects, initial screening and data collection, a fully automatic system has been developed to mount, locate, centre to the optimal diffraction volume, characterize and, if possible, collect data from multiple cryocooled crystals. Using the capabilities of pixel-array detectors, the system is as fast as a human operator, taking an average of 6 min per sample depending on the sample size and the level of characterization required. Using a fast X-ray-based routine, samples are located and centred systematically at the position of highest diffraction signal and important parameters for sample characterization, such as flux, beam size and crystal volume, are automatically taken into account, ensuring the calculation of optimal data-collection strategies. The system is now in operation at the new ESRF beamline MASSIF-1 and has been used by both industrial and academic users for many different sample types, including crystals of less than 20 µm in the smallest dimension. To date, over 8000 samples have been evaluated on MASSIF-1 without any human intervention.

  4. Structural transitions in crystals of native aspartate carbamoyltransferase

    International Nuclear Information System (INIS)

    Gouaux, J.E.; Lipscomb, W.N.

    1989-01-01

    Screened precession x-ray photographs of crystals of native aspartate carbamoyltransferase ligated with L-aspartate and phosphate reveal the presence of a crystal unit-cell dimension that is intermediate between the T (tense) and R (relaxed) states. Characterizing the intermediate (I) crystal is a c-axis unit-cell dimension of 149 angstrom, halfway between the c-axis length of the T (c = 142 angstrom) and R (c = 156 angstrom) states, in the space group P321. Preservation of the P321 space group indicates that the intermediate crystal form retains a threefold axis of symmetry, and therefore the enzyme has at minimum a threefold axis; however, it is not known whether the molecular twofold axis is conserved. The I crystals are formed by soaking T-state crystals with L-aspartate and phosphate. By raising the concentration of L-aspartate the authors can further transform the I crystals, without fragmentation, to a form that has the same unit-cell dimensions as R-state crystals grown in the presence of N-(phosphonoacetyl)-L-aspartate

  5. Interfacial ordering of thermotropic liquid crystals triggered by the secondary structures of oligopeptides.

    Science.gov (United States)

    Wang, Xiaoguang; Yang, Pei; Mondiot, Frederic; Li, Yaoxin; Miller, Daniel S; Chen, Zhan; Abbott, Nicholas L

    2015-12-07

    We report that assemblies formed by eight oligopeptides at phospholipid-decorated interfaces of thermotropic liquid crystals (LCs) trigger changes in ordering of the LCs that are dependent on the secondary structures of the oligopeptides (as characterized in situ using infrared-visible sum-frequency spectroscopy).

  6. Solid-state syntheses and single-crystal characterizations of three tetravalent thorium and uranium silicates

    International Nuclear Information System (INIS)

    Jin, Geng Bang; Soderholm, L.

    2015-01-01

    Colorless crystals of ThSiO 4 (huttonite) (1) and (Ca 0.5 Na 0.5 ) 2 NaThSi 8 O 20 (2) have been synthesized by the solid-state reactions of ThO 2 , CaSiO 3 , and Na 2 WO 4 at 1073 K. Green crystals of (Ca 0.5 Na 0.5 ) 2 NaUSi 8 O 20 (3) have been synthesized by the solid-state reactions of UO 2 , CaSiO 3 , and Na 2 WO 4 at 1003 K. All three compounds have been characterized by single-crystal X-ray diffraction. Compound 1 adopts a monazite-type three-dimensional condensed structure, which is built from edge- and corner-shared ThO 9 polyhedra and SiO 4 tetrahedra. Compounds 2 and 3 are isostructural and they crystallize in a steacyite-type structure. The structure consists of discrete pseudocubic [Si 8 O 20 ] 8− polyanions, which are connected by An 4+ cations into a three-dimensional framework. Each An atom coordinates to eight monodentate [Si 8 O 20 ] 8− moieties in a square antiprismatic geometry. Na + and Ca 2+ ions reside in the void within the framework. Raman spectra of 1, 2, and 3 were collected on single crystal samples. 1 displays more complex vibrational bands than thorite. Raman spectra of 2 and 3 are analogous with most of vibrational bands located at almost the same regions. - Graphical abstract: A Raman spectrum and crystal structures of (Ca 0.5 Na 0.5 ) 2 NaAnSi 8 O 20 (An=Th, U), which contain pseudocubic [Si 8 O 20 ] 8− polyanions and eight-coordinate An 4+ cations. - Highlights: • Single crystal growth of three tetravalent actinide silicates from melts. • Single-crystal structures and Raman spectra of (Ca 0.5 Na 0.5 ) 2 NaAnSi 8 O 20 (An=Th, U). • First report of Raman spectrum of huttonite on single crystal samples

  7. Crystal structure of actinide metals at high compression

    International Nuclear Information System (INIS)

    Fast, L.; Soederlind, P.

    1995-08-01

    The crystal structures of some light actinide metals are studied theoretically as a function of applied pressure. The first principles electronic structure theory is formulated in the framework of density functional theory, with the gradient corrected local density approximation of the exchange-correlation functional. The light actinide metals are shown to be well described as itinerant (metallic) f-electron metals and generally, they display a crystal structure which have, in agreement with previous theoretical suggestions, increasing degree of symmetry and closed-packing upon compression. The theoretical calculations agree well with available experimental data. At very high compression, the theory predicts closed-packed structures such as the fcc or the hcp structures or the nearly closed-packed bcc structure for the light actinide metals. A simple canonical band picture is presented to explain in which particular closed-packed form these metals will crystallize at ultra-high pressure

  8. Synthesis of rare-earth selenate and selenite materials under 'sol-gel' hydrothermal conditions: crystal structures and characterizations of La(HSeO3)(SeO4) and KNd(SeO4)2

    International Nuclear Information System (INIS)

    Liu Wei; Chen Haohong; Yang Xinxin; Li Mangrong; Zhao Jingtai

    2004-01-01

    Two rare-earth compounds containing selenium atoms, La(HSeO 3 )(SeO 4 ) with a new open framework structure and KNd(SeO 4 ) 2 with a layered structure, have been synthesized under ''sol-gel'' hydrothermal conditions for the first time. Single-crystals of La(HSeO 3 )(SeO 4 ) crystallize in the monoclinic system (P2 1 , a=8.5905(17)A, b=7.2459(14)A, c=9.5691(19)A, β=104.91(3) o , Z=2, RAll=0.032). The structure contains puckered polyhedral layers made of LaO x (x=9,10) and SeO 4 groups, which are connected via SeO 3 -uints to the 3D structure. The crytal structure of KNd(SeO 4 ) 2 (monoclinc, P2 1 /c, a=8.7182(17)A, b=7.3225(15)A, c=11.045(2)A, β=91.38(3) o , Z=4, RAll=0.051) contains honeycomb-like six-ring NdO 9 polyhedra forming layers which are further decorated with SeO 4 tetrahedra. The K + ions occupy the interspaces of these layers and provide the charge balance

  9. Probing Zeolite Crystal Architecture and Structural Imperfections using Differently Sized Fluorescent Organic Probe Molecules.

    Science.gov (United States)

    Hendriks, Frank C; Schmidt, Joel E; Rombouts, Jeroen A; Lammertsma, Koop; Bruijnincx, Pieter C A; Weckhuysen, Bert M

    2017-05-05

    A micro-spectroscopic method has been developed to probe the accessibility of zeolite crystals using a series of fluorescent 4-(4-diethylaminostyryl)-1-methylpyridinium iodide (DAMPI) probes of increasing molecular size. Staining large zeolite crystals with MFI (ZSM-5) topology and subsequent mapping of the resulting fluorescence using confocal fluorescence microscopy reveal differences in structural integrity: the 90° intergrowth sections of MFI crystals are prone to develop structural imperfections, which act as entrance routes for the probes into the zeolite crystal. Polarization-dependent measurements provide evidence for the probe molecule's alignment within the MFI zeolite pore system. The developed method was extended to BEA (Beta) crystals, showing that the previously observed hourglass pattern is a general feature of BEA crystals with this morphology. Furthermore, the probes can accurately identify at which crystal faces of BEA straight or sinusoidal pores open to the surface. The results show this method can spatially resolve the architecture-dependent internal pore structure of microporous materials, which is difficult to assess using other characterization techniques such as X-ray diffraction. © 2017 The Authors. Published by Wiley-VCH Verlag GmbH & Co. KGaA.

  10. The crystal structure of the phosphatidylinositol 4-kinase IIalpha

    Czech Academy of Sciences Publication Activity Database

    Bäumlová, Adriana; Chalupská, Dominika; Rozycki, B.; Jovic, M.; Wisniewski, E.; Klíma, Martin; Dubánková, Anna; Kloer, D. P.; Nencka, Radim; Balla, T.; Bouřa, Evžen

    2015-01-01

    Roč. 22, č. 1 (2015), s. 5 ISSN 1211-5894. [Discussions in Structural Molecular Biology. Annual Meeting of the Czech Society for Structural Biology /13./. 19.03.2015-21.03.2015, Nové Hrady] EU Projects: European Commission(XE) 333916 - STARPI4K Institutional support: RVO:61388963 Keywords : PI4K IIalpha * crystal structure Subject RIV: CE - Biochemistry

  11. Crystallization and preliminary X-ray characterization of the nitrile reductase QueF: a queuosine-biosynthesis enzyme

    International Nuclear Information System (INIS)

    Swairjo, Manal A.; Reddy, Robert R.; Lee, Bobby; Van Lanen, Steven G.; Brown, Shannon; Crécy-Lagard, Valérie de; Iwata-Reuyl, Dirk; Schimmel, Paul

    2005-01-01

    Structural informatics and modelling correctly predicted that substrate was required to obtain diffracting crystals of the first characterized nitrile oxidoreductase: the homododecameric QueF. QueF (MW = 19.4 kDa) is a recently characterized nitrile oxidoreductase which catalyzes the NADPH-dependent reduction of 7-cyano-7-deazaguanine (preQ 0 ) to 7-aminomethyl-7-deazaguanine, a late step in the biosynthesis of the modified tRNA nucleoside queuosine. Initial crystals of homododecameric Bacillus subtilis QueF diffracted poorly to 8.0 Å. A three-dimensional model based on homology with the tunnel-fold enzyme GTP cyclohydrolase I suggested catalysis at intersubunit interfaces and a potential role for substrate binding in quaternary structure stabilization. Guided by this insight, a second crystal form was grown that was strictly dependent on the presence of preQ 0 . This crystal form diffracted to 2.25 Å resolution

  12. Crystal Structure of the Marburg Virus VP35 Oligomerization Domain

    Energy Technology Data Exchange (ETDEWEB)

    Bruhn, Jessica F.; Kirchdoerfer, Robert N.; Urata, Sarah M.; Li, Sheng; Tickle, Ian J.; Bricogne, Gérard; Saphire, Erica Ollmann (Scripps); (Globel Phasing); (UCSD)

    2016-11-09

    ABSTRACT

    Marburg virus (MARV) is a highly pathogenic filovirus that is classified in a genus distinct from that of Ebola virus (EBOV) (generaMarburgvirusandEbolavirus, respectively). Both viruses produce a multifunctional protein termed VP35, which acts as a polymerase cofactor, a viral protein chaperone, and an antagonist of the innate immune response. VP35 contains a central oligomerization domain with a predicted coiled-coil motif. This domain has been shown to be essential for RNA polymerase function. Here we present crystal structures of the MARV VP35 oligomerization domain. These structures and accompanying biophysical characterization suggest that MARV VP35 is a trimer. In contrast, EBOV VP35 is likely a tetramer in solution. Differences in the oligomeric state of this protein may explain mechanistic differences in replication and immune evasion observed for MARV and EBOV.

    IMPORTANCEMarburg virus can cause severe disease, with up to 90% human lethality. Its genome is concise, only producing seven proteins. One of the proteins, VP35, is essential for replication of the viral genome and for evasion of host immune responses. VP35 oligomerizes (self-assembles) in order to function, yet the structure by which it assembles has not been visualized. Here we present two crystal structures of this oligomerization domain. In both structures, three copies of VP35 twist about each other to form a coiled coil. This trimeric assembly is in contrast to tetrameric predictions for VP35 of Ebola virus and to known structures of homologous proteins in the measles, mumps, and Nipah viruses. Distinct oligomeric states of the Marburg and Ebola virus VP35 proteins may explain differences between them in polymerase function and immune evasion. These findings may provide a more accurate understanding of the

  13. Structure of initial crystals formed during human amelogenesis

    Science.gov (United States)

    Cuisinier, F. J. G.; Voegel, J. C.; Yacaman, J.; Frank, R. M.

    1992-02-01

    X-ray diffraction analysis revealed only the existence of carbonated hydroxyapatite (c.HA) during amelogenesis, whereas conventional transmission electron microscopy investigations showed that developing enamel crystals have a ribbon-like habit. The described compositional changes could be an indication for the presence of minerals different from c.HA. However, the absence of identification of such a mineral shows the need of studies by high resolution electron microscopy (HREM) of initial formed human enamel crystals. We demonstrate the existence of two crystal families involved in the early stages of biomineralization: (a) nanometer-size particles which appeared as a precursor phase; (b) ribbon-like crystals, with a structure closely related to c.HA, which by a progressive thickening process tend to attain the mature enamel crystal habit.

  14. Characterization of lime mortar additivated with crystallization modifiers

    NARCIS (Netherlands)

    Granneman, S.J.C.; Lubelli, B.; van Hees, R.P.J.

    2018-01-01

    Additivating mortars with crystallization modifiers is a novel approach to mitigate salt crystallization damage in historic masonry. Once verified the effectiveness of crystallization modifiers in bulk solution, the next step consists in verifying whether: (i) modifiers are still effective when

  15. Synthesis and characterization of gel-grown cobalt tartrate crystals

    Indian Academy of Sciences (India)

    ... in electronics, optics and industries. A series of pure and mixed crystals ... bility method. A few researchers reported the growth of crystals of strontium tartrate ... grow it by chemical reaction method using the gel technique. The crystallization ...

  16. Crystal growth and characterization of Tm doped mixed rare-earth aluminum perovskite

    Energy Technology Data Exchange (ETDEWEB)

    Totsuka, Daisuke, E-mail: totsuka@imr.tohoku.ac.jp [Institute for Materials Research, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai, Miyagi 980-8577 (Japan); Nihon Kessho Kogaku Co., Ltd., 810-5 Nobe-cho, Tatebayashi, Gunma 374-0047 (Japan); Yanagida, Takayuki [New Industry Creation Hatchery Center (NICHe), 6-6-10 Aoba, Aramaki, Aoba-ku, Sendai, Miyagi 980-8579 (Japan); Sugiyama, Makoto; Fujimoto, Yutaka; Yokota, Yuui [Institute for Materials Research, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai, Miyagi 980-8577 (Japan); Yoshikawa, Akira [Institute for Materials Research, Tohoku University, 2-1-1 Katahira, Aoba-ku, Sendai, Miyagi 980-8577 (Japan); New Industry Creation Hatchery Center (NICHe), 6-6-10 Aoba, Aramaki, Aoba-ku, Sendai, Miyagi 980-8579 (Japan)

    2012-04-15

    Highlights: Black-Right-Pointing-Pointer (Lu{sub x}Gd{sub y}Y{sub 0.99-x-y}Tm{sub 0.01})AP single crystals were grown by the {mu}-PD method. Black-Right-Pointing-Pointer The grown crystals were single phase with perovskite structure (Pbnm). Significant segregation of Lu and Gd was detected in the growth direction. Black-Right-Pointing-Pointer Some absorption bands due to Tm{sup 3+}, Gd{sup 3+} and color centers were exhibited. Black-Right-Pointing-Pointer Radioluminescence spectra showed several emission peaks ascribed to Tm{sup 3+} and Gd{sup 3+}. -- Abstract: In this work, we present results of structural characterization and optical properties including radio luminescence of (Lu{sub x}Gd{sub y}Y{sub 0.99-x-y}Tm{sub 0.01})AP single crystal scintillators for (x, y) = (0.30, 0.19), (0, 0.19) and (0, 0) grown by the micro-pulling-down ({mu}-PD) method. The grown crystals were single phase materials with perovskite structure (Pbnm) as confirmed by XRD and had a good crystallinity. The distribution of the crystal constituents in growth direction was evaluated, and significant segregation of Lu and Gd was detected in (Lu{sub 0.30}Gd{sub 0.19}Y{sub 0.50}Tm{sub 0.01})AP sample. The crystals demonstrated 70% transmittance in visible wavelength range and some absorption bands due to Tm{sup 3+}, Gd{sup 3+} and color centers were exhibited in 190-900 nm. The radioluminescence measurement under X-ray irradiation demonstrated several emission peaks ascribed to 4f-4f transitions of Tm{sup 3+} and Gd{sup 3+}. The ratio of emission intensity in longer wavelength range was increased when Y was replaced by Lu or Gd.

  17. Synthesis and Single Crystal Structures of Substituted-1,3-Selenazol-2-amines

    Directory of Open Access Journals (Sweden)

    Guoxiong Hua

    2016-12-01

    Full Text Available The synthesis and X-ray single crystal structures of a series of new 4-substituted-1,3-selenazol-2-amines is reported. The efficient preparation of these compounds was carried out by two-component cyclization of the selenoureas with equimolar amounts of α-haloketones. The selenoureas were obtained from the reaction of Woollins’ reagent with cyanamides, followed by hydrolysis with water. All new compounds have been characterized by IR spectroscopy, multi-NMR (1H, 13C, 77Se spectroscopy, accurate mass measurement and single crystal X-ray structure analysis.

  18. Optical and Structural Characterizations of GaN Nano structures

    International Nuclear Information System (INIS)

    Shekari, L.; Abu Hassan, H.; Thahab, S.M.

    2011-01-01

    We have grown wurtzite GaN nano wires (NWs) on polished silicon (Si) either with or without Au as catalyst, using commercial GaN powder by thermal evaporation in an atmosphere of argon (Ar) gas. Structural and optical characterizations were performed using high resolution X-ray diffraction (HR-XRD), scanning electron microscopy (SEM), photoluminescence (PL) and energy-dispersive X-ray spectroscopy (EDX) spectroscopy. Results indicate that the nano wires are of single-crystal hexagonal GaN and the nano wires on Si with Au catalyst are more oriented than those without Au catalyst; and using catalyst make the NWs grow much faster and quite well-ordered. The compositional quality of the grown nano wires on the substrates are mostly same, however the nano wires on the Au coated silicon are of low density, while the nano wires on the Si are of high density. (author)

  19. Synthesis, crystal structures and properties of new quinolinium derivatives

    Science.gov (United States)

    Zhang, Xinyuan; Jiang, Xingxing; Li, Yin; Lin, Zheshuai; Zhang, Guochun; Wu, Yicheng

    2015-11-01

    Four phenyl-substituted quinolinium salts with different counter anions, C27H27NO4S, C26H25NO5S, C25H22NO5SCl, and C25H22NO5SBr, were synthesized and their single crystals were successfully grown from methanol solution by slow evaporation. Single crystal X-ray diffraction analyses showed that C27H27NO4S crystal belongs to the noncentrosymmetric orthorhombic space group Pna21, and the other three crystals belong to centrosymmetric monoclinic space group P21/n. Their first order hyperpolarization and macroscopic nonlinearity were analyzed and physical properties were characterized by UV-vis absorption spectroscopy, and differential scanning calorimetric and thermal gravimetric analysis.

  20. Preparation and characterization of single-crystal multiferroic nanofiber composites

    Energy Technology Data Exchange (ETDEWEB)

    Ren, Zhaohui; Xiao, Zhen; Yin, Simin; Mai, Jiangquan; Liu, Zhenya; Xu, Gang; Li, Xiang; Shen, Ge [State Key Lab of Silicon Materials, Department of Material Science and Engineering, Cyrus Tang Center for Sensor Materials and Applications, Zhejiang University, Hangzhou 310027 (China); Han, Gaorong, E-mail: hgr@zju.edu.cn [State Key Lab of Silicon Materials, Department of Material Science and Engineering, Cyrus Tang Center for Sensor Materials and Applications, Zhejiang University, Hangzhou 310027 (China)

    2013-03-05

    Graphical abstract: One-dimensional single-crystal multiferroic composites composed of PbTiO{sub 3} nanofiber-CoFe{sub 2}O{sub 4} nanodot have been prepared for the first time by a facile in situ solid state sintering method. The composites demonstrate ferroelectricity and ferromagnetism as well as strong coupling between them. Highlights: ► 1D single-crystal multiferroic PTO-CFO was prepared via in situ solid state sintering method. ► A simple epitaxial growth relation has been found between the PTO–CFO composites. ► The composites reveal ferroelectricity and ferromagnetism as well as coupling between them. -- Abstract: One-dimensional single-crystal multiferroic composites consisting of PbTiO{sub 3} (PTO) nanofiber-CoFe{sub 2}O{sub 4} (CFO) nanodot were prepared using an in situ solid state sintering method, where pre-perovskite PTO nanofibers and CFO nanodots were used as precursors. Structural analyses by using transmission electron microscopy, scanning electron microscopy and X-ray diffraction determined a epitaxial growth relation between the PTO nanofiber and the CFO nanodot. Ferromagnetism and ferroelectricity of the nanofiber composites were investigated by using vibarting sample magnetometer (VSM) and piezoresponse force microscopy (PFM)

  1. Surface characterization of amorphous and crystallized Fe 80B 20

    Science.gov (United States)

    Huntley, D. R.; Overbury, S. H.; Zehner, D. M.; Budai, J. D.; Brower, W. E.

    1986-11-01

    Recent studies of catalysis by amorphous metals have prompted an interest in their surface properties. We have utilized Auger electron spectroscopy, X-ray photoelectron spectroscopy and low energy alkali ion scattering to study the surface composition, electronic properties and topography of amorphous and crystallized Fe 80B 20 ribbons. The majorresults are that the surface stoichiometry is approximately that of the bulk, unaltered by segregation. Bulk crystallization results in the diffusion of impurities to the surface, but does not change the Fe/B ratio. A small shift in the B1s core level binding energy was observed on crystalline, annealed surfaces relative to amorphous or sputtered surfaces, but no shifts were observed in the iron core level energies. A weak feature due to the B2p levels was observed in the valence band spectra from sputtered surfaces. The surfaces exhibit atomic scale roughness which is not altered by bulk crystallization. Finally, there were no observable differences in the structure, composition or electronic properties between the two sides of the ribbons.

  2. Crystal structures of two thiacalix[4]arene derivatives anchoring four ...

    Indian Academy of Sciences (India)

    Administrator

    Abstract. The crystal structures of two thiacalixarene derivatives anchoring thiadiazole functional groups at lower rim, C60H72O4S12N8 (1), C64H80O4S12N8 (2), have been determined by single crystal X-ray diffraction. The thiacalix[4]arene framework in both 1 and 2 adopts the 1,3-alternate conformation. Com- pound 1 ...

  3. Crystal structure of ethyl 2,4-dichloroquinoline-3-carboxylate

    Directory of Open Access Journals (Sweden)

    Alberto Cabrera

    2015-12-01

    Full Text Available In the crystal structure of the title compound, C12H9Cl2NO2, the mean planes through the quinoline and carboxylate groups have r.m.s. deviations of 0.006 and 0.021 Å, respectively, and form a dihedral angle of 87.06 (19°. In the crystal, molecules are linked via very weak C—H...O hydrogen bonds, forming chains, which propagate along the c-axis direction.

  4. Molten salt flux synthesis and crystal structure of a new open-framework uranyl phosphate Cs{sub 3}(UO{sub 2}){sub 2}(PO{sub 4})O{sub 2}: Spectroscopic characterization and cationic mobility studies

    Energy Technology Data Exchange (ETDEWEB)

    Yagoubi, S., E-mail: said.yagoubi@cea.fr [LEEL SIS2M UMR 3299 CEA-CNRS-Université Paris-Sud 11, CEA Saclay, F-91191 Gif-Sur-Yvette (France); Renard, C.; Abraham, F. [Unité de Catalyse et de Chimie du Solide, UCCS UMR CNRS 8181, ENSCL-USTL, B.P. 90108, 59652 Villeneuve d’Ascq Cedex (France); Obbade, S. [Laboratoire d’Electrochimie et de Physicochimie des Matériaux et des Interfaces, LEPMI, UMR 5279, CNRS-Grenoble INP-UdS-UJF, 1130 Rue de la Piscine, BP75, 38402 Saint-Martin d’Hères (France)

    2013-04-15

    The reaction of triuranyl diphosphate tetrahydrate precursor (UO{sub 2}){sub 3}(PO{sub 4}){sub 2}(H{sub 2}O){sub 4} with a CsI flux at 750 °C yields a yellow single crystals of new compound Cs{sub 3}(UO{sub 2}){sub 2}(PO{sub 4})O{sub 2}. The crystal structure (monoclinic, space group C2/c, a=13.6261 (13) Å, b=8.1081(8) Å, c=12.3983(12) Å, β=114.61(12)°, V=1245.41(20) Å{sup 3} with Z=4) has been solved using direct methods and Fourier difference techniques. A full-matrix least-squares refinement on the basis of F{sup 2} yielded R1=0.028 and wR2=0.071 for 79 parameters and 1352 independent reflections with I≥2σ(I) collected on a BRUKER AXS diffractometer with MoKα radiation and a charge-coupled device detector. The crystal structure is built by two independent uranium atoms in square bipyramidal coordination, connected by two opposite corners to form infinite chains {sup 1}{sub ∞}[UO{sub 5}] and by one phosphorus atom in a tetrahedral environment PO{sub 4}. The two last entities {sup 1}{sub ∞}[UO{sub 5}] and PO{sub 4} are linked by sharing corners to form a three-dimensional structure presenting different types of channels occupied by Cs{sup +} alkaline cations. Their mobility within the tunnels were studied between 280 and 800 °C and compared with other tunneled uranyl minerals. The infrared spectrum shows a good agreement with the values inferred from the single crystal structure analysis of uranyl phosphate compound. - Graphical abstract: Arrhenius plot of the electrical conductivity of tunneled compounds Cs{sub 3}U{sub 2}PO{sub 10} and CsU{sub 2}Nb{sub 2}O{sub 11.5}. Highlights: ► The reaction of (UO{sub 2}){sub 3}(PO{sub 4}){sub 2}(H{sub 2}O){sub 4} in excess of molten CsI leads to single-crystals of new tunneled compound Cs{sub 3}(UO{sub 2}){sub 2}(PO{sub 4})O{sub 2}. ► Ionic conductivity measurements and crystal structure analysis indicate a strong connection of the Cs{sup +} cations to the tunnels. ► A low symmetry in Cs{sub 3}(UO{sub 2

  5. Preliminary characterization of (nucleoside-2′-O-)-methyltransferase crystals from Meaban and Yokose flaviviruses

    International Nuclear Information System (INIS)

    Mastrangelo, Eloise; Bollati, Michela; Milani, Mario; Lamballeire, Xavier de; Brisbare, Nadege; Dalle, Karen; Lantez, Violaine; Egloff, Marie-Pierre; Coutard, Bruno; Canard, Bruno; Gould, Ernest; Forrester, Naomi; Bolognesi, Martino

    2006-01-01

    Two methyltransferases from flaviviruses (Meaban and Yokose viruses) have been overexpressed and crystallized. Diffraction data and characterization of the two crystal forms are presented, together with a preliminary molecular-replacement solution for both enzymes. Viral methyltranferases (MTase) are involved in the third step of the mRNA-capping process, transferring a methyl group from S-adenosyl-l-methionine (SAM) to the capped mRNA. MTases are classified into two groups: (guanine-N7)-methyltransferases (N7MTases), which add a methyl group onto the N7 atom of guanine, and (nucleoside-2′-O-)-methyltransferases (2′OMTases), which add a methyl group to a ribose hydroxyl. The MTases of two flaviviruses, Meaban and Yokose viruses, have been overexpressed, purified and crystallized in complex with SAM. Characterization of the crystals together with details of preliminary X-ray diffraction data collection (at 2.8 and 2.7 Å resolution, respectively) are reported here. The sequence homology relative to Dengue virus 2′OMTase and the structural conservation of specific residues in the putative active sites suggest that both enzymes belong to the 2′OMTase subgroup

  6. Preliminary characterization of (nucleoside-2′-O-)-methyltransferase crystals from Meaban and Yokose flaviviruses

    Energy Technology Data Exchange (ETDEWEB)

    Mastrangelo, Eloise; Bollati, Michela; Milani, Mario [Department of Biomolecular Sciences and Biotechnology, CNR-INFM, University of Milano, Via Celoria 26, 20133 Milano (Italy); Lamballeire, Xavier de; Brisbare, Nadege [Unité des Virus Emergents, Faculté de Médecine, 27 Boulevard Jean Moulin, 13005 Marseille (France); Dalle, Karen; Lantez, Violaine; Egloff, Marie-Pierre; Coutard, Bruno; Canard, Bruno [Laboratoire Architecture et Fonction des Macromolécules Biologiques, UMR 6098 CNRS ESIL, Case 932, 163 Avenue de Luminy, 13288 Marseille CEDEX 9 (France); Gould, Ernest; Forrester, Naomi [CEH Oxford, Mansfield Road, Oxford OX1 3SR (United Kingdom); Bolognesi, Martino, E-mail: martino.bolognesi@unimi.it [Department of Biomolecular Sciences and Biotechnology, CNR-INFM, University of Milano, Via Celoria 26, 20133 Milano (Italy)

    2006-08-01

    Two methyltransferases from flaviviruses (Meaban and Yokose viruses) have been overexpressed and crystallized. Diffraction data and characterization of the two crystal forms are presented, together with a preliminary molecular-replacement solution for both enzymes. Viral methyltranferases (MTase) are involved in the third step of the mRNA-capping process, transferring a methyl group from S-adenosyl-l-methionine (SAM) to the capped mRNA. MTases are classified into two groups: (guanine-N7)-methyltransferases (N7MTases), which add a methyl group onto the N7 atom of guanine, and (nucleoside-2′-O-)-methyltransferases (2′OMTases), which add a methyl group to a ribose hydroxyl. The MTases of two flaviviruses, Meaban and Yokose viruses, have been overexpressed, purified and crystallized in complex with SAM. Characterization of the crystals together with details of preliminary X-ray diffraction data collection (at 2.8 and 2.7 Å resolution, respectively) are reported here. The sequence homology relative to Dengue virus 2′OMTase and the structural conservation of specific residues in the putative active sites suggest that both enzymes belong to the 2′OMTase subgroup.

  7. Isolation, crystallization and crystal structure determination of bovine kidney Na(+),K(+)-ATPase.

    Science.gov (United States)

    Gregersen, Jonas Lindholt; Mattle, Daniel; Fedosova, Natalya U; Nissen, Poul; Reinhard, Linda

    2016-04-01

    Na(+),K(+)-ATPase is responsible for the transport of Na(+) and K(+) across the plasma membrane in animal cells, thereby sustaining vital electrochemical gradients that energize channels and secondary transporters. The crystal structure of Na(+),K(+)-ATPase has previously been elucidated using the enzyme from native sources such as porcine kidney and shark rectal gland. Here, the isolation, crystallization and first structure determination of bovine kidney Na(+),K(+)-ATPase in a high-affinity E2-BeF3(-)-ouabain complex with bound magnesium are described. Crystals belonging to the orthorhombic space group C2221 with one molecule in the asymmetric unit exhibited anisotropic diffraction to a resolution of 3.7 Å with full completeness to a resolution of 4.2 Å. The structure was determined by molecular replacement, revealing unbiased electron-density features for bound BeF3(-), ouabain and Mg(2+) ions.

  8. Band structures and localization properties of aperiodic layered phononic crystals

    Energy Technology Data Exchange (ETDEWEB)

    Yan Zhizhong, E-mail: zzyan@bit.edu.cn [Department of Applied Mathematics, Beijing Institute of Technology, Beijing 100081 (China); Zhang Chuanzeng [Department of Civil Engineering, University of Siegen, D-57078 Siegen (Germany)

    2012-03-15

    The band structures and localization properties of in-plane elastic waves with coupling of longitudinal and transverse modes oblique propagating in aperiodic phononic crystals based on Thue-Morse and Rudin-Shapiro sequences are studied. Using transfer matrix method, the concept of the localization factor is introduced and the correctness is testified through the Rytov dispersion relation. For comparison, the perfect periodic structure and the quasi-periodic Fibonacci system are also considered. In addition, the influences of the random disorder, local resonance, translational and/or mirror symmetries on the band structures of the aperiodic phononic crystals are analyzed in this paper.

  9. Crystal structure and thermal property of polyethylene glycol octadecyl ether

    International Nuclear Information System (INIS)

    Meng, Jie-yun; Tang, Xiao-fen; Li, Wei; Shi, Hai-feng; Zhang, Xing-xiang

    2013-01-01

    Highlights: ► The crystal structure of C18En for n ≥ 20 is a monoclinic system. ► Polyethylene glycol octadecyl ether crystallizes perfectly. ► The number of repeat units has significant effect on the melting, crystallizing temperature and enthalpy. ► The thermal stable temperature increases rapidly with increasing the number of repeat unit. - Abstract: The crystal structure, phase change property and thermal stable temperature (T d ) of polyethylene glycol octadecyl ether [HO(CH 2 CH 2 O) n C 18 H 37 , C18En] with various numbers of repeat units (n = 2, 10, 20 and 100) as phase change materials (PCMs) were investigated using temperature variable Fourier transformed infrared spectroscopy (FTIR), wide-angle X-ray diffraction (XRD), differential scanning calorimetry (DSC), and thermogravimetric analysis (TG). C18En crystallizes perfectly at 0 °C; and the crystal structure for n ≥ 20 is a monoclinic system. The number of repeat units has great effect on the phase change properties of C18En. The thermal stable temperature increases rapidly with increasing the number of repeat units. They approach to that of PEG-2000 as the number of repeat units is more than 10. T d increases rapidly with increasing the number of repeat units. C18En are a series of promising polymeric PCMs

  10. CsPb2Br5 Single Crystals: Synthesis and Characterization

    KAUST Repository

    Dursun, Ibrahim

    2017-08-02

    CsPb2Br5 is a ternary halogen-plumbate material with close characteristics to well-reported halide perovskites. Due to its unconventional two-dimensional structure, CsPb2Br5 is being looked at broadly for potential applications in optoelectronics. CsPb2Br5 investigations are currently limited to nanostructures and powder forms of the material, which present unclear and conflicting optical properties. In this study, we present the synthesis and characterization of CsPb2Br5 bulk single crystals, which enabled us to finally clarify the material\\'s optical features. Our CsPb2Br5 crystal has a two-dimensional structure with Pb2Br5- layers spaced by Cs+ cations, and exhibits a ~3.1 eV indirect bandgap with no emission in the visible spectrum.

  11. Crystallization and preliminary characterization of three different crystal forms of human saposin C heterologously expressed in Pichia pastoris

    International Nuclear Information System (INIS)

    Schultz-Heienbrok, Robert; Remmel, Natascha; Klingenstein, R.; Rossocha, Maksim; Sandhoff, Konrad; Saenger, Wolfram; Maier, Timm

    2006-01-01

    Three different crystal forms were obtained of human saposin C. The structures could not be determined by molecular replacement using known solution structures of the protein as search models, supporting the notion of a highly flexible protein. The amphiphilic saposin proteins (A, B, C and D) act at the lipid–water interface in lysosomes, mediating the hydrolysis of membrane building blocks by water-soluble exohydrolases. Human saposin C activates glucocerebrosidase and β-galactosylceramidase. The protein has been expressed in Pichia pastoris, purified and crystallized in three different crystal forms, diffracting to a maximum resolution of 2.5 Å. Hexagonal crystals grew from 2-propanol-containing solution and contain a single molecule in the asymmetric unit according to the Matthews coefficient. Orthorhombic and tetragonal crystals were both obtained with pentaerythritol ethoxylate and are predicted to contain two molecules in the asymmetric unit. Attempts to determine the respective crystal structures by molecular replacement using either the known NMR structure of human saposin C or a related crystal structure as search models have so far failed. The failure of the molecular-replacement method is attributed to conformational changes of the protein, which are known to be required for its biological activity. Crystal structures of human saposin C therefore might be the key to mapping out the conformational trajectory of saposin-like proteins

  12. Solving RNA's structural secrets: interaction with antibodies and crystal structure of a nuclease resistant RNA

    International Nuclear Information System (INIS)

    Wallace, S.T.

    1998-10-01

    This Ph.D. thesis concerns the structural characterization of RNA. The work is split into two sections: 1) in vitro selection and characterization of RNAs which bind antibiotics and 2) crystal structure of a nuclease resistant RNA molecule used in antisense applications. Understanding antibiotic-RNA interactions is crucial in aiding rational drug design. We were interested in studying antibiotic interactions with RNAs small enough to characterize at the molecular and possibly at the atomic level. In order to do so, we previously performed in vitro selection to find small RNAs which bind to the peptide antibiotic viomycin and the aminoglycoside antibiotic streptomycin. The characterization of the viomycin-binding RNAs revealed the necessity of a pseudoknot-structure in order to interact with the antibiotic. The RNAs which were selected to interact with streptomycin require the presence of magnesium to bind the antibiotic. One of the RNAs, upon interacting with streptomycin undergoes a significant conformational change spanning the entire RNA sequence needed to bind the antibiotic. In a quest to design oligodeoxynucleotides (ODNs) which are able to specifically bid and inactivate the mRNA of a gene, it is necessary to fulfill two criteria: 1) increase binding affinity between the ODN and the target RNA and 2) increase the ODN's resistance to nuclease degradation. An ODN with an aminopropyl modification at the 2' position of its ribose has emerged as the most successful candidate at fulfilling both criteria. It is the most nuclease resistant modification known to date. We were interested in explaining how this modification is able to circumvent degradation by nucleases. A dodecamer containing a single 2'-O-aminopropyl modified nucleotide was crystallized and the structure was solved to a resolution of 1.6 A. In an attempt to explain the nuclease resistance, the crystal coordinates were modeled into the active exonuclease site of DNA polymerase I. We propose the

  13. Twinned crystals of adeno-associated virus serotype 3b prove suitable for structural studies

    International Nuclear Information System (INIS)

    Lerch, Thomas F.; Xie, Qing; Ongley, Heather M.; Hare, Joan; Chapman, Michael S.

    2009-01-01

    Crystals of adeno-associated virus serotype 3b, a human DNA virus with promise as a vector for gene therapy, have been grown, diffract X-rays to ∼2.6 Å resolution and are suitable for structure determination in spite of twinning. Adeno-associated viruses (AAVs) are leading candidate vectors for gene-therapy applications. The AAV-3b capsid is closely related to the well characterized AAV-2 capsid (87% identity), but sequence and presumably structural differences lead to distinct cell-entry and immune-recognition properties. In an effort to understand these differences and to perhaps harness them, diffraction-quality crystals of purified infectious AAV-3b particles have been grown and several partial diffraction data sets have been recorded. The crystals displayed varying levels of merohedral twinning that in earlier times would have rendered them unsuitable for structure determination, but here is shown to be a tractable complication

  14. Crystal structure of 4-methylsulfanyl-2-phenylquinazoline

    Directory of Open Access Journals (Sweden)

    Mohammed B. Alshammari

    2014-08-01

    Full Text Available In the title compound, C15H12N2S, the methylthioquinazoline group is planar with the methyl C displaced by only 0.116 (3 Å from the plane of the quinazoline moiety. The dihedral angle between the phenyl ring and the quinazoline ring system is 13.95 (5°. In the crystal, each molecule is linked by π–π stacking between to two adjacent inversion-related molecules. On one side, the inverted quinazoline groups interact with a centroid–centroid distance of 3.7105 (9 Å. On the other side, the quinazoline group interacts with the pyrimidine and phenyl rings of the second neighbour with centroid–centroid distances of 3.5287 (8 and 3.8601 (9 Å, respectively.

  15. Crystal structure of rubidium peroxide ammonia disolvate

    Directory of Open Access Journals (Sweden)

    Tobias Grassl

    2017-02-01

    Full Text Available The title compound, Rb2O2·2NH3, has been obtained as a reaction product of rubidium metal dissolved in liquid ammonia and glucuronic acid. As a result of the low-temperature crystallization, a disolvate was formed. To our knowledge, only one other solvate of an alkali metal peroxide is known: Na2O2·8H2O has been reported by Grehl et al. [Acta Cryst. (1995, C51, 1038–1040]. We determined the peroxide bond length to be 1.530 (11 Å, which is in accordance with the length reported by Bremm & Jansen [Z. Anorg. Allg. Chem. (1992, 610, 64–66]. One of the ammonia solvate molecules is disordered relative to a mirror plane, with 0.5 occupancy for the corresponding nitrogen atom.

  16. Acid indium strontium phosphate SrIn2[PO3(OH)]4: synthesis and crystal structure

    International Nuclear Information System (INIS)

    Rusakov, D.A.; Bobylev, A.P.; Komissarova, L.N.; Filaretov, A.A.; Danilov, V.P.

    2007-01-01

    Acid indium-strontium phosphate SrIn 2 [PO 3 (OH)] 4 is synthesized and characterized. Crystal structure and lattice parameters ate determined. In atoms in SrIn 2 [PO 3 (OH)] 4 structure are in distorted InO 6 octahedrons and form with PO 3 (OH) tetrahedrons mixed paraskeleton {In 2 [PO 3 (OH)] 4 } 3∞ 2- with emptinesses occupied by big Sr 2+ cations. The compound is thermally stable up to 400 Deg C [ru

  17. Crystal structure of (E)-3-fluoro-N-((5-nitrothiophen-2-yl)methylene)aniline

    Energy Technology Data Exchange (ETDEWEB)

    Karataş, Şadiye; Tanak, Hasan, E-mail: hasantanak@gmail.com [Amasya University, Department of Physics, Faculty of Arts and Sciences (Turkey); Ağar, Ayşen Alaman [Ondokuz Mayıs University, Department of Chemistry, Faculty of Arts and Sciences (Turkey)

    2016-05-15

    The structure of the title compound C{sub 11}H{sub 7}FN{sub 2}O{sub 2}S was characterized by single crystal X-ray diffraction. The compound crystallizes in the monoclinic space group P2{sub 1}/n with Z = 12, i.e. with three molecules in asymmetric unit. The molecules are not planar: the dihedral angles between the planes of thiophene and the benzene rings are 42.3(3)°, 42.0(3)°, and 48.9(2)°. In the crystal, intermolecular C–H···F interactions link the molecules through R{sub 2}{sup 2} (14) ring motif. The crystal packing is also stabilized by π···π interactions.

  18. Crystals structure of Na3Li(TiF6)2

    International Nuclear Information System (INIS)

    Popov, D.Yu.; Antokhina, T.F.; Gerasimenko, A.V.; Kajdalova, T.A.; Sergienko, V.I.

    2004-01-01

    Crystals of Na 3 Li(TiF 6 ) 2 (1) were synthesized in aqueous solution and characterized by the elementary and X-ray phase analysis methods. According to X-ray diffraction analysis data compound 1 is crystallized in a tetragonal crystal system with the following parameters: a=5.130(1), c=18.046(4) A, Z=2, space group P4-bar2 1 c. Alternating layers on the basis of dimers made up by octahedrons of TiF 6 and Na(1)F 6 constitute the frame of compound 1 crystal structure. The dimer layers are joined in a continuous frame by Na(2) and Li cations. Coordination polyhedron of Li atom is tetrahedron (Li-F 1.898(3) A) [ru

  19. Studies on the structural, optical and dielectric properties of samarium coordinated with salicylic acid single crystal

    Science.gov (United States)

    Singh, Harjinder; Slathia, Goldy; Gupta, Rashmi; Bamzai, K. K.

    2018-04-01

    Samarium coordinated with salicylic acid was successfully grown as a single crystal by low temperature solution technique using mixed solvent of methanol and water in equal ratio. Structural characterization was carried out by single crystal X-ray diffraction analysis and it crystallizes in centrosymmetric space group P121/c1. FTIR and UV-Vis-NIR spectroscopy confirmed the compound formation and help to determine the mode of binding of the ligand to the rare earth-metal ion. Dielectric constant and dielectric loss have been measured over the frequency range 100 Hz - 30MHz. The decrease in dielectric constant with increases in frequency is due to the transition from interfacial polarization to dipolar polarization. The small value of dielectric constant at higher frequency ensures that the crystal is good candidate for NLO devices. Dielectric loss represents the resistive nature of the material.

  20. Solid-melt interface structure and growth of Cu alloy single crystals

    International Nuclear Information System (INIS)

    Tomimitsu, Hiroshi; Kamada, Kohji.

    1983-01-01

    Crystal-melt interface behavior during the growth of Cu-base solid solutions by the Bridgman method is discussed on the basis of experimental evidence obtained by neutron diffraction topography. Advantages of neutron diffraction topography for the characterization of large single crystals, such as dealt with in this paper, are emphasized. Evidence was odserved of extremely regular crystal growth along directions, irrespective of the macroscopic growth direction. This contrasts with the previously believed (110) normal growth which is a conclusion of growth theory based on molecular kinetics at the solid-melt interface. In consequence, we believe that the kinetics at the interface is a minor factor in the meltgrowth of metal single crystals. Revised melt-growth theory should include both the growth and the formation of the regular structure as evidenced by neutron diffraction topography. (author)

  1. Hydrothermal synthesis, structure and characterization of new ...

    Indian Academy of Sciences (India)

    Unknown

    Keywords. Hydrothermal; crystal structure; solid electrolyte; iron (III) pyrophosphate. 1. Introduction ... tion, structure and electrical conductivity and the higher values of ..... type cavity structure. Acknowledgements. The authors would like to express their thanks to DST,. New Delhi, for financial assistance under the projects.

  2. Synthesis, characterization, X-ray crystal structure and conductometry studying of a number of new Schiff base complexes; a new example of binuclear square pyramidal geometry of Cu(II) complex bridged with an oxo group

    Science.gov (United States)

    Golbedaghi, Reza; Alavipour, Ehsan

    2015-11-01

    Three new binuclear Cu(II), Mn(II), Co(II) complexes [Cu2(L) (ClO4)](ClO4)2 (1), [Mn2(L) (ClO4)](ClO4)2 (2), and [Co2(L) (ClO4)](ClO4)2 (3), {L = 1,3-bis(2-((Z)-(2-aminopropylimino)methyl)phenoxy)propan-2-ol} have been synthesized. Single crystal X-ray structure analysis of complex 1 showed that the complex is binuclear and all nitrogen and oxygen atoms of ligand (N4O3) are coordinated to two Cu(II) center ions. In addition, the crystal structure studying shows, a perchlorate ion has been bridged to the Cu(II) metal centers. However, two distorted square pyramidal Cu(II) ions are bridged asymmetrically by a perchlorate ion and oxygen of hydroxyl group of Schiff base ligand. In addition, the conductometry behaviors of all complexes were studied in acetonitrile solution.

  3. Synthesis and structural characterization of actinide oxalate compounds

    International Nuclear Information System (INIS)

    Tamain, C.

    2011-01-01

    Oxalic acid is a well-known reagent to recover actinides thanks to the very low solubility of An(IV) and An(III) oxalate compounds in acidic solution. Therefore, considering mixed-oxide fuel or considering minor actinides incorporation in ceramic fuel materials for transmutation, oxalic co-conversion is convenient to synthesize mixed oxalate compounds, precursors of oxide solid solutions. As the existing oxalate single crystal syntheses are not adaptable to the actinide-oxalate chemistry or to their manipulation constrains in gloves box, several original crystal growth methods were developed. They were first validate and optimized on lanthanides and uranium before the application to transuranium elements. The advanced investigations allow to better understand the syntheses and to define optimized chemical conditions to promote crystal growth. These new crystal growth methods were then applied to a large number of mixed An1(IV)-An2(III) or An1(IV)-An2(IV) systems and lead to the formation of the first original mixed An1(IV)-An2(III) and An1(IV)-An2(IV) oxalate single crystals. Finally thanks to the first thorough structural characterizations of these compounds, single crystal X-ray diffraction, EXAFS or micro-RAMAN, the particularly weak oxalate-actinide compounds structural database is enriched, which is essential for future studied nuclear fuel cycles. (author) [fr

  4. Crystal structure of TiNi nanoparticles obtained by Ar ion beam deposition

    International Nuclear Information System (INIS)

    Castro, A. Torres; Cuellar, E. Lopez; Mendez, U. Ortiz; Yacaman, M. Jose

    2008-01-01

    Nanoparticles are a state of matter that have properties different from either molecules or bulk solids, turning them into a very interesting class of materials to study. In the present work, the crystal structure of TiNi nanoparticles obtained by ion beam deposition is characterized. TiNi nanoparticles were obtained from TiNi wire samples by sputtering with Ar ions using a Gatan precision ion polishing system. The TiNi nanoparticles were deposited on a Lacey carbon film that was used for characterization by transmission electron microscopy. The nanoparticles were characterized by high-resolution transmission electron microscopy, high-angle annular dark-field imaging, electron diffraction, scanning transmission electron microscopy and energy-dispersive X-ray spectroscopy. Results of nanodiffraction seem to indicate that the nanoparticles keep the same B2 crystal structure as the bulk material but with a decreased lattice parameter

  5. SPAD array chips with full frame readout for crystal characterization

    Energy Technology Data Exchange (ETDEWEB)

    Fischer, Peter; Blanco, Roberto; Sacco, Ilaria; Ritzert, Michael [Heidelberg University (Germany); Weyers, Sascha [Fraunhofer Institute for Microelectronic Circuits and Systems (Germany)

    2015-05-18

    We present single photon sensitive 2D camera chips containing 88x88 avalanche photo diodes which can be read out in full frame mode with up to 400.000 frames per second. The sensors have an imaging area of ~5mm x 5mm covered by square pixels of ~56µm x 56µm with a ~55% fill factor in the latest chip generation. The chips contain a self triggering logic with selectable (column) multiplicities of up to >=4 hits within an adjustable coincidence time window. The photon accumulation time window is programmable as well. First prototypes have demonstrated low dark count rates of <50kHz/mm2 (SPAD area) at 10 degree C for 10% masked pixels. One chip version contains an automated readout of the photon cluster position. The readout of the detailed photon distribution for single events allows the characterization of light sharing, optical crosstalk etc., in crystals or crystal arrays as they are used in PET instrumentation. This knowledge could lead to improvements in spatial or temporal resolution.

  6. The crystal structure of urea nitrate

    NARCIS (Netherlands)

    Harkema, Sybolt; Feil, D.

    1969-01-01

    The structure of urea nitrate has been solved, by the use of three-dimensional X-ray data. Data were collected using Cu Ke and Mo K0~ radiations. The structure consists of layers with urea and nitrate groups held together by hydrogen bonds. The positions of all hydrogen atoms were found. The final R

  7. A crystal structure prediction enigma solved

    DEFF Research Database (Denmark)

    Hoser, Anna Agnieszka; Sovago, Ioana; Lanzac, A.

    2017-01-01

    The seemingly unpredictable structure of gallic acid monohydrate form IV has been investigated using accurate X-ray diffraction measurements at temperatures of 10 and 123 K. The measurements demonstrate that the structure is commensurately modulated at 10 K and disordered at higher temperatures...

  8. Solving Crystal Structures from Powder Diffraction Data

    DEFF Research Database (Denmark)

    Christensen, A. Nørlund; Lehmann, M. S.; Nielsen, Mogens

    1985-01-01

    High resolution powder data from both neutron and X-ray (synchrotron) sources have been used to estimate the possibility of direct structure determination from powder data. Two known structures were resolved by direct methods with neutron and X-ray data. With synchrotron X-ray data, the measured ...

  9. High-Q microwave resonators with a photonic crystal structure

    International Nuclear Information System (INIS)

    Schuster, M.

    2001-08-01

    The localisation of electromagnetic energy at a defect in a photonic crystal is similar to a well known effect employed to construct high-Q microwave resonators: In a whispering gallery (WHG-) mode resonator the high Q-factor is achieved by localisation of the electromagnetic field energy by total reflection inside a disk made of dielectric material. The topic of this work is to demonstrate, that WHG-like modes can exist in an air defect in a photonic crystal that extends over several lattice periods; and that a high-Q microwave resonator can be made, utilizing these resonant modes. In numerical simulations, the transmission properties of a photonic crystal structure with hexagonal lattice symmetry have been investigated with a transfer-matrix-method. The eigenmodes of a defect structure in a photonic crystal have been calculated with a quasi-3d finite element integration technique. Experimental results confirm the simulated transmission properties and show the existence of modes inside the band gap, when a defect is introduced in the crystal. Resonator measurements show that a microwave resonator can be operated with those defect modes. It was found out that the main losses of the resonator were caused by bad microwave properties of the used dielectric material and by metal losses on the top and bottom resonator walls. Furthermore, it turned out that the detection of the photonic crystal defect mode was difficult because of a lack of simulation possibilities and high housing mode density in the resonator. (orig.)

  10. Introduction to optical methods for characterizing liquid crystals at interfaces.

    Science.gov (United States)

    Miller, Daniel S; Carlton, Rebecca J; Mushenheim, Peter C; Abbott, Nicholas L

    2013-03-12

    This Instructional Review describes methods and underlying principles that can be used to characterize both the orientations assumed spontaneously by liquid crystals (LCs) at interfaces and the strength with which the LCs are held in those orientations (so-called anchoring energies). The application of these methods to several different classes of LC interfaces is described, including solid and aqueous interfaces as well as planar and nonplanar interfaces (such as those that define a LC-in-water emulsion droplet). These methods, which enable fundamental studies of the ordering of LCs at polymeric, chemically functionalized, and biomolecular interfaces, are described in this Instructional Review on a level that can be easily understood by a nonexpert reader such as an undergraduate or graduate student. We focus on optical methods because they are based on instrumentation that is found widely in research and teaching laboratories.

  11. The characterization of tungsten disulfide single crystals doped with gold

    International Nuclear Information System (INIS)

    Dumcenco, D.O.; Huang, Y.S.; Tiong, K.K.; Liang, C.H.; Chen, C.H.

    2007-01-01

    Single crystals of WS 2 doped with gold (WS 2 :Au) have been grown by the chemical vapour transport method using iodine as a transporting agent. Hall measurements indicate that the samples are p-type in nature. The doping effect of the materials are characterized by conductivity, surface photovoltage and piezo reflectance measurements. The higher conductivity respect to that of the undoped one suggests that more charge carriers are available for conduction in the doped compound. The surface photovoltage spectrum reveals an impurity level located below the A exciton. The direct band-edge excitonic transition energies for WS 2 :Au show redshifts and the broadening parameters of the excitonic transition features increase due to impurity scattering. (authors)

  12. Thermal-induced conformational changes in the product release area drive the enzymatic activity of xylanases 10B: Crystal structure, conformational stability and functional characterization of the xylanase 10B from Thermotoga petrophila RKU-1

    International Nuclear Information System (INIS)

    Santos, Camila Ramos; Meza, Andreia Navarro; Hoffmam, Zaira Bruna; Silva, Junio Cota; Alvarez, Thabata Maria; Ruller, Roberto; Giesel, Guilherme Menegon; Verli, Hugo; Squina, Fabio Marcio; Prade, Rolf Alexander; Murakami, Mario Tyago

    2010-01-01

    Research highlights: → The hyperthermostable xylanase 10B from Thermotoga petrophila RKU-1 produces exclusively xylobiose at the optimum temperature. → Circular dichroism spectroscopy suggests a coupling effect of temperature-induced structural changes with its enzymatic behavior. → Crystallographic and molecular dynamics studies indicate that conformational changes in the product release area modulate the enzyme action mode. -- Abstract: Endo-xylanases play a key role in the depolymerization of xylan and recently, they have attracted much attention owing to their potential applications on biofuels and paper industries. In this work, we have investigated the molecular basis for the action mode of xylanases 10B at high temperatures using biochemical, biophysical and crystallographic methods. The crystal structure of xylanase 10B from hyperthermophilic bacterium Thermotoga petrophila RKU-1 (TpXyl10B) has been solved in the native state and in complex with xylobiose. The complex crystal structure showed a classical binding mode shared among other xylanases, which encompasses the -1 and -2 subsites. Interestingly, TpXyl10B displayed a temperature-dependent action mode producing xylobiose and xylotriose at 20 o C, and exclusively xylobiose at 90 o C as assessed by capillary zone electrophoresis. Moreover, circular dichroism spectroscopy suggested a coupling effect of temperature-induced structural changes with this particular enzymatic behavior. Molecular dynamics simulations supported the CD analysis suggesting that an open conformational state adopted by the catalytic loop (Trp297-Lys326) provokes significant modifications in the product release area (+1,+2 and +3 subsites), which drives the enzymatic activity to the specific release of xylobiose at high temperatures.

  13. Thermal-induced conformational changes in the product release area drive the enzymatic activity of xylanases 10B: Crystal structure, conformational stability and functional characterization of the xylanase 10B from Thermotoga petrophila RKU-1

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Camila Ramos; Meza, Andreia Navarro [Laboratorio Nacional de Biociencias (LNBio), Centro Nacional de Pesquisa em Energia e Materiais, Campinas, SP (Brazil); Hoffmam, Zaira Bruna; Silva, Junio Cota; Alvarez, Thabata Maria; Ruller, Roberto [Laboratorio Nacional de Ciencia e Tecnologia do Bioetanol (CTBE), Centro Nacional de Pesquisa em Energia e Materiais, Campinas, SP (Brazil); Giesel, Guilherme Menegon; Verli, Hugo [Centro de Biotecnologia, Universidade Federal do Rio Grande do Sul, Porto Alegre, RS (Brazil); Squina, Fabio Marcio [Laboratorio Nacional de Ciencia e Tecnologia do Bioetanol (CTBE), Centro Nacional de Pesquisa em Energia e Materiais, Campinas, SP (Brazil); Prade, Rolf Alexander [Department of Microbiology and Molecular Genetics, Oklahoma State University, Stillwater, OK (United States); Murakami, Mario Tyago, E-mail: mario.murakami@lnbio.org.br [Laboratorio Nacional de Biociencias (LNBio), Centro Nacional de Pesquisa em Energia e Materiais, Campinas, SP (Brazil)

    2010-12-10

    Research highlights: {yields} The hyperthermostable xylanase 10B from Thermotoga petrophila RKU-1 produces exclusively xylobiose at the optimum temperature. {yields} Circular dichroism spectroscopy suggests a coupling effect of temperature-induced structural changes with its enzymatic behavior. {yields} Crystallographic and molecular dynamics studies indicate that conformational changes in the product release area modulate the enzyme action mode. -- Abstract: Endo-xylanases play a key role in the depolymerization of xylan and recently, they have attracted much attention owing to their potential applications on biofuels and paper industries. In this work, we have investigated the molecular basis for the action mode of xylanases 10B at high temperatures using biochemical, biophysical and crystallographic methods. The crystal structure of xylanase 10B from hyperthermophilic bacterium Thermotoga petrophila RKU-1 (TpXyl10B) has been solved in the native state and in complex with xylobiose. The complex crystal structure showed a classical binding mode shared among other xylanases, which encompasses the -1 and -2 subsites. Interestingly, TpXyl10B displayed a temperature-dependent action mode producing xylobiose and xylotriose at 20 {sup o}C, and exclusively xylobiose at 90 {sup o}C as assessed by capillary zone electrophoresis. Moreover, circular dichroism spectroscopy suggested a coupling effect of temperature-induced structural changes with this particular enzymatic behavior. Molecular dynamics simulations supported the CD analysis suggesting that an open conformational state adopted by the catalytic loop (Trp297-Lys326) provokes significant modifications in the product release area (+1,+2 and +3 subsites), which drives the enzymatic activity to the specific release of xylobiose at high temperatures.

  14. Copper coordination polymers constructed from thiazole-5-carboxylic acid: Synthesis, crystal structures, and structural transformation

    Energy Technology Data Exchange (ETDEWEB)

    Meundaeng, Natthaya; Rujiwatra, Apinpus [Department of Chemistry, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand); Prior, Timothy J., E-mail: t.prior@hull.ac.uk [Chemistry, University of Hull, Kingston upon Hull HU6 7RX (United Kingdom)

    2017-01-15

    We have successfully prepared crystals of thiazole-5-carboxylic acid (5-Htza) (L) and three new thiazole-5-carboxylate-based Cu{sup 2+} coordination polymers with different dimensionality, namely, 1D [Cu{sub 2}(5-tza){sub 2}(1,10-phenanthroline){sub 2}(NO{sub 3}){sub 2}] (1), 2D [Cu(5-tza){sub 2}(MeOH){sub 2}] (2), and 3D [Cu(5-tza){sub 2}]·H{sub 2}O (3). These have been characterized by single crystal X-ray diffraction and thermogravimetry. Interestingly, the 2D network structure of 2 can directly transform into the 3D framework of 3 upon removal of methanol molecules at room temperature. 2 can also undergo structural transformation to produce the same 2D network present in the known [Cu(5-tza){sub 2}]·1.5H{sub 2}O upon heat treatment for 2 h. This 2D network can adsorb water and convert to 3 upon exposure to air. - Highlights: • Rare examples of coordination polymers of thiazole-5-carboxylic acid were prepared. • Non-covalent interactions play a key role on the assembly of the complexes in solid state. • Structural transformation of a 2D framework to a 3D upon removal of methanol is observed.

  15. Crystal-Size-Dependent Structural Transitions in Nanoporous Crystals: Adsorption-Induced Transitions in ZIF-8

    KAUST Repository

    Zhang, Chen

    2014-09-04

    © 2014 American Chemical Society. Understanding the crystal-size dependence of both guest adsorption and structural transitions of nanoporous solids is crucial to the development of these materials. We find that nano-sized metal-organic framework (MOF) crystals have significantly different guest adsorption properties compared to the bulk material. A new methodology is developed to simulate the adsorption and transition behavior of entire MOF nanoparticles. Our simulations predict that the transition pressure significantly increases with decreasing particle size, in agreement with crystal-size-dependent experimental measurements of the N2-ZIF-8 system. We also propose a simple core-shell model to examine this effect on length scales that are inaccessible to simulations and again find good agreement with experiments. This study is the first to examine particle size effects on structural transitions in ZIFs and provides a thermodynamic framework for understanding the underlying mechanism.

  16. Studies on the growth and characterization of tris (glycine) calcium({Iota}{Iota}) dichloride-a nonlinear optical crystal

    Energy Technology Data Exchange (ETDEWEB)

    Dhanaraj, P.V. [Centre for Crystal Growth, SSN College of Engineering, Kalavakkam 603 110 (India); Rajesh, N.P., E-mail: rajeshnp@ssn.edu.i [Centre for Crystal Growth, SSN College of Engineering, Kalavakkam 603 110 (India)

    2011-01-01

    A systematic characterization of a novel nonlinear optical material tris (glycine) calcium({Iota}{Iota}) dichloride (TGCC) is performed. The solubility and metastable zone width of TGCC were studied. TGCC single crystal of dimensions 34x23x5 mm{sup 3} was grown by the slow evaporation technique. Single crystal X-ray diffraction studies reveal that the crystal belongs to orthorhombic system. Energy dispersive X-ray analysis confirms the presence of elements in the crystal. Structural perfection of the as-grown single crystal was studied through multicrystal X-ray diffraction analysis. The thermal characteristics of TGCC were analyzed by thermogravimetric and differential thermal analysis and differential scanning calorimetry. The transmittance of TGCC crystal has been used to calculate the optical band gap of the crystal. Chemical etching studies of TGCC crystal was carried out. The dielectric and mechanical behavior of the crystals were analyzed. The second harmonic conversion property of TGCC was identified by the Kurtz and Perry powder technique and was observed to be higher than that of KDP.

  17. Crystal structure of aspartame anhydrate from powder diffraction data. Structural aspects of the dehydration process of aspartame

    NARCIS (Netherlands)

    Guguta, C.; Meekes, H.L.M.; Gelder, R. de

    2006-01-01

    Aspartame has three pseudo-polymorphic forms, two hydrates and a hemi-hydrate, for which crystal structures were determined from single-crystal diffraction data. This paper presents the crystal structure of the anhydrate, which was obtained by dehydrating the hemi-hydrate. The crystal structure of

  18. On structure of some laminated crystals with organic molecules

    International Nuclear Information System (INIS)

    Volodina, G.F.; Ivanova, V.Ya.; Malinovskij, T.I.

    1982-01-01

    A survey is made of papers dealing with intercalation of organic molecules into crystals of dihalcogenides of some transition metals (TaS 2 , TiS 2 , NbS 2 , ZrS 2 , TaSe 2 ), variation of their structure and physical properties. Among the used intercalates ammonia, pyridine, aniline and other aromatic amines proved to be most satisfactory from the viewpoint of reaction rate and product stability. A possibility is discussed of intercalation into PbI 2 and CdI 2 crystals that are of the same structural type as dihalcogenides

  19. Single crystal growth and characterization of kagomé-lattice shandites Co3Sn2-xInxS2

    Science.gov (United States)

    Kassem, Mohamed A.; Tabata, Yoshikazu; Waki, Takeshi; Nakamura, Hiroyuki

    2015-09-01

    Single crystals of the shandite-type half metallic ferromagnet Co3Sn2S2, and its In-substituted compounds, Co3Sn2-xInxS2 (0crystals. Single crystals of the two end members, Co3Sn2S2 and Co3In2S2, and solid solutions with low In concentrations (x≤0.35) were grown out of Sn and In self flux. Solid solution single crystals with higher In concentrations were grown out of Sn, In and Pb mixture flux. Grown crystals were characterized using the powder x-ray diffraction, wavelength-dispersive x-ray spectroscopy and magnetization measurements. The shandite structure with R3¯m symmetry was confirmed and crystal structure parameters of the obtained plate-shaped hexagonal crystals were refined using the Rietveld analysis. Magnetization measurements show suppression of the ferromagnetic ordering, observed in Co3Sn2S2, by In-substitution as reported for polycrystalline samples. The obtained crystals are useful to study anisotropy in magnetic and transport properties and further interesting magnetotransport properties of the layered compounds.

  20. Characterization of photonic structures using visible and infrared polarimetry

    Directory of Open Access Journals (Sweden)

    Kral Z.

    2010-06-01

    Full Text Available Photonic Crystals are materials with a spatial periodic variation of the refractive index on the wavelength scale. This confers these materials interesting photonic properties such as the existence of photonic bands and forbidden photon frequency ranges, the photonic band gaps. Among their applications it is worth mentioning the achievement of low-threshold lasers and high-Q resonant cavities. A particular case of the Photonic Crystals is well-known and widely studied since a long time: the periodic thin film coatings. The characterization of thin film coatings is a classical field of study with a very well established knowledge. However, characterization of 2D and 3D photonic crystals needs to be studied in detail as it poses new problems that have to be solved. In this sense, Polarimetry is a specially suited tool given their inherent anisotropy: photonic bands depend strongly on the propagation direction and on polarization. In this work we show how photonic crystal structures can be characterized using polarimetry equipment. We compare the numerical modeling of the interaction of the light polarization with the photonic crystal with the polarimetry measurements. With the S-Matrix formalism, the Mueller matrix of a Photonic Crystal for a given wavelength, angle of incidence and propagation direction can be obtained. We will show that useful information from polarimetry (and also from spectrometry can be obtained when multivariate spectra are considered. We will also compare the simulation results with Polarimetry measurements on different kinds of samples: macroporous silicon photonic crystals in the near-IR range and Laser-Interference-Lithography nanostructured photoresist.

  1. Systematic analysis of crystal and molecular structures

    Czech Academy of Sciences Publication Activity Database

    Hašek, Jindřich; Dohnálek, Jan

    2012-01-01

    Roč. 19, č. 2 (2012), s. 86-87 ISSN 1211-5894. [Struktura 2012. Kolokvium Krystalografické společnosti. 11.06.2012-14.06.2012, Klatovy] R&D Projects: GA ČR GA310/09/1407 Institutional research plan: CEZ:AV0Z40500505 Institutional support: RVO:61389013 Keywords : structure databases * structure-function relations * organic and inorganic materials Subject RIV: EE - Microbiology, Virology

  2. The crystal structure of Toxoplasma gondii pyruvate kinase 1.

    Directory of Open Access Journals (Sweden)

    Rebecca Bakszt

    2010-09-01

    Full Text Available Pyruvate kinase (PK, which catalyzes the final step in glycolysis converting phosphoenolpyruvate to pyruvate, is a central metabolic regulator in most organisms. Consequently PK represents an attractive therapeutic target in cancer and human pathogens, like Apicomplexans. The phylum Aplicomplexa, a group of exclusively parasitic organisms, includes the genera Plasmodium, Cryptosporidium and Toxoplasma, the etiological agents of malaria, cryptosporidiosis and toxoplasmosis respectively. Toxoplasma gondii infection causes a mild illness and is a very common infection affecting nearly one third of the world's population.We have determined the crystal structure of the PK1 enzyme from T. gondii, with the B domain in the open and closed conformations. We have also characterized its enzymatic activity and confirmed glucose-6-phosphate as its allosteric activator. This is the first description of a PK enzyme in a closed inactive conformation without any bound substrate. Comparison of the two tetrameric TgPK1 structures indicates a reorientation of the monomers with a concomitant change in the buried surface among adjacent monomers. The change in the buried surface was associated with significant B domain movements in one of the interacting monomers.We hypothesize that a loop in the interface between the A and B domains plays an important role linking the position of the B domain to the buried surface among monomers through two α-helices. The proposed model links the catalytic cycle of the enzyme with its domain movements and highlights the contribution of the interface between adjacent subunits. In addition, an unusual ordered conformation was observed in one of the allosteric binding domains and it is related to a specific apicomplexan insertion. The sequence and structural particularity would explain the atypical activation by a mono-phosphorylated sugar. The sum of peculiarities raises this enzyme as an emerging target for drug discovery.

  3. The crystal structure of Toxoplasma gondii pyruvate kinase 1.

    Science.gov (United States)

    Bakszt, Rebecca; Wernimont, Amy; Allali-Hassani, Abdellah; Mok, Man Wai; Hills, Tanya; Hui, Raymond; Pizarro, Juan C

    2010-09-14

    Pyruvate kinase (PK), which catalyzes the final step in glycolysis converting phosphoenolpyruvate to pyruvate, is a central metabolic regulator in most organisms. Consequently PK represents an attractive therapeutic target in cancer and human pathogens, like Apicomplexans. The phylum Aplicomplexa, a group of exclusively parasitic organisms, includes the genera Plasmodium, Cryptosporidium and Toxoplasma, the etiological agents of malaria, cryptosporidiosis and toxoplasmosis respectively. Toxoplasma gondii infection causes a mild illness and is a very common infection affecting nearly one third of the world's population. We have determined the crystal structure of the PK1 enzyme from T. gondii, with the B domain in the open and closed conformations. We have also characterized its enzymatic activity and confirmed glucose-6-phosphate as its allosteric activator. This is the first description of a PK enzyme in a closed inactive conformation without any bound substrate. Comparison of the two tetrameric TgPK1 structures indicates a reorientation of the monomers with a concomitant change in the buried surface among adjacent monomers. The change in the buried surface was associated with significant B domain movements in one of the interacting monomers. We hypothesize that a loop in the interface between the A and B domains plays an important role linking the position of the B domain to the buried surface among monomers through two α-helices. The proposed model links the catalytic cycle of the enzyme with its domain movements and highlights the contribution of the interface between adjacent subunits. In addition, an unusual ordered conformation was observed in one of the allosteric binding domains and it is related to a specific apicomplexan insertion. The sequence and structural particularity would explain the atypical activation by a mono-phosphorylated sugar. The sum of peculiarities raises this enzyme as an emerging target for drug discovery.

  4. The Crystal Structure of Toxoplasma gondii Pyruvate Kinase 1

    Energy Technology Data Exchange (ETDEWEB)

    Bakszt, R.; Wernimont, A; Allali-Hassani, A; Mok, M; Hills, T; Hui, R; Pizarro, J

    2010-01-01

    Pyruvate kinase (PK), which catalyzes the final step in glycolysis converting phosphoenolpyruvate to pyruvate, is a central metabolic regulator in most organisms. Consequently PK represents an attractive therapeutic target in cancer and human pathogens, like Apicomplexans. The phylum Aplicomplexa, a group of exclusively parasitic organisms, includes the genera Plasmodium, Cryptosporidium and Toxoplasma, the etiological agents of malaria, cryptosporidiosis and toxoplasmosis respectively. Toxoplasma gondii infection causes a mild illness and is a very common infection affecting nearly one third of the world's population. We have determined the crystal structure of the PK1 enzyme from T. gondii, with the B domain in the open and closed conformations. We have also characterized its enzymatic activity and confirmed glucose-6-phosphate as its allosteric activator. This is the first description of a PK enzyme in a closed inactive conformation without any bound substrate. Comparison of the two tetrameric TgPK1 structures indicates a reorientation of the monomers with a concomitant change in the buried surface among adjacent monomers. The change in the buried surface was associated with significant B domain movements in one of the interacting monomers. We hypothesize that a loop in the interface between the A and B domains plays an important role linking the position of the B domain to the buried surface among monomers through two {alpha}-helices. The proposed model links the catalytic cycle of the enzyme with its domain movements and highlights the contribution of the interface between adjacent subunits. In addition, an unusual ordered conformation was observed in one of the allosteric binding domains and it is related to a specific apicomplexan insertion. The sequence and structural particularity would explain the atypical activation by a mono-phosphorylated sugar. The sum of peculiarities raises this enzyme as an emerging target for drug discovery.

  5. Two Voriconazole salts: Syntheses, crystal structures, solubility and bioactivities

    Science.gov (United States)

    Tang, Gui-Mei; Wang, Yong-Tao

    2018-01-01

    Two Voriconazole salts, namely, (H2FZ)2+·2(Cl-) (1) and (HFZ)+·NO3- (2) (FZ = (2R,3S)-2-(2,4-difluorophenyl)-3-(5-fluoro-4-pyrimidiny)-1-(1H-1,2,4-triazol-1-yl)-2-butanol) have been obtained through the reaction of Voriconazole, hydrochloric acid and nitrate acid, respectively. They were structurally characterized by FT-IR, elemental analyses (EA), single crystal X-ray diffraction, and thermogravimetric analysis (TGA). A variety of hydrogen bonds (Osbnd H⋯N, Nsbnd H⋯Cl/O, Csbnd H⋯N/OF/Cl) were observed in the compounds 1 and 2, through which a 3D supramolecular architecture is generated. Both two salts 1 and 2 show the promising bioactivities against Aspergillus species (Aspergillus niger, Aspergillus terreus, Aspergillus fumigatus and Aspergillus flavus) and Candida ones (Candida albicans, Candida krusei, Candida glabrata and Cryptococcus neoformans), which is obviously more excellent than that of FZ. Additionally, the solubility of two salts is considerably higher than that of the drug Voriconazole.

  6. Benzofuranyl Esters: Synthesis, Crystal Structure Determination, Antimicrobial and Antioxidant Activities

    Directory of Open Access Journals (Sweden)

    C. S. Chidan Kumar

    2015-09-01

    Full Text Available A series of five new 2‐(1‐benzofuran‐2‐yl‐2‐oxoethyl 4-(un/substitutedbenzoates 4(a–e, with the general formula of C8H5O(C=OCH2O(C=OC6H4X, X = H, Cl, CH3, OCH3 or NO2, was synthesized in high purity and good yield under mild conditions. The synthesized products 4(a–e were characterized by FTIR, 1H-, 13C- and 1H-13C HMQC NMR spectroscopic analysis and their 3D structures were confirmed by single-crystal X-ray diffraction studies. These compounds were screened for their antimicrobial and antioxidant activities. The tested compounds showed antimicrobial ability in the order of 4b < 4a < 4c < 4d < 4e and the highest potency with minimum inhibition concentration (MIC value of 125 µg/mL was observed for 4e. The results of antioxidant activities revealed the highest activity for compound 4e (32.62% ± 1.34% in diphenyl-2-picrylhydrazyl (DPPH radical scavenging, 4d (31.01% ± 4.35% in ferric reducing antioxidant power (FRAP assay and 4a (27.11% ± 1.06% in metal chelating (MC activity.

  7. Photonics of liquid-crystal structures: A review

    Energy Technology Data Exchange (ETDEWEB)

    Palto, S. P., E-mail: palto@online.ru; Blinov, L M; Barnik, M I; Lazarev, V V; Umanskii, B A; Shtykov, N M [Russian Academy of Sciences, Shubnikov Institute of Crystallography (Russian Federation)

    2011-07-15

    The original results of studies of the electro-optical and laser effects which have been performed at the Laboratory of Liquid Crystals of the Institute of Crystallography, Russian Academy of Sciences, over the last few years are reviewed. Cholesteric liquid crystals as vivid representatives of photonic structures and their behavior in an electric field are considered in detail. The formation of higher harmonics in the periodic distribution of the director field in a helical liquid crystal structure and, correspondingly, the new (anharmonic) mode of electro-optical effects are discussed. Another group of studies is devoted to bistable light switching by an electric field in chiral nematics. Polarization diffraction gratings controlled by an electric field are also considered. The results of studies devoted to microlasers on various photonic structures with cholesteric and nematic liquid crystals are considered in detail. Particular attention is given to the new regime: leaky-mode lasing. Designs of liquid crystal light amplifiers and their polarization, field, and spectral characteristics are considered in the last section.

  8. Thioaluminogermanate M(AlS2)(GeS2)4 (M = Na, Ag, Cu): Synthesis, Crystal Structures, Characterization, Ion-Exchange and Solid-State 27Al and 23Na NMR Spectroscopy

    KAUST Repository

    Alahmary, Fatimah S.

    2018-03-14

    The new thioaluminogermanate Na(AlS2)(GeS2)4 (1) was successfully synthesized by a direct combination reaction. The compound crystallizes in the monoclinic space group P21/n (no. 14) with unit cell parameters a = 6.803(3) Å, b = 38.207(2) Å, c = 6.947(4) Å, and β = 119.17(3)°. The crystal structure is composed of a [(AlS2)(GeS2)4]− 3D polyanionic network, in which Al and Ge atoms share the atomic positions and Na cations occupy the channels and voids formed by the connection of (Ge/Al)S4 tetrahedra. The title compound shows a cation-exchange property with monovalent Ag+ and Cu+ ions at room temperature in solvent media, resulting in the formation of the isostructural compounds Ag(AlS2)(GeS2)4 (2) and Cu(AlS2)(GeS2)4 (3), respectively. The ion-exchange products Ag(AlS2)(GeS2)4 (2) and Cu(AlS2)(GeS2)4 (3) show higher air stability and narrower bandgap energies compared to those of the parent compound Na(AlS2)(GeS2)4 (1).

  9. Thioaluminogermanate M(AlS2)(GeS2)4 (M = Na, Ag, Cu): Synthesis, Crystal Structures, Characterization, Ion-Exchange and Solid-State 27Al and 23Na NMR Spectroscopy

    KAUST Repository

    Alahmary, Fatimah S.; Davaasuren, Bambar; Emwas, Abdul-Hamid M.; Rothenberger, Alexander

    2018-01-01

    The new thioaluminogermanate Na(AlS2)(GeS2)4 (1) was successfully synthesized by a direct combination reaction. The compound crystallizes in the monoclinic space group P21/n (no. 14) with unit cell parameters a = 6.803(3) Å, b = 38.207(2) Å, c = 6.947(4) Å, and β = 119.17(3)°. The crystal structure is composed of a [(AlS2)(GeS2)4]− 3D polyanionic network, in which Al and Ge atoms share the atomic positions and Na cations occupy the channels and voids formed by the connection of (Ge/Al)S4 tetrahedra. The title compound shows a cation-exchange property with monovalent Ag+ and Cu+ ions at room temperature in solvent media, resulting in the formation of the isostructural compounds Ag(AlS2)(GeS2)4 (2) and Cu(AlS2)(GeS2)4 (3), respectively. The ion-exchange products Ag(AlS2)(GeS2)4 (2) and Cu(AlS2)(GeS2)4 (3) show higher air stability and narrower bandgap energies compared to those of the parent compound Na(AlS2)(GeS2)4 (1).

  10. CRYSTAL STRUCTURE ANALYSIS OF A PUTATIVE OXIDOREDUCTASE FROM KLEBSIELLA PNEUMONIAE

    Energy Technology Data Exchange (ETDEWEB)

    Baig, M.; Brown, A.; Eswaramoorthy, S.; Swaminathan, S.

    2009-01-01

    Klebsiella pneumoniae, a gram-negative enteric bacterium, is found in nosocomial infections which are acquired during hospital stays for about 10% of hospital patients in the United States. The crystal structure of a putative oxidoreductase from K. pneumoniae has been determined. The structural information of this K. pneumoniae protein was used to understand its function. Crystals of the putative oxidoreductase enzyme were obtained by the sitting drop vapor diffusion method using Polyethylene glycol (PEG) 3350, Bis-Tris buffer, pH 5.5 as precipitant. These crystals were used to collect X-ray data at beam line X12C of the National Synchrotron Light Source (NSLS) at Brookhaven National Laboratory (BNL). The crystal structure was determined using the SHELX program and refi ned with CNS 1.1. This protein, which is involved in the catalysis of an oxidation-reduction (redox) reaction, has an alpha/beta structure. It utilizes nicotinamide adenine dinucleotide phosphate (NADP) or nicotine adenine dinucleotide (NAD) to perform its function. This structure could be used to determine the active and co-factor binding sites of the protein, information that could help pharmaceutical companies in drug design and in determining the protein’s relationship to disease treatment such as that for pneumonia and other related pathologies.

  11. Solving crystal structures with the symmetry minimum function

    International Nuclear Information System (INIS)

    Estermann, M.A.

    1995-01-01

    Unravelling the Patterson function (the auto-correlation function of the crystal structure) (A.L. Patterson, Phys. Rev. 46 (1934) 372) can be the only way of solving crystal structures from neutron and incomplete diffraction data (e.g. powder data) when direct methods for phase determination fail. The negative scattering lengths of certain isotopes and the systematic loss of information caused by incomplete diffraction data invalidate the underlying statistical assumptions made in direct methods. In contrast, the Patterson function depends solely on the quality of the available diffraction data. Simpson et al. (P.G. Simpson et al., Acta Crystallogr. 18 (1965) 169) showed that solving a crystal structure with a particular superposition of origin-shifted Patterson functions, the symmetry minimum function, is advantageous over using the Patterson function alone, for single-crystal X-ray data.This paper describes the extension of the Patterson superposition approach to neutron data and powder data by (a) actively using the negative regions in the Patterson map caused by negative scattering lengths and (b) using maximum entropy Patterson maps (W.I.F. David, Nature 346 (1990) 731). Furthermore, prior chemical knowledge such as bond lengths and angles from known fragments have been included. Two successful structure solutions of a known and a previously unknown structure (M. Hofmann, J. Solid State Chem., in press) illustrate the potential of this new development. ((orig.))

  12. Synthesis, Crystal Structure, and DFT Calculations of 1,3-Diisobutyl Thiourea

    Directory of Open Access Journals (Sweden)

    Ataf A. Altaf

    2015-01-01

    Full Text Available 1,3-Diisobutyl thiourea was synthesized and characterized by single crystal X-ray diffraction. It gives a monoclinic (α = γ = 90 and β  ≠ 90 structure with the space group P21/c. The unit cell dimensions are a = 11.5131 (4 Å, b = 9.2355 (3 Å, c = 11.3093 (5 Å, α = 90°, β = 99.569° (2, γ = 90°, V = 1185.78 (8 Å3, and Z = 4. The crystal packing is stabilized by intermolecular (N–H⋯S hydrogen bonding in the molecules. The optimized geometry and Mullikan's charges of the said molecule calculated with the help of DFT using B3LYP-6-311G model support the crystal structure.

  13. PAK4 crystal structures suggest unusual kinase conformational movements.

    Science.gov (United States)

    Zhang, Eric Y; Ha, Byung Hak; Boggon, Titus J

    2018-02-01

    In order for protein kinases to exchange nucleotide they must open and close their catalytic cleft. These motions are associated with rotations of the N-lobe, predominantly around the 'hinge region'. We conducted an analysis of 28 crystal structures of the serine-threonine kinase, p21-activated kinase 4 (PAK4), including three newly determined structures in complex with staurosporine, FRAX486, and fasudil (HA-1077). We find an unusual motion between the N-lobe and C-lobe of PAK4 that manifests as a partial unwinding of helix αC. Principal component analysis of the crystal structures rationalizes these movements into three major states, and analysis of the kinase hydrophobic spines indicates concerted movements that create an accessible back pocket cavity. The conformational changes that we observe for PAK4 differ from previous descriptions of kinase motions, and although we observe these differences in crystal structures there is the possibility that the movements observed may suggest a diversity of kinase conformational changes associated with regulation. Protein kinases are key signaling proteins, and are important drug targets, therefore understanding their regulation is important for both basic research and clinical points of view. In this study, we observe unusual conformational 'hinging' for protein kinases. Hinging, the opening and closing of the kinase sub-domains to allow nucleotide binding and release, is critical for proper kinase regulation and for targeted drug discovery. We determine new crystal structures of PAK4, an important Rho-effector kinase, and conduct analyses of these and previously determined structures. We find that PAK4 crystal structures can be classified into specific conformational groups, and that these groups are associated with previously unobserved hinging motions and an unusual conformation for the kinase hydrophobic core. Our findings therefore indicate that there may be a diversity of kinase hinging motions, and that these may

  14. Simulation and design of the photonic crystal microwave accelerating structure

    International Nuclear Information System (INIS)

    Song Ruiying; Wu Congfeng; He Xiaodong; Dong Sai

    2007-01-01

    The authors have derived the global band gaps for general two-dimensional (2D) photonic crystal microwave accelerating structures formed by square or triangular arrays of metal posts. A coordinate-space, finite-difference code was used to calculate the complete dispersion curves for the lattices. The fundamental and higher frequency global photonic band gaps were determined numerically. The structure formed by triangular arrays of metal posts with a missing rod at the center has advantages of higher-order-modes (HOM) suppression and main mode restriction under the condition of a/b<0.2. The relationship between the RF properties and the geometrical parameters have been studied for the 9.37 GHz photonic crystal accelerating structure. The Rs, Q, Rs/Q of the new structure may be comparable to the disk-loaded accelerating structure. (authors)

  15. Synthesis, Crystal Structure, Density Function Theory, Molecular ...

    African Journals Online (AJOL)

    Tropical Journal of Pharmaceutical Research ... Purpose: To determine the exact structure and antimicrobial activity of 2-(3-(4 phenylpiperazin-1-yl) ... Besides HOMO– LUMO energy gap was performed at B3LYP/6-31G (d,p) level of theory.

  16. Crystal engineering of ibuprofen compounds: From molecule to crystal structure to morphology prediction by computational simulation and experimental study

    Science.gov (United States)

    Zhang, Min; Liang, Zuozhong; Wu, Fei; Chen, Jian-Feng; Xue, Chunyu; Zhao, Hong

    2017-06-01

    We selected the crystal structures of ibuprofen with seven common space groups (Cc, P21/c, P212121, P21, Pbca, Pna21, and Pbcn), which was generated from ibuprofen molecule by molecular simulation. The predicted crystal structures of ibuprofen with space group P21/c has the lowest total energy and the largest density, which is nearly indistinguishable with experimental result. In addition, the XRD patterns for predicted crystal structure are highly consistent with recrystallization from solvent of ibuprofen. That indicates that the simulation can accurately predict the crystal structure of ibuprofen from the molecule. Furthermore, based on this crystal structure, we predicted the crystal habit in vacuum using the attachment energy (AE) method and considered solvent effects in a systematic way using the modified attachment energy (MAE) model. The simulation can accurately construct a complete process from molecule to crystal structure to morphology prediction. Experimentally, we observed crystal morphologies in four different polarity solvents compounds (ethanol, acetonitrile, ethyl acetate, and toluene). We found that the aspect ratio decreases of crystal habits in this ibuprofen system were found to vary with increasing solvent relative polarity. Besides, the modified crystal morphologies are in good agreement with the observed experimental morphologies. Finally, this work may guide computer-aided design of the desirable crystal morphology.

  17. Single Crystals of Organolead Halide Perovskites: Growth, Characterization, and Applications

    KAUST Repository

    Peng, Wei

    2017-01-01

    Despite their outstanding charge transport characteristics, organolead halide perovskite single crystals grown by hitherto reported crystallization methods are not suitable for most optoelectronic devices due to their small aspect ratios

  18. Growth and characterization of nonlinear optical single crystals: bis ...

    Indian Academy of Sciences (India)

    Administrator

    molecules have received great attention for NLO applica- tions. However ... Figure 3. Single crystals of bis(cyclohexylammonium) terephthalate (crystal a) and cyclohexylammo- .... from ground state to higher energy states.17 Optical window ...

  19. Crystallization and preliminary crystallographic characterization of the PAS domains of EAG and ELK potassium channels

    International Nuclear Information System (INIS)

    Adaixo, Ricardo; Morais-Cabral, João Henrique

    2010-01-01

    The N-terminal PAS domains from the eukaryotic EAG potassium channels are thought to have a regulatory function. Here the expression, purification, crystallization and preliminary crystallographic characterization of two of these domains are described. Per–Arnt–Sim (PAS) domains are ubiquitous in nature; they are ∼130-amino-acid protein domains that adopt a fairly conserved three-dimensional structure despite their low degree of sequence homology. These domains constitute the N-terminus or, less frequently, the C-terminus of a number of proteins, where they exert regulatory functions. PAS-containing proteins generally display two or more copies of this motif. In this work, the crystallization and preliminary analysis of the PAS domains of two eukaryotic potassium channels from the ether-à-go-go (EAG) family are reported

  20. Impact of growth temperature on the crystal habits, forms and structures of VO2 nanocrystals

    International Nuclear Information System (INIS)

    Loeffler, Stefan; Auer, Erwin; Lugstein, Alois; Bertagnolli, Emmerich; Weil, Matthias

    2011-01-01

    We investigated the impact of the process temperature on the habits, forms and crystal structure of VO 2 nanocrystals grown by a vapor-transport method on (0001) quartz substrates. Four distinct growth regimes were discerned: orthorhombic nanowires, sheets, hemispheres, and nanowires with a monoclinic structure. The nanostructures were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), and transmission electron microscopy (TEM). I/V characterization of individual nanowires was enabled by Ti/Au contact formation via electron beam lithography and lift-off techniques. The expected metal-insulator transition (MIT) was found in monoclinic VO 2 nanowires. (orig.)

  1. Characterization of polypropylene–polyethylene blends by temperature rising elution and crystallization analysis fractionation

    Science.gov (United States)

    del Hierro, Pilar

    2010-01-01

    The introduction of single-site catalysts in the polyolefins industry opens new routes to design resins with improved performance through multicatalyst-multireactor processes. Physical combination of various polyolefin types in a secondary extrusion process is also a common practice to achieve new products with improved properties. The new resins have complex structures, especially in terms of composition distribution, and their characterization is not always an easy task. Techniques like temperature rising elution fractionation (TREF) or crystallization analysis fractionation (CRYSTAF) are currently used to characterize the composition distribution of these resins. It has been shown that certain combinations of polyolefins may result in equivocal results if only TREF or CRYSTAF is used separately for their characterization. PMID:20730530

  2. Magnetic assembly of nonmagnetic particles into photonic crystal structures.

    Science.gov (United States)

    He, Le; Hu, Yongxing; Kim, Hyoki; Ge, Jianping; Kwon, Sunghoon; Yin, Yadong

    2010-11-10

    We report the rapid formation of photonic crystal structures by assembly of uniform nonmagnetic colloidal particles in ferrofluids using external magnetic fields. Magnetic manipulation of nonmagnetic particles with size down to a few hundred nanometers, suitable building blocks for producing photonic crystals with band gaps located in the visible regime, has been difficult due to their weak magnetic dipole moment. Increasing the dipole moment of magnetic holes has been limited by the instability of ferrofluids toward aggregation at high concentration or under strong magnetic field. By taking advantage of the superior stability of highly surface-charged magnetite nanocrystal-based ferrofluids, in this paper we have been able to successfully assemble 185 nm nonmagnetic polymer beads into photonic crystal structures, from 1D chains to 3D assemblies as determined by the interplay of magnetic dipole force and packing force. In a strong magnetic field with large field gradient, 3D photonic crystals with high reflectance (83%) in the visible range can be rapidly produced within several minutes, making this general strategy promising for fast creation of large-area photonic crystals using nonmagnetic particles as building blocks.

  3. Crystal structure and vibrational spectra of piperazinium bis(4-hydroxybenzenesulphonate) molecular-ionic crystal

    Science.gov (United States)

    Marchewka, M. K.; Pietraszko, A.

    2008-02-01

    The piperazinium bis(4-hydroxybenzenesulphonate) crystallizes from water solution at room temperature in P2 1/ c space group of monoclinic system. The crystals are built up of doubly protonated piperazinium cations and ionized 4-hydroxybenzenesulphonate anions that interact through weak hydrogen bonds of O-H⋯O and N-H⋯O type. Mutual orientation of anions is determined by non-conventional hydrogen bonds of C-H⋯π type. Room temperature powder FT IR and FT Raman measurements were carried out. The vibrational spectra are in full agreement with the structure obtained from X-ray crystallography. The big single crystals of the title salt can be grown.

  4. Structural science using single crystal and pulse neutron scattering

    International Nuclear Information System (INIS)

    Noda, Yukio; Kimura, Hiroyuki; Watanabe, Masashi; Ishikawa, Yoshihisa; Tamura, Itaru; Arai, Masatoshi; Takahashi, Miwako; Ohshima, Ken-ichi; Abe, Hiroshi; Kamiyama, Takashi

    2008-01-01

    The application to single crystal neutron structural analysis is overviewed. Special attention is paid to the pulse neutron method, which will be available soon under J-PARC project in Japan. New proposal and preliminary experiment using Sirius at KENS are described. (author)

  5. BiFeO3 Crystal Structure at Low Temperatures

    International Nuclear Information System (INIS)

    Palewicz, A.; Sosnowska, I.; Przenioslo, R.; Hewat, A.W.

    2010-01-01

    The crystal and magnetic structure of BiFeO 3 have been studied with the use of high resolution neutron diffraction between 5 K and 300 K. The atomic coordinates in BiFeO 3 are almost unchanged between 5 K and 300 K. (authors)

  6. Effect of domains configuration on crystal structure in ferroelectric ...

    Indian Academy of Sciences (India)

    2017-09-09

    Sep 9, 2017 ... It is well known that domains and crystal structure control the physical properties of ferroelectrics. ... The as-prepared ceramics were crushed to fine pow- ders. ..... [1] Gao J, Xue D, Wang Y, Wang D, Zhang L, Wu H et al 2011.

  7. Magnetic structure of URhSi single crystal

    Czech Academy of Sciences Publication Activity Database

    Prokeš, K.; Andreev, Alexander V.; Honda, F.; Sechovský, V.

    2003-01-01

    Roč. 261, - (2003), s. 131-138 ISSN 0304-8853 R&D Projects: GA ČR GA202/02/0739 Institutional research plan: CEZ:AV0Z1010914 Keywords : URhSi single crystal * magnetization * neutron diffraction * magnetic structure determination Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.910, year: 2003

  8. Fine structure of fields in 2D photonic crystal waveguides

    DEFF Research Database (Denmark)

    Lavrinenko, Andrei; Volkov, V. S.; Bozhevolnyi, S. I.

    2006-01-01

    We resolve fine structure of fields in a single-row missing photonic crystal waveguide by finite-difference time-domain modelling and SNOM measurements. Both linear dispersion and slow-light regimes in proximity of the cutoff are addressed in the analysis....

  9. Unusual Features of Crystal Structures of Some Simple Copper Compounds

    Science.gov (United States)

    Douglas, Bodie

    2009-01-01

    Some simple copper compounds have unusual crystal structures. Cu[subscript 3]N is cubic with N atoms at centers of octahedra formed by 6 Cu atoms. Cu[subscript 2]O (cuprite) is also cubic; O atoms are in tetrahedra formed by 4 Cu atoms. These tetrahedra are linked by sharing vertices forming two independent networks without linkages between them.…

  10. Isomorph invariance of the structure and dynamics of classical crystals

    DEFF Research Database (Denmark)

    Albrechtsen, Dan; Olsen, Andreas Elmerdahl; Pedersen, Ulf Rørbæk

    2014-01-01

    This paper shows by computer simulations that some crystalline systems have curves in their thermodynamic phase diagrams, so-called isomorphs, along which structure and dynamics in reduced units are invariant to a good approximation. The crystals are studied in a classical-mechanical framework...

  11. Variational cellular model of the molecular and crystal electronic structure

    International Nuclear Information System (INIS)

    Ferreira, L.G.; Leite, J.R.

    1977-12-01

    A variational version of the cellular method is developed to calculate the electronic structure of molecules and crystals. Due to the simplicity of the secular equation, the method is easy to be implemented. Preliminary calculations on the hydrogen molecular ion suggest that it is also accurate and of fast convergence [pt

  12. Crystallized solids characterization by X-ray diffraction

    International Nuclear Information System (INIS)

    Broll, N.

    1996-01-01

    This work deals with the crystallized solids characterization by X-ray diffraction. The powders diffraction principle is described. Then are given the different powders diffraction experimental methods. An X-ray diffraction device is essentially constituted of three parts: the X-rays source, the sample and the detector. The source is usually constituted by an X-rays tube whereas the sample can be fixed on a photographic chamber or put on a goniometer. The different photographic chambers which can be used (Debye-Scherrer, Seeman-Bohlin and Guinier) are described. The powders diffractometer the most used is a Bragg-Brentano focusing diffractometer because it allows to obtain very sharp spectral lines and an important diffracted intensity. The detectors which are the mainly used are the scintillation counters. The most important use in powders diffractometry is the identification of the different phases of a sample. The phases identification consists to compare the unknown sample spectrum at those of standard materials indexed until now. Two methods exist at present. They are explained and their limits in the phases search are given. Another use of the X-ray diffraction is the quantitative analysis. It consists to determine the concentrations of each crystal phases of a sample. The principles of these quantitative methods are given. The lattice parameters of a polycrystal material can be determined from its X-ray pattern too with a very high precision. The way to index powders patterns is given. The residual stresses of materials can also be estimated. The principle of this measured method is explained. It is at last possible to study from an X-ray pattern, the material grain orientations during the different steps of preparation and working. (O.M.). 13 refs., 19 figs., 1 tab

  13. Synthesis, crystal structures and properties of lead phosphite compounds

    International Nuclear Information System (INIS)

    Song, Jun-Ling; Hu, Chun-Li; Xu, Xiang; Kong, Fang; Mao, Jiang-Gao

    2015-01-01

    Here, we report the preparation and characterization of two lead(II) phosphites, namely, Pb_2(HPO_3)_2 and Pb_2(HPO_3)(NO_3)_2 through hydrothermal reaction or simple solution synthesis, respectively. A new lead phosphite, namely, Pb_2(HPO_3)_2, crystallizes in the noncentrosymmetric space group Cmc2_1 (no. 36), which features 3D framework formed by the interconnection of 2D layer of lead(II) phosphites and 1D chain of [Pb(HPO_3)_5]_∞. The nonlinear optical properties of Pb_2(HPO_3)(NO_3)_2 have been studied for the first time. The synergistic effect of the stereo-active lone-pairs on Pb"2"+ cations and π-conjugated NO_3 units in Pb_2(HPO_3)(NO_3)_2 produces a moderate second harmonic generation (SHG) response of ∼1.8×KDP (KH_2PO_4), which is phase matchable (type I). IR, UV–vis spectra and thermogravimetric analysis (TGA) for the two compounds were also measured. - Graphical abstract: Two lead phosphites Pb_2(HPO_3)_2 and Pb_2(HPO_3)(NO_3)_2 are studied. A new lead phosphite Pb_2(HPO_3)_2 features a unique 3D framework structure and Pb_2(HPO_3)(NO_3)_2 shows a moderate SHG response of ∼1.8×KDP (KH_2PO_4). - Highlights: • A new lead phosphite, Pb_2(HPO_3)_2 is reported. • Pb_2(HPO_3)_2 features a unique 3D framework structure. • NLO property of Pb_2(HPO_3)(NO_3)_2 is investigated. • Pb_2(HPO_3)(NO_3)_2 produces a moderate SHG response of ∼1.8×KDP (KH_2PO_4).

  14. A unified picture of the crystal structures of metals

    Science.gov (United States)

    Söderlind, Per; Eriksson, Olle; Johansson, Börje; Wills, J. M.; Boring, A. M.

    1995-04-01

    THE crystal structures of the light actinides have intrigued physicists and chemists for several decades1. Simple metals and transition metals have close-packed, high-symmetry structures, such as body-centred cubic, face-centred cubic and hexagonal close packing. In contrast, the structures of the light actinides are very loosely packed and of low symmetry-tetragonal, orthorhombic and monoclinic. To understand these differences, we have performed total-energy calculations, as a function of volume, for both high-and low-symmetry structures of a simple metal (aluminium), a non-magnetic transition metal (niobium), a ferromagnetic transition metal (iron) and a light actinide (uranium). We find that the crystal structure of all of these metals is determined by the balance between electrostatic (Madelung) interactions, which favour high symmetry, and a Peierls distortion of the crystal lattice, which favours low symmetry. We show that simple metals and transition metals can adopt low-symmetry structures on expansion of the lattice; and we predict that, conversely, the light actinides will undergo transitions to structures of higher symmetry on compression.

  15. A unified picture of the crystal structures of metals

    International Nuclear Information System (INIS)

    Soederlind, P.; Eriksson, O.; Johansson, B.; Wills, J.M.; Boring, A.M.

    1995-01-01

    The crystal structures of the light actinides have intrigued physicists and chemists for several decades. Simple metals and transition metals have close-packed, high-symmetry structures, such as body-centred cubic, face-centred cubic hexagonal close packing. In contrast, the structures of the light actinides are very loosely packed and of low symmetry -tetragonal, orthorhombic and monoclinic. To understand these differences, we have have performed total-energy calculations, as a function of volume, for both high- and low-symmetry structures of a simple metal (aluminium), a non-magnetic transition metal (niobium), a ferromagnetic transition metal (iron) and a light actinide (uranium). We find that the crystal structure of all these metals is determined by the balance between electrostatic (Madelung) interactions, which favour high symmetry, and a Peierls distortion of the crystal lattice, which favours low symmetry. We show that simple metals and transition metals can adopt low-symmetry structures on expansion of the lattice; and we predict that, conversely, the light actinides will undergo transitions to structures of higher symmetry on compression. (author)

  16. Coefficient of crystal lattice matching as a parameter of substrate - crystal structure compatibility in silumins

    Directory of Open Access Journals (Sweden)

    J. Piątkowski

    2009-07-01

    Full Text Available Adding high-melting point elements (Mo, Nb, Ni, Ti, W to complex silumins results in hardening of the latter ones, owing to the formation of new intermetallic phases of the AlxMey type, with refinement of dendrites in α solution and crystals in β phase. The hardening is also due to the effect of various inoculants. An addition of the inoculant is expected to form substrates, the crystal lattice of which, or some (privileged lattice planes and interatomic spaces should bear a strong resemblance to the crystal nucleus. To verify this statement, using binary phase equilibria systems, the coefficient of crystal lattice matching, being one of the measures of the crystallographic similarity, was calculated. A compatibility of this parameter (up to 20% may decide about the structure compatibility between the substrate and crystal which, in turn, is responsible for the effectiveness of alloy modification. Investigations have proved that, given the temperature range of their formation, the density, the lattice type, and the lattice parameter, some intermetallic phases of the AlxMey type can act as substrates for the crystallisation of aluminium and silicon, and some of the silumin hardening phases.

  17. Band structures in Sierpinski triangle fractal porous phononic crystals

    International Nuclear Information System (INIS)

    Wang, Kai; Liu, Ying; Liang, Tianshu

    2016-01-01

    In this paper, the band structures in Sierpinski triangle fractal porous phononic crystals (FPPCs) are studied with the aim to clarify the effect of fractal hierarchy on the band structures. Firstly, one kind of FPPCs based on Sierpinski triangle routine is proposed. Then the influence of the porosity on the elastic wave dispersion in Sierpinski triangle FPPCs is investigated. The sensitivity of the band structures to the fractal hierarchy is discussed in detail. The results show that the increase of the hierarchy increases the sensitivity of ABG (Absolute band gap) central frequency to the porosity. But further increase of the fractal hierarchy weakens this sensitivity. On the same hierarchy, wider ABGs could be opened in Sierpinski equilateral triangle FPPC; whilst, a lower ABG could be opened at lower porosity in Sierpinski right-angled isosceles FPPCs. These results will provide a meaningful guidance in tuning band structures in porous phononic crystals by fractal design.

  18. Band structures in Sierpinski triangle fractal porous phononic crystals

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Kai; Liu, Ying, E-mail: yliu5@bjtu.edu.cn; Liang, Tianshu

    2016-10-01

    In this paper, the band structures in Sierpinski triangle fractal porous phononic crystals (FPPCs) are studied with the aim to clarify the effect of fractal hierarchy on the band structures. Firstly, one kind of FPPCs based on Sierpinski triangle routine is proposed. Then the influence of the porosity on the elastic wave dispersion in Sierpinski triangle FPPCs is investigated. The sensitivity of the band structures to the fractal hierarchy is discussed in detail. The results show that the increase of the hierarchy increases the sensitivity of ABG (Absolute band gap) central frequency to the porosity. But further increase of the fractal hierarchy weakens this sensitivity. On the same hierarchy, wider ABGs could be opened in Sierpinski equilateral triangle FPPC; whilst, a lower ABG could be opened at lower porosity in Sierpinski right-angled isosceles FPPCs. These results will provide a meaningful guidance in tuning band structures in porous phononic crystals by fractal design.

  19. Domain Structures in Nematic Liquid Crystals on a Polycarbonate Surface

    Directory of Open Access Journals (Sweden)

    Vasily F. Shabanov

    2013-08-01

    Full Text Available Alignment of nematic liquid crystals on polycarbonate films obtained with the use of solvents with different solvations is studied. Domain structures occurring during the growth on the polymer surface against the background of the initial thread-like or schlieren texture are demonstrated. It is established by optical methods that the domains are stable formations visualizing the polymer surface structures. In nematic droplets, the temperature-induced transition from the domain structure with two extinction bands to the structure with four bands is observed. This transition is shown to be caused by reorientation of the nematic director in the liquid crystal volume from the planar alignment to the homeotropic state with the pronounced radial configuration of nematic molecules on the surface. The observed textures are compared with different combinations of the volume LC orientations and the radial distribution of the director field and the disclination lines at the polycarbonate surface.

  20. Crystal structure and energy band and optical properties of phosphate Sr3P4O13

    International Nuclear Information System (INIS)

    Zhang, Y.-C.; Cheng, W.-D.; Wu, D.-S.; Zhang, H.; Chen, D.-G.; Gong, Y.-J.; Kan, Z.-G.

    2004-01-01

    A single crystal of the compound Sr 3 P 4 O 13 has been found and the crystal structure has been characterized by means of single crystal X-ray diffraction analysis. The compound crystallizes in triclinic system and belongs to space group P1-bar. It builds up from SrO 7 polyhedra and P 4 O 13 -6 anions and has a layered structure, and the Sr atoms are located in the interlayer space. The absorption and luminescence spectrum of Sr 3 P 4 O 13 microcrystals have been measured. The calculated results of crystal energy band structure by the DFT show that the solid state of Sr 3 P 4 O 13 is an isolator with direct band gap. The calculated total and partial density of states indicate that the top valence bands are contributions from P 3p and O 2p states and low conduction bands mostly originate from Sr atomic states. The calculated optical response functions expect that the Sr 3 P 4 O 13 is a low refractive index, and it is possible that the Sr 3 P 4 O 13 is used to make transparent material between the UV and FR light zone

  1. Structural characterization of indium oxide nanostructures: a Raman analysis

    International Nuclear Information System (INIS)

    Berengue, Olivia M; Rodrigues, Ariano D; Chiquito, Adenilson J; Dalmaschio, Cleocir J; Leite, Edson R; Lanfredi, Alexandre J C

    2010-01-01

    In this work we report on structural and Raman spectroscopy measurements of pure and Sn-doped In 2 O 3 nanowires. Both samples were found to be cubic and high quality single crystals. Raman analysis was performed to obtain the phonon modes of the nanowires and to confirm the compositional and structural information given by structural characterization. Cubic-like phonon modes were detected in both samples and their distinct phase was evidenced by the presence of tin doping. As a consequence, disorder effects were detected evidenced by the break of the Raman selection rules.

  2. Protein crystal structure analysis using synchrotron radiation at atomic resolution

    International Nuclear Information System (INIS)

    Nonaka, Takamasa

    1999-01-01

    We can now obtain a detailed picture of protein, allowing the identification of individual atoms, by interpreting the diffraction of X-rays from a protein crystal at atomic resolution, 1.2 A or better. As of this writing, about 45 unique protein structures beyond 1.2 A resolution have been deposited in the Protein Data Bank. This review provides a simplified overview of how protein crystallographers use such diffraction data to solve, refine, and validate protein structures. (author)

  3. Crystal structure of new AsS2 compound

    International Nuclear Information System (INIS)

    Bolotina, N. B.; Brazhkin, V. V.; Dyuzheva, T. I.; Lityagina, L. M.; Kulikova, L. F.; Nikolaev, N. A.; Verin, I. A.

    2013-01-01

    AsS 2 single crystals have been obtained for the first time from an As 2 S 3 melt at pressures above 6 GPa and temperatures above 800 K in the As 2 S 3 → AsS + AsS 2 reaction. The monoclinic structure of the new high-pressure phase is solved by X-ray diffraction analysis and compared to the structure of high-pressure AsS phase, which was studied previously.

  4. Spatially periodic structures, under femtosecond pulsed excitation of crystals

    International Nuclear Information System (INIS)

    Martynovitch, Evgueni F.; Petite, Guillaume; Dresvianski, Vladimir P.; Starchenko, Anton A.

    2004-01-01

    Measuring the luminescence intensity of specially prepared irradiation defects induced in crystals, we observe that the longitudinal structure of quasi-interferences induced by two orthogonally polarized femtosecond pulses propagating together with different velocities is insensitive to the spatial broadening due to velocity dispersion in the crystals. On the contrary, it does depend on the pulse duration when it is changed by varying the spectral width of the radiation. It thus allows a direct measurement of the coherence time of such pulses. Stability of the axial selectivity is a good sign, taking away a number of serious limitations concerning possible applications

  5. TaRh2B2 and NbRh2B2: Superconductors with a chiral noncentrosymmetric crystal structure.

    Science.gov (United States)

    Carnicom, Elizabeth M; Xie, Weiwei; Klimczuk, Tomasz; Lin, Jingjing; Górnicka, Karolina; Sobczak, Zuzanna; Ong, Nai Phuan; Cava, Robert J

    2018-05-01

    It is a fundamental truth in solid compounds that the physical properties follow the symmetry of the crystal structure. Nowhere is the effect of symmetry more pronounced than in the electronic and magnetic properties of materials-even the projection of the bulk crystal symmetry onto different crystal faces is known to have a substantial impact on the surface electronic states. The effect of bulk crystal symmetry on the properties of superconductors is widely appreciated, although its study presents substantial challenges. The effect of a lack of a center of symmetry in a crystal structure, for example, has long been understood to necessitate that the wave function of the collective electron state that gives rise to superconductivity has to be more complex than usual. However, few nonhypothetical materials, if any, have actually been proven to display exotic superconducting properties as a result. We introduce two new superconductors that in addition to having noncentrosymmetric crystal structures also have chiral crystal structures. Because the wave function of electrons in solids is particularly sensitive to the host material's symmetry, crystal structure chirality is expected to have a substantial effect on their superconducting wave functions. Our two experimentally obtained chiral noncentrosymmetric superconducting materials have transition temperatures to superconductivity that are easily experimentally accessible, and our basic property characterization suggests that their superconducting properties may be unusual. We propose that their study may allow for a more in-depth understanding of how chirality influences the properties of superconductors and devices that incorporate them.

  6. Crystal structure representations for machine learning models of formation energies

    Energy Technology Data Exchange (ETDEWEB)

    Faber, Felix [Department of Chemistry, Institute of Physical Chemistry and National Center for Computational Design and Discovery of Novel Materials, University of Basel Switzerland; Lindmaa, Alexander [Department of Physics, Chemistry and Biology, Linköping University, SE-581 83 Linköping Sweden; von Lilienfeld, O. Anatole [Department of Chemistry, Institute of Physical Chemistry and National Center for Computational Design and Discovery of Novel Materials, University of Basel Switzerland; Argonne Leadership Computing Facility, Argonne National Laboratory, 9700 S. Cass Avenue Lemont Illinois 60439; Armiento, Rickard [Department of Physics, Chemistry and Biology, Linköping University, SE-581 83 Linköping Sweden

    2015-04-20

    We introduce and evaluate a set of feature vector representations of crystal structures for machine learning (ML) models of formation energies of solids. ML models of atomization energies of organic molecules have been successful using a Coulomb matrix representation of the molecule. We consider three ways to generalize such representations to periodic systems: (i) a matrix where each element is related to the Ewald sum of the electrostatic interaction between two different atoms in the unit cell repeated over the lattice; (ii) an extended Coulomb-like matrix that takes into account a number of neighboring unit cells; and (iii) an ansatz that mimics the periodicity and the basic features of the elements in the Ewald sum matrix using a sine function of the crystal coordinates of the atoms. The representations are compared for a Laplacian kernel with Manhattan norm, trained to reproduce formation energies using a dataset of 3938 crystal structures obtained from the Materials Project. For training sets consisting of 3000 crystals, the generalization error in predicting formation energies of new structures corresponds to (i) 0.49, (ii) 0.64, and (iii) 0.37eV/atom for the respective representations.

  7. Crystal structure and magnetism of UOsAl

    Energy Technology Data Exchange (ETDEWEB)

    Andreev, A.V., E-mail: andreev@fzu.cz [Institute of Physics, Academy of Sciences, Na Slovance 2, 182 21 Prague (Czech Republic); Daniš, S. [Department of Condensed Matter Physics, Charles University, Ke Karlovu 5, 121 16 Prague (Czech Republic); Šebek, J.; Henriques, M.S.; Vejpravová, J. [Institute of Physics, Academy of Sciences, Na Slovance 2, 182 21 Prague (Czech Republic); Gorbunov, D.I. [Institute of Physics, Academy of Sciences, Na Slovance 2, 182 21 Prague (Czech Republic); Dresden High Magnetic Field Laboratory (HLD-EMFL), Helmholtz-Zentrum, Dresden-Rossendorf, D-01314 Dresden (Germany); Havela, L. [Department of Condensed Matter Physics, Charles University, Ke Karlovu 5, 121 16 Prague (Czech Republic)

    2017-04-15

    Crystal structure, magnetization, and specific heat were studied on single crystal of uranium intermetallic compound UOsAl. It is a hexagonal Laves phase of MgZn{sub 2} type, space group P6{sub 3}/mmc, with lattice parameters a=536.4 pm, c=845.3 pm. Shortest inter-uranium distance 313 pm (along the c-axis) is considerably smaller than the Hill limit (340 pm). The compound is a weakly temperature-dependent paramagnet with magnetic susceptibility of ≈1.5*10{sup −8} m{sup 3} mol{sup −1} (at T=2 K), which is slightly higher with magnetic field along the a-axis compared to the c-axis. The Sommerfeld coefficient of electronic specific heat has moderate value of γ=36 mJ mol{sup −1} K{sup −2}. - Highlights: • Crystal structure and magnetic properties were studied on single crystal of UOsAl with hexagonal structure of MgZn{sub 2} type. • Shortest inter-uranium distance 313 pm (along the c-axis) is considerably smaller than the Hill limit (340 pm). • UOsAl has paramagnetic ground state as the compounds with T=Fe and Ru, i.e. 3d and 4d analogues of Os.

  8. Icosahedral symmetry described by an incommensurately modulated crystal structure model

    DEFF Research Database (Denmark)

    Wolny, Janusz; Lebech, Bente

    1986-01-01

    A crystal structure model of an incommensurately modulated structure is presented. Although six different reciprocal vectors are used to describe the model, all calculations are done in three dimensions making calculation of the real-space structure trivial. Using this model, it is shown that both...... the positions of the bragg reflections and information about the relative intensities of these reflections are in full accordance with the diffraction patterns reported for microcrystals of the rapidly quenched Al86Mn14 alloy. It is also shown that at least the local structure possesses full icosahedral...

  9. Twinning structures in near-stoichiometric lithium niobate single crystals

    International Nuclear Information System (INIS)

    Yao, Shuhua; Chen, Yanfeng

    2010-01-01

    A near-stoichiometric lithium niobate single crystal has been grown by the Czochralski method in a hanging double crucible with a continuous powder supply system. Twins were found at one of the three characteristic growth ridges of the as-grown crystal. The twin structure was observed and analyzed by transmission synchrotron topography. The image shifts ΔX and ΔY in the transmission synchrotron topograph were calculated for the 3 anti 2 anti 12 and 0 anti 222 reflections based on results from high-resolution X-ray diffractometry. It is confirmed that one of the {01 anti 1 anti 2} m planes is the composition face of the twin and matrix crystals. The formation mechanism of these twins is discussed. (orig.)

  10. Crystal structure of N-(quinolin-6-ylhydroxylamine

    Directory of Open Access Journals (Sweden)

    Anuruddha Rajapakse

    2014-11-01

    Full Text Available The title compound, C9H8N2O, crystallized with four independent molecules in the asymmetric unit. The four molecules are linked via one O—H...N and two N—H...N hydrogen bonds, forming a tetramer-like unit. In the crystal, molecules are further linked by O—H...N and N—H...O hydrogen bonds forming layers parallel to (001. These layers are linked via C—H...O hydrogen bonds and a number of weak C—H...π interactions, forming a three-dimensional structure. The crystal was refined as a non-merohedral twin with a minor twin component of 0.319.

  11. Production, purification, crystallization and structure determination of H-1 Parvovirus

    International Nuclear Information System (INIS)

    Halder, Sujata; Nam, Hyun-Joo; Govindasamy, Lakshmanan; Vogel, Michèle; Dinsart, Christiane; Salomé, Nathalie; McKenna, Robert; Agbandje-McKenna, Mavis

    2012-01-01

    The production, purification, crystallization and crystallographic analysis of H-1 Parvovirus, a gene-therapy vector, are reported. Crystals of H-1 Parvovirus (H-1PV), an antitumor gene-delivery vector, were obtained for DNA-containing capsids and diffracted X-rays to 2.7 Å resolution using synchrotron radiation. The crystals belonged to the monoclinic space group P2 1 , with unit-cell parameters a = 255.4, b = 350.4, c = 271.6 Å, β = 90.34°. The unit cell contained two capsids, with one capsid per crystallographic asymmetric unit. The H-1PV structure has been determined by molecular replacement and is currently being refined

  12. Band structure and optical properties of diglycine nitrate crystal

    International Nuclear Information System (INIS)

    Andriyevsky, Bohdan; Ciepluch-Trojanek, Wioleta; Romanyuk, Mykola; Patryn, Aleksy; Jaskolski, Marcin

    2005-01-01

    Experimental and theoretical investigations of the electron energy characteristics and optical spectra for diglycine nitrate crystal (DGN) (NH 2 CH 2 COOH) 2 .HNO 3 , in the paraelectric phase (T=295K) are presented. Spectral dispersion of light reflection R(E) have been measured in the range of 3-22eV and the optical functions n(E) and k(E) have been calculated using Kramers-Kronig relations. First principal calculations of the electron energy characteristic and optical spectra of DGN crystal have been performed in the frame of density functional theory using CASTEP code (CAmbridge Serial Total Energy Package). Optical transitions forming the low-energy edge of fundamental absorption are associated with the nitrate groups NO 3 . Peculiarities of the band structure and DOS projected onto glycine and NO 3 groups confirm the molecular character of DGN crystal

  13. Growth and characterization of nonlinear optical single crystal: Nicotinic L-tartaric

    Energy Technology Data Exchange (ETDEWEB)

    Sheelarani, V.; Shanthi, J., E-mail: shanthinelson@gmail.com [Department of Physics, Avinashilingam Institute for Home Science and Higher Education for Women, Coimbatore-641043 (India)

    2015-06-24

    Nonlinear optical single crystals were grown from Nicotinic and L-Tartaric acid by slow evaporation technique at room temperature. Structure of the grown crystal was confirmed by single crystal X-ray diffraction studies, The crystallinity of the Nicotinic L-Tartaric (NLT) crystals was confirmed from the powder XRD pattern. The transparent range and cut off wavelength of the grown crystal was studied by the UV–Vis spectroscopic analysis.The thermal stability of the crystal was studied by TG-DTA. The second harmonic generation (SHG) efficiency of NLT was confirmed by Kurtz Perry technique.

  14. Synthesis, characterization and crystal structure of the new pentahydrate of bis(2,2'-bipyridine-κ(2)N,N')(oxalato-κ(2)O(1),O(2))nickel(II).

    Science.gov (United States)

    Farkašová, Nela; Cernák, Juraj; Tomás, Milagros; Falvello, Larry R

    2014-05-01

    The reaction of NiCl2, K2C2O4·H2O and 2,2'-bipyridine (bpy) in water-ethanol solution at 281 K yields light-purple needles of the new pentahydrate of bis(2,2'-bipyridine)oxalatonickel(II), [Ni(C2O4)(C10H8N2)2]·5H2O or [Ni(ox)(bpy)2]·5H2O, while at room temperature, deep-pink prisms of the previously reported tetrahydrate [Ni(ox)(bpy)2]·4H2O [Román, Luque, Guzmán-Miralles & Beitia (1995), Polyhedron, 14, 2863-2869] were gathered. The asymmetric unit in the crystal structure of the new pentahydrate incorporates the discrete molecular complex [Ni(ox)(bpy)2] and five solvent water molecules. Within the complex molecule, all three ligands are bonded as chelates. The complex molecules are involved in an extended system of hydrogen bonds with the solvent water molecules. Additionally, π-π interactions also contribute to the stabilization of the extended structure. The dehydration of the pentahydrate starts at 323 K and proceeds in at least two steps as determined by thermal analysis.

  15. First principles investigation of the structure of a bacteriochlorophyll crystal

    Energy Technology Data Exchange (ETDEWEB)

    Marchi, M. [Max-Planck-Institut fuer Festkoerperforschung, Stuttgart (Germany)]|[Centre d`Etudes Saclay, Gif-sur-Yvette (France); Hutter, J.; Parrinello, M. [Max-Planck-Institut fuer Festkoerperforschung, Stuttgart (Germany)

    1996-08-21

    In this communication we present an ab initio study of the crystal of methyl bacteriophorbide (MeBPheo) a, a bacteriochlorophyll derivative, and high-precision structure of which is available. Our main purpose has been to investigate the viability of the technique toward complex molecular systems relevant to biologically important phenomena, in this particular case photosynthesis. Here we present the following results: First, we show that DFT is capable of calculating nuclear positions in excellent agreement with the experimental X-ray structure. Second, the calculated electronic density of the HOMO orbital reveals a {pi} type bond between rings I and III, consistent with the one-dimensional chain structure of the MeBPheo a molecules in the crystal. Finally, after performing the optimization of the molecular geometry with one electron in the LUMO state, we find localized bond length changes near the ring II of the MeBPheo a. 19 refs., 3 figs.

  16. High-brightness tapered laser diodes with photonic crystal structures

    Science.gov (United States)

    Li, Yi; Du, Weichuan; Kun, Zhou; Gao, Songxin; Ma, Yi; Tang, Chun

    2018-02-01

    Beam quality of tapered laser diodes is limited by higher order lateral mode. On purpose of optimizing the brightness of tapered laser diodes, we developed a novel design of tapered diodes. This devices based on InGaAs/AlGaAs asymmetry epitaxial structure, containing higher order lateral mode filtering schemes especially photonic crystal structures, which fabricated cost effectively by using standard photolithography and dry etch processes. Meanwhile, the effects of photonic crystal structures on mode control are also investigated theoretically by FDBPM (Finite-Difference Beam Propagation Method) calculation. We achieved a CW optical output power of 6.9W at 940nm for a single emitter with 4 mm cavity length. A nearly diffraction limited beam of M2 ≍1.9 @ 0.5W has been demonstrated, and a highest brightness of β =75MW/(cm2 ·sr) was reached.

  17. Crystal structure and thermal behavior of KB3O6

    International Nuclear Information System (INIS)

    Bubnova, R.S.; Fundamenskij, V.S.; Filatov, S.K.; Polyakova, I.G.

    2004-01-01

    The structure of potassium triborate prepared in metastable state by crystallization from melt at ∼ 800 deg C was studied by the method of X-ray diffraction analysis. It was ascertained that KB 3 O 6 belongs to monoclinic crystal system, space group P2 1 /c, a = 9.319(1), b = 6.648(1), c = 21.094(2) A, β = 94.38(1) deg, Z = 12. The compound is referred to a new structural type. Anion of the structure is a single boron-oxygen frame formed by three independent rigid triborate rings of [B 3 O 5 ] - , each of them consisting of two BO 3 triangles and BO 4 tetrahedron. Phase transformations during KB 3 O 6 heating up to 800 deg C, as well as thermal expansion in the range of 20-650 deg C, were studied [ru

  18. Synthesis, spectral characterization and X-ray crystal structure studies of 3-(benzo[d][1,3]dioxol-5-yl)-5-(3-methylthiophen-2-yl)-4,5-dihydro-1H-pyrazole-1-carboxamide: Hirshfeld surface, DFT and thermal analysis

    Science.gov (United States)

    Kumara, Karthik; Dileep Kumar, A.; Naveen, S.; Ajay Kumar, K.; Lokanath, N. K.

    2018-06-01

    A novel pyrazole derivative, 3-(benzo[d][1,3]dioxol-5-yl)-5-(3-methylthiophen-2-yl)-4,5-dihydro-1H-pyrazole-1-carboxamide was synthesized and characterized by elemental analysis, FT-IR, NMR (1H and 13C), MS, UV-visible spectra and finally the structure was confirmed by the single crystal X-ray diffraction studies. The title compound (C16H15N3O3S) crystallized in the triclinic crystal system, with the space group Pī. A dihedral angle of 65.84(1)° between the pyrazole and the thiophene rings confirms the twisted conformation between them. The X-ray structure revealed that the pyrazole ring adopts an E-form and an envelope conformation on C7 atom. The crystal and molecular structure of the title compound is stabilized by inter molecular hydrogen bonds. The compound possesses three dimensional supramolecular self-assembly, in which Csbnd H⋯O and Nsbnd H⋯O chains build up two dimensional arrays, which are extended to 3D network through Csbnd H···Cg and Csbnd O···Cg interactions. The structure also exhibits intramolecular hydrogen bonds of the type Nsbnd H⋯N and π···π stacking interactions, which contributes to the crystal packing. Further, Hirshfeld surface analysis was carried out for the graphical visualization of several short intermolecular interactions on the molecular surface while the 2D finger-print plot provides percentage contribution of each individual atom-to-atom interactions. The thermal decomposition of the compound has been studied by thermogravimetric analysis. The molecular geometries and electronic structures of the compounds were fully optimized, calculated with ab-initio methods by HF, DFT/B3LYP functional in combination of different basis set with different solvent environment and the structural parameters were compared with the experimental data. The Mulliken atomic charges and molecular electrostatic potential on molecular van der Waals (vdW) surface were calculated to know the electrophilic and nucleophilic regions

  19. Non-isothermal crystallization kinetics and characterization of biodegradable poly(butylene succinate-co-neopentyl glycol succinate) copolyesters

    International Nuclear Information System (INIS)

    Xie, Wen-Jie; Zhou, Xiao-Ming

    2015-01-01

    Both biodegradable aliphatic neat poly(butylene succinate) (PBS) and poly(butylene succinate-co-neopentyl glycol succinate) (P(BS-co-NPGS)) copolyesters with different 1,4-butanediol/neopentyl glycol ratios were synthesized through a two-step process of transesterification and polycondensation using stannous chloride and 4-Methylbenzenesulfonic acid as the co-catalysts. The structure, non-isothermal crystallization behavior, crystalline morphology and crystal structure of neat PBS and P(BS-co-NPGS) copolyesters were characterized by 1 H NMR, differential scanning calorimetry (DSC), polarized optical microscope (POM) and wide angle X-ray diffraction (WAXD), respectively. The Avrami equation modified by Jeziorny and Mo's method was employed to describe the non-isothermal crystallization kinetics of the neat PBS and its copolyesters. The modified Avrami equation could adequately describe the primary stage of non-isothermal crystallization kinetics of the neat PBS and its copolyesters. Mo's method provided a fairly satisfactory description of the non-isothermal crystallization of neat PBS and its copolyesters. Interestingly, the values of 1/t 1/2 , Z c and F(T) obtained by the modified Avrami equation and Mo's method analysis indicated that the crystallization rate increased first and then decreased with an increase of NPGS content compared that of neat PBS, whereas the crystallization mechanism almost kept unchanged. The results of tensile testing showed that the ductility of PBS was largely improved by incorporating NPGS units. The elongation at break increased remarkably with increasing NPGS content. In particular, the sample with 20% NPGS content showed around 548% elongation at break. - Highlights: • The incorporation of NPGS units reduced the spherulite size of BS unit. • The existence of NPGS units did not change the crystal structure of BS unit. • The NPGS units incorporated in PBS could significantly improve the ductility of PBS. • The

  20. Structural and electrical characterization of zinc oxide doped with antimony

    Directory of Open Access Journals (Sweden)

    G. Juárez Díaz

    2014-08-01

    Full Text Available In this work we report the results of structural and electrical characterization realized on zinc oxide single crystal samples with (001 orientation, which were doped with antimony. Doping was carried out by antimony thermal diffusion at 1000 °C for periods of 1 and 2 hours under nitrogen environment from a solid source formed by antimony oxide. Electrical characterization by I-V curves and Hall effect shown an increase in acceptor concentration which demonstrates that doping is effective and create holes in zinc oxide samples.

  1. Molecular Complex of Lumiflavin and 2-Aminobenzoic Acid : Crystal Structure, Crystal Spectra, and Solution Properties

    OpenAIRE

    Shieh, Huey-Sheng; Ghisla, Sandro; Hanson, Louise Karle; Ludwig, Martha L.; Nordman, Christer E.

    1981-01-01

    The molecular complex lumiflavin-2-aminobenzoic acid monohydrate (C13H12N402●C7H7N02●H2O)crystallizes from aqueous solution as red triclinic prisms. The space group is P1 with cell dimensions a = 9.660 A, b = 14.866 Å, c = 7.045 Å, α = 95.44°, β = 95.86°, and γ = 105.66°. The crystal structure was solved by direct methods and refined by block-diagonal least-squares procedures to an R value of 0.050 on the basis of 1338 observed reflections. The structure is composed of stacks of alternating l...

  2. Crystal growth and characterization of REFeAsO (RE = La, Nd) and LaFePO

    Energy Technology Data Exchange (ETDEWEB)

    Adamski, Agnes; Abdel-Hafiez, Mahmoud; Krellner, Cornelius [Physikalisches Institut, Goethe Universitaet, D-60438 Frankfurt am Main (Germany)

    2016-07-01

    Since the discovery of iron-based superconductors, much effort was put on the crystal growth of the various systems and their characterization. Although, the initial flurry of activities was mainly performed on the 1111 systems, the focus has been rapidly shifted towards other materials, were large high-quality crystals are available. In contrast, the growth of sizeable high-quality single crystals of 1111 compounds is extremely challenging, slowing down the scientific progress in this type of compounds. Here we report on the crystal growth of 1111-type materials under ambient pressure conditions and by using the flux technique. The influence of the material to flux ratio was systematically studied. Subsequently, the obtained samples were analyzed with powder diffractometry, electron microscope, energy dispersive X-ray analysis, Laue diffractometry and magnetic measurements to analyze the structural and magnetic properties.

  3. Crystal growth and characterization of new semiorganic nonlinear optical single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Kulshrestha, Shobha, E-mail: shobha011986@gmail.com; Shrivastava, A. K., E-mail: ashwaniaks@rediffmail.com [School of Studies in Physics, Jiwaji University Gwalior (M.P.) – 474 011 (India)

    2016-05-06

    An organic material of a L-histidine monohydrochloride single crystal was grown in a distilled water solution using the slow evaporation method at 40–45°C. The grown crystal was transparent and colourless, with a size of about 20 × 9 × 5 mm{sup 3}, obtained within a period of 21 days. The solubility of grown crystals have found out at various temperatures. The UV-visible transmittance studies show that the grown crystals have wide optical transparency in the entire visible region It is observed that the crystal has transparency window from 255nm to 700nm and its energy gap (Eg) found to be is 3.1eV. The grown crystal was subjected to powder X-ray diffraction analysis, confirming that the orthorhombic crystalline nature of the crystal. To identify the surface morphology, the as grown crystal was subjected to FE-SEM technique. The chemical composition of the grown crystal was estimated by Energy dispersive X-ray analysis. The optical behaviour of the grown crystal was analyzed by PL study.

  4. Photonic guiding structures in lithium niobate crystals produced by energetic ion beams

    Science.gov (United States)

    Chen, Feng

    2009-10-01

    A range of ion beam techniques have been used to fabricate a variety of photonic guiding structures in the well-known lithium niobate (LiNbO3 or LN) crystals that are of great importance in integrated photonics/optics. This paper reviews the up-to-date research progress of ion-beam-processed LiNbO3 photonic structures and reports on their fabrication, characterization, and applications. Ion beams are being used with this material in a wide range of techniques, as exemplified by the following examples. Ion beam milling/etching can remove the selected surface regions of LiNbO3 crystals via the sputtering effects. Ion implantation and swift ion irradiation can form optical waveguide structures by modifying the surface refractive indices of the LiNbO3 wafers. Crystal ion slicing has been used to obtain bulk-quality LiNbO3 single-crystalline thin films or membranes by exfoliating the implanted layer from the original substrate. Focused ion beams can either generate small structures of micron or submicron dimensions, to realize photonic bandgap crystals in LiNbO3, or directly write surface waveguides or other guiding devices in the crystal. Ion beam-enhanced etching has been extensively applied for micro- or nanostructuring of LiNbO3 surfaces. Methods developed to fabricate a range of photonic guiding structures in LiNbO3 are introduced. Modifications of LiNbO3 through the use of various energetic ion beams, including changes in refractive index and properties related to the photonic guiding structures as well as to the materials (i.e., electro-optic, nonlinear optic, luminescent, and photorefractive features), are overviewed in detail. The application of these LiNbO3 photonic guiding structures in both micro- and nanophotonics are briefly summarized.

  5. Characterization of genetic structure of Podophyllum hexandrum ...

    African Journals Online (AJOL)

    Characterization of genetic structure of Podophyllum hexandrum populations, an endangered medicinal herb of Northwestern Himalaya, using ISSR-PCR markers and its relatedness with podophyllotoxin content.

  6. A hybrid computational-experimental approach for automated crystal structure solution

    Science.gov (United States)

    Meredig, Bryce; Wolverton, C.

    2013-02-01

    Crystal structure solution from diffraction experiments is one of the most fundamental tasks in materials science, chemistry, physics and geology. Unfortunately, numerous factors render this process labour intensive and error prone. Experimental conditions, such as high pressure or structural metastability, often complicate characterization. Furthermore, many materials of great modern interest, such as batteries and hydrogen storage media, contain light elements such as Li and H that only weakly scatter X-rays. Finally, structural refinements generally require significant human input and intuition, as they rely on good initial guesses for the target structure. To address these many challenges, we demonstrate a new hybrid approach, first-principles-assisted structure solution (FPASS), which combines experimental diffraction data, statistical symmetry information and first-principles-based algorithmic optimization to automatically solve crystal structures. We demonstrate the broad utility of FPASS to clarify four important crystal structure debates: the hydrogen storage candidates MgNH and NH3BH3; Li2O2, relevant to Li-air batteries; and high-pressure silane, SiH4.

  7. Crystal structure of human protein kinase CK2

    DEFF Research Database (Denmark)

    Niefind, K; Guerra, B; Ermakowa, I

    2001-01-01

    The crystal structure of a fully active form of human protein kinase CK2 (casein kinase 2) consisting of two C-terminally truncated catalytic and two regulatory subunits has been determined at 3.1 A resolution. In the CK2 complex the regulatory subunits form a stable dimer linking the two catalyt...... as a docking partner for various protein kinases. Furthermore it shows an inter-domain mobility in the catalytic subunit known to be functionally important in protein kinases and detected here for the first time directly within one crystal structure.......The crystal structure of a fully active form of human protein kinase CK2 (casein kinase 2) consisting of two C-terminally truncated catalytic and two regulatory subunits has been determined at 3.1 A resolution. In the CK2 complex the regulatory subunits form a stable dimer linking the two catalytic...... subunits, which make no direct contact with one another. Each catalytic subunit interacts with both regulatory chains, predominantly via an extended C-terminal tail of the regulatory subunit. The CK2 structure is consistent with its constitutive activity and with a flexible role of the regulatory subunit...

  8. Crystal structure optimisation using an auxiliary equation of state

    Science.gov (United States)

    Jackson, Adam J.; Skelton, Jonathan M.; Hendon, Christopher H.; Butler, Keith T.; Walsh, Aron

    2015-11-01

    Standard procedures for local crystal-structure optimisation involve numerous energy and force calculations. It is common to calculate an energy-volume curve, fitting an equation of state around the equilibrium cell volume. This is a computationally intensive process, in particular, for low-symmetry crystal structures where each isochoric optimisation involves energy minimisation over many degrees of freedom. Such procedures can be prohibitive for non-local exchange-correlation functionals or other "beyond" density functional theory electronic structure techniques, particularly where analytical gradients are not available. We present a simple approach for efficient optimisation of crystal structures based on a known equation of state. The equilibrium volume can be predicted from one single-point calculation and refined with successive calculations if required. The approach is validated for PbS, PbTe, ZnS, and ZnTe using nine density functionals and applied to the quaternary semiconductor Cu2ZnSnS4 and the magnetic metal-organic framework HKUST-1.

  9. Crystal structure optimisation using an auxiliary equation of state

    International Nuclear Information System (INIS)

    Jackson, Adam J.; Skelton, Jonathan M.; Hendon, Christopher H.; Butler, Keith T.; 3 Institute and Department of Materials Science and Engineering, Yonsei University, Seoul 120-749 (Korea, Republic of))" data-affiliation=" (Centre for Sustainable Chemical Technologies and Department of Chemistry, University of Bath, Claverton Down, Bath BA2 7AY (United Kingdom); Global E3 Institute and Department of Materials Science and Engineering, Yonsei University, Seoul 120-749 (Korea, Republic of))" >Walsh, Aron

    2015-01-01

    Standard procedures for local crystal-structure optimisation involve numerous energy and force calculations. It is common to calculate an energy–volume curve, fitting an equation of state around the equilibrium cell volume. This is a computationally intensive process, in particular, for low-symmetry crystal structures where each isochoric optimisation involves energy minimisation over many degrees of freedom. Such procedures can be prohibitive for non-local exchange-correlation functionals or other “beyond” density functional theory electronic structure techniques, particularly where analytical gradients are not available. We present a simple approach for efficient optimisation of crystal structures based on a known equation of state. The equilibrium volume can be predicted from one single-point calculation and refined with successive calculations if required. The approach is validated for PbS, PbTe, ZnS, and ZnTe using nine density functionals and applied to the quaternary semiconductor Cu 2 ZnSnS 4 and the magnetic metal-organic framework HKUST-1

  10. Crystal structure optimisation using an auxiliary equation of state

    Energy Technology Data Exchange (ETDEWEB)

    Jackson, Adam J.; Skelton, Jonathan M.; Hendon, Christopher H.; Butler, Keith T. [Centre for Sustainable Chemical Technologies and Department of Chemistry, University of Bath, Claverton Down, Bath BA2 7AY (United Kingdom); Walsh, Aron, E-mail: a.walsh@bath.ac.uk [Centre for Sustainable Chemical Technologies and Department of Chemistry, University of Bath, Claverton Down, Bath BA2 7AY (United Kingdom); Global E" 3 Institute and Department of Materials Science and Engineering, Yonsei University, Seoul 120-749 (Korea, Republic of)

    2015-11-14

    Standard procedures for local crystal-structure optimisation involve numerous energy and force calculations. It is common to calculate an energy–volume curve, fitting an equation of state around the equilibrium cell volume. This is a computationally intensive process, in particular, for low-symmetry crystal structures where each isochoric optimisation involves energy minimisation over many degrees of freedom. Such procedures can be prohibitive for non-local exchange-correlation functionals or other “beyond” density functional theory electronic structure techniques, particularly where analytical gradients are not available. We present a simple approach for efficient optimisation of crystal structures based on a known equation of state. The equilibrium volume can be predicted from one single-point calculation and refined with successive calculations if required. The approach is validated for PbS, PbTe, ZnS, and ZnTe using nine density functionals and applied to the quaternary semiconductor Cu{sub 2}ZnSnS{sub 4} and the magnetic metal-organic framework HKUST-1.

  11. Crystallization, characterization and preliminary X-ray crystallographic analysis of GK2848, a putative carbonic anhydrase of Geobacillus kaustophilus

    International Nuclear Information System (INIS)

    Ragunathan, Preethi; Raghunath, Gokul; Kuramitsu, Seiki; Yokoyama, Shigeyuki; Kumarevel, Thirumananseri; Ponnuraj, Karthe

    2013-01-01

    The expression, purification, characterization and crystallization of GK2848, a carbonic anhydrase from G. kaustophilus, are described. The crystals diffracted to a resolution of 2.70 Å. GK2848, a hypothetical protein from the thermophilic organism Geobacillus kaustophilus, was cloned and overexpressed in Escherichia coli. The protein was purified to homogeneity using Ni–NTA affinity-column and gel-filtration chromatography. The purified protein was crystallized using the sitting-drop vapour-diffusion method. The crystals diffracted to a resolution of 2.70 Å and belonged to the orthorhombic space group P2 1 2 1 2. GK2848 bears sequence homology to carbonic anhydrases of various bacterial species, indicating that it belongs to the carbonic anhydrase family of proteins. A subsequent carbonic anhydrase activity assay of GK2848 using the Wilbur–Anderson method confirmed its function as a carbonic anhydrase. A preliminary structure solution was obtained by molecular replacement using MOLREP. Mutation and biochemical characterization of the protein are in progress. The structure and functional analysis of GK2848 might provide valuable information on a novel class of carbonic anhydrases, as none of its homologous structures have been characterized

  12. Characterization of ion Coulomb crystals in a linear Paul trap

    International Nuclear Information System (INIS)

    Okada, K.; Takayanagi, T.; Wada, M.; Ohtani, S.; Schuessler, H. A.

    2010-01-01

    We describe a simple and fast method for simulating observed images of ion Coulomb crystals. In doing so, cold elastic collisions between Coulomb crystals and virtual very light atoms are implemented in a molecular dynamics (MD) simulation code. Such an approach reproduces the observed images of Coulomb crystals by obtaining density plots of the statistics of existence of each ion. The simple method has the advantage of short computing time in comparison with previous calculation methods. As a demonstration of the simulation, the formation of a planar Coulomb crystal with a small number of ions has been investigated in detail in a linear ion trap both experimentally and by simulation. However, also large Coulomb crystals including up to 1400 ions have been photographed and simulated to extract the secular temperature and the number of ions. For medium-sized crystals, a comparison between experiments and calculations has been performed. Moreover, an MD simulation of the sympathetic cooling of small molecular ions was performed in order to test the possibility of extracting the temperature and the number of refrigerated molecular ions from crystal images of laser-cooled ions. Such information is basic to studying ultracold ion-molecule reactions using ion Coulomb crystals including sympathetically cooled molecular ions.

  13. CRYSTAL AND MOLECULAR STRUCTURE OF 5-NITROPIRIDINE PIPERIDINE-SULFENAMIDE

    OpenAIRE

    Brito, Iván; León, Yasna; Arias, Mauricio; Vargas, Danitza; Carmona, Francisco; Ramírez, Eduardo; Restovic, Ambrosio; Cárdenas, Alejandro; Wittke, Oscar; López-Rodríguez, Matías

    2002-01-01

    The crystal and molecular structure of 5-nitropiridine piperidine-sulfenamide, C10H13N3O2 S is described and compared with other sulfenamides and with other similar compounds. This structure belongs to a type of divalent sulphur compound and crystallizes in the orthorhombic space group Pnma with a= 27.810(4), b=6.797(1), c=6.110(1)Å, and Dx =1.376 g cm-3 with Z=4. The S-N bond distance of 1.699(4) Å is shorter than a single S-N bond [1.74 Å]. The NO2-(C6H3N)-S-N(C 5H10) molecule lies on a cry...

  14. Parallelization for X-ray crystal structural analysis program

    Energy Technology Data Exchange (ETDEWEB)

    Watanabe, Hiroshi [Japan Atomic Energy Research Inst., Tokyo (Japan); Minami, Masayuki; Yamamoto, Akiji

    1997-10-01

    In this report we study vectorization and parallelization for X-ray crystal structural analysis program. The target machine is NEC SX-4 which is a distributed/shared memory type vector parallel supercomputer. X-ray crystal structural analysis is surveyed, and a new multi-dimensional discrete Fourier transform method is proposed. The new method is designed to have a very long vector length, so that it enables to obtain the 12.0 times higher performance result that the original code. Besides the above-mentioned vectorization, the parallelization by micro-task functions on SX-4 reaches 13.7 times acceleration in the part of multi-dimensional discrete Fourier transform with 14 CPUs, and 3.0 times acceleration in the whole program. Totally 35.9 times acceleration to the original 1CPU scalar version is achieved with vectorization and parallelization on SX-4. (author)

  15. Band structure and optical properties of opal photonic crystals

    Science.gov (United States)

    Pavarini, E.; Andreani, L. C.; Soci, C.; Galli, M.; Marabelli, F.; Comoretto, D.

    2005-07-01

    A theoretical approach for the interpretation of reflectance spectra of opal photonic crystals with fcc structure and (111) surface orientation is presented. It is based on the calculation of photonic bands and density of states corresponding to a specified angle of incidence in air. The results yield a clear distinction between diffraction in the direction of light propagation by (111) family planes (leading to the formation of a stop band) and diffraction in other directions by higher-order planes (corresponding to the excitation of photonic modes in the crystal). Reflectance measurements on artificial opals made of self-assembled polystyrene spheres are analyzed according to the theoretical scheme and give evidence of diffraction by higher-order crystalline planes in the photonic structure.

  16. An arc detector for neutron crystal structure investigations

    Energy Technology Data Exchange (ETDEWEB)

    Habib, N [Reactor and Neutron Physics Dept., Nuclear Research Center. AEA, Cairo (Egypt)

    1997-12-31

    An arc detector for neutron structure investigations of powder crystals using time-of-flight technique is described. In order to enable the measurement of integral intensity from about 1/4 of the Debye-Scherrer ring and for simplicity reasons, the scattering angle 20-90 degree was chosen and a special arc collimator was built. The arc collimator-detector had a divergency of about 20 minutes of arc, and the distance between detector-sample was 64 cm. Four {sup 3} He detectors were fixed on the arc of the collimator. Both efficiency and space sensitivity of the detector were determined using a point neutron source. Results of measurements show that parameters of the arc detector are acceptable for high resolution crystal structure investigations. 6 figs.

  17. Crystal structure of N′-hydroxypyrimidine-2-carboximidamide

    Directory of Open Access Journals (Sweden)

    Nithianantham Jeeva Jasmine

    2014-10-01

    Full Text Available The title compound, C5H6N4O, is approximately planar, with an angle of 11.04 (15° between the planes of the pyrimidine ring and the non-H atoms of the carboximidamide unit. The molecule adopts an E configuration about the C=N double bond. In the crystal, adjacent molecules are linked by pairs of N—H...O hydrogen bonds, forming inversion dimers with an R22(10 ring motif. The dimers are further linked via N—H...N and O—H...N hydrogen bonds into a sheet structure parallel to the ac plane. The crystal structure also features N—H...O and weak C—H...O hydrogen bonds and offset π–π stacking interactions between adjacent pyrimidine rings [centroid–centroid distance = 3.622 (1 Å].

  18. Four highly pseudosymmetric and/or twinned structures of d(CGCGCG) 2 extend the repertoire of crystal structures of Z-DNA

    Energy Technology Data Exchange (ETDEWEB)

    Luo, Zhipu; Dauter, Zbigniew; Gilski, Miroslaw

    2017-10-30

    DNA oligomer duplexes containing alternating cytosines and guanines in their sequences tend to form left-handed helices of the Z-DNA type, with the sugar and phosphate backbone in a zigzag conformation and a helical repeat of two successive nucleotides. Z-DNA duplexes usually crystallize as hexagonally arranged parallel helical tubes, with various relative orientations and translation of neighboring duplexes. Four novel high-resolution crystal structures of d(CGCGCG)2duplexes are described here. They are characterized by a high degree of pseudosymmetry and/or twinning, with three or four independent duplexes differently oriented in a monoclinicP21lattice of hexagonal metric. The various twinning criteria give somewhat conflicting indications in these complicated cases of crystal pathology. The details of molecular packing in these crystal structures are compared with other known crystal forms of Z-DNA.

  19. CCDC 1515632: Experimental Crystal Structure Determination : hexakis(dimethyl sulfoxide)-manganese(ii) tetraiodide

    KAUST Repository

    Haque, M.A.; Davaasuren, Bambar; Rothenberger, Alexander; Wu, Tao

    2016-01-01

    An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from

  20. CCDC 1475929: Experimental Crystal Structure Determination : trimethylammonium tribromo-tin(iv)

    KAUST Repository

    Dang, Yangyang; Zhong, Cheng; Zhang, Guodong; Ju, Dianxing; Wang, Lei; Xia, Shengqing; Xia, Haibing; Tao, Xutang

    2016-01-01

    An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from

  1. CCDC 1475930: Experimental Crystal Structure Determination : trimethylammonium trichloro-tin(iv)

    KAUST Repository

    Dang, Yangyang; Zhong, Cheng; Zhang, Guodong; Ju, Dianxing; Wang, Lei; Xia, Shengqing; Xia, Haibing; Tao, Xutang

    2016-01-01

    An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from

  2. CCDC 1475931: Experimental Crystal Structure Determination : trimethylammonium trichloro-tin(iv)

    KAUST Repository

    Dang, Yangyang; Zhong, Cheng; Zhang, Guodong; Ju, Dianxing; Wang, Lei; Xia, Shengqing; Xia, Haibing; Tao, Xutang

    2016-01-01

    An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from

  3. CCDC 1482638: Experimental Crystal Structure Determination : trimethylammonium trichloro-tin(iv)

    KAUST Repository

    Dang, Yangyang; Zhong, Cheng; Zhang, Guodong; Ju, Dianxing; Wang, Lei; Xia, Shengqing; Xia, Haibing; Tao, Xutang

    2016-01-01

    An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from

  4. Potassium and magnesium succinatouranilates – Synthesis and crystal structure

    Energy Technology Data Exchange (ETDEWEB)

    Novikov, S.A., E-mail: serg.alex.novikov@gmail.com [Samara National Research University, 443086 Samara (Russian Federation); Grigoriev, M.S. [Frumkin Institute of Physical Chemistry and Electrochemistry RAS, 119071 Moscow (Russian Federation); Serezhkina, L.B.; Serezhkin, V.N. [Samara National Research University, 443086 Samara (Russian Federation)

    2017-04-15

    Single crystal X-ray diffraction has been applied to determine the structures of two new uranyl coordination polymers: K{sub 2}[(UO{sub 2}){sub 2}(C{sub 4}H{sub 4}O{sub 4}){sub 3}] (1) and [Mg(H{sub 2}O){sub 6}] [(UO{sub 2}){sub 2}(C{sub 4}H{sub 4}O{sub 4}){sub 3}]·2H{sub 2}O (2), where C{sub 4}H{sub 4}O{sub 4}{sup 2-} is succinate anion. Crystals of 1 and 2 contain polymeric complex anions [(UO{sub 2}){sub 2}(C{sub 4}H{sub 4}O{sub 4}){sub 3}]{sup 2-} with the same A{sub 2}Q{sup 02}{sub 3} crystallochemical formula (A=UO{sub 2}{sup 2+}, Q{sup 02}=C{sub 4}O{sub 4}H{sub 4}{sup 2-}), and have layered (1) or chain (2) structure. It has been found, that conformation of succinate ions is one of the factors, which affects the structure of [(UO{sub 2}){sub 2}(C{sub 4}H{sub 4}O{sub 4}){sub 3}]{sup 2-} anions. IR spectra of these new compounds are in good agreement with crystallographic data. Topological analysis of the uranium dicarboxylates with A{sub 2}Q{sup 02}{sub 3} crystallochemical formula has shown the presence of five isomers which differ from each other in coordination sequences and / or dimensionality. - Graphical abstract: Crystal structures of two new uranium(VI) coordination polymers with succinate linkers, namely K{sub 2}[(UO{sub 2}){sub 2}(C{sub 4}H{sub 4}O{sub 4}){sub 3}] (1) and [Mg(H{sub 2}O){sub 6}][(UO{sub 2}){sub 2}(C{sub 4}H{sub 4}O{sub 4}){sub 3}]·2H{sub 2}O (2), were determined by single-crystal XRD. Crystals of studied compounds are based on 2D or 1D structural units with the same composition and crystallochemical formula. Topological isomerism in A{sub 2}Q{sup 02}{sub 3} crystallochemical group and conformations of succinate anions in uranyl complexes are under discussion. - Highlights: • Two new uranium coordination polymers were synthesized. • Their structural units have the same composition and crystallochemical formula. • In spite the same composition and CCF dimensionality of units is different. • Structural features of uranyl CPs

  5. Tuning optical properties of opal photonic crystals by structural defects engineering

    Science.gov (United States)

    di Stasio, F.; Cucini, M.; Berti, L.; Comoretto, D.; Abbotto, A.; Bellotto, L.; Manfredi, N.; Marinzi, C.

    2009-06-01

    We report on the preparation and optical characterization of three dimensional colloidal photonic crystal (PhC) containing an engineered planar defect embedding photoactive push-pull dyes. Free standing polystyrene films having thickness between 0.6 and 3 mm doped with different dipolar chromophores were prepared. These films were sandwiched between two artificial opals creating a PhC structure with planar defect. The system was characterized by reflectance at normal incidence angle (R), variable angle transmittance (T) and photoluminescence spectroscopy (PL) Evidence of defect states were observed in T and R spectra which allow the light to propagate for selected frequencies within the pseudogap (stop band).

  6. Crystal Structure of the Human Laminin Receptor Precursor

    Energy Technology Data Exchange (ETDEWEB)

    Jamieson,K.; Wu, J.; Hubbard, S.; Meruelo, D.

    2008-01-01

    The human laminin receptor (LamR) interacts with many ligands, including laminin, prions, Sindbis virus, and the polyphenol (-)-epigallocatechin-3-gallate (EGCG), and has been implicated in a number of diseases. LamR is overexpressed on tumor cells, and targeting LamR elicits anti-cancer effects. Here, we report the crystal structure of human LamR, which provides insights into its function and should facilitate the design of novel therapeutics targeting LamR.

  7. Incommensurate composite crystal structure of scandium-II

    International Nuclear Information System (INIS)

    Fujihisa, Hiroshi; Gotoh, Yoshito; Yamawaki, Hiroshi; Sakashita, Mami; Takeya, Satoshi; Honda, Kazumasa; Akahama, Yuichi; Kawamura, Haruki

    2005-01-01

    The long-unknown crystal structure of the high pressure phase scandium-II was solved by powder x-ray diffraction and was found to have tetragonal host channels along the c axis and guest chains that are incommensurate with the host, as well as the high pressure phases of Ba, Sr, Bi, and Sb. The pressure dependences of the lattice constants, the incommensurability, the atomic distances, and the atomic volume were investigated

  8. Band structure and optical properties of opal photonic crystals

    OpenAIRE

    Pavarini, E.; Andreani, L. C.; Soci, C.; Galli, M.; Marabelli, F.; Comoretto, D.

    2005-01-01

    A theoretical approach for the interpretation of reflectance spectra of opal photonic crystals with fcc structure and (111) surface orientation is presented. It is based on the calculation of photonic bands and density of states corresponding to a specified angle of incidence in air. The results yield a clear distinction between diffraction in the direction of light propagation by (111) family planes (leading to the formation of a stop band) and diffraction in other directions by higher-order...

  9. Crystal structures of unsymmetrically mixed β-pyrrole substituted ...

    Indian Academy of Sciences (India)

    NiTPP(Ph)3(CN)5, 3 complex was synthesized and its solvated structure was examined by crystallography. ... sive interactions among the peripheral substituents.28,29 ... 1H NMR spectra of porphyrins were. 1047 ... Single crystals of MTPP(Ph)3Cl5 (M = 2H and Ni(II)) .... by ∼0.3–0.6ppm but β-pyrrole phenyls do not show.

  10. Crystal structure of the sodium-potassium pump

    DEFF Research Database (Denmark)

    Morth, J Preben; Pedersen, Bjørn Panyella; Toustrup-Jensen, Mads S

    2007-01-01

    The Na+,K+-ATPase generates electrochemical gradients for sodium and potassium that are vital to animal cells, exchanging three sodium ions for two potassium ions across the plasma membrane during each cycle of ATP hydrolysis. Here we present the X-ray crystal structure at 3.5 A resolution......-subunit is contained within a pocket between transmembrane helices and seems to be a novel regulatory element controlling sodium affinity, possibly influenced by the membrane potential. Udgivelsesdato: 2007-Dec-13...

  11. Crystal structure studies on plate/shelf like disodium ditungstate

    Indian Academy of Sciences (India)

    Inorganic materials; disodium ditungstate; crystal structure; scanning electron microscopy; X-ray ... generation, and horizontal electric furnace with quartz tube ... Unit cell dimensions: a = 7·22192(11) Е, b = 11·91559(17) Е, c = 14·74755(23) Е. Cell content: 8 Na2W2O7). Atom. Position. X(σ(X)). Y(σ(Y)). Z(σ(Z)). B(σ(B)). W (1).

  12. Crystal structure of the uranyl-oxide mineral rameauite

    Czech Academy of Sciences Publication Activity Database

    Plášil, Jakub; Škoda, R.; Čejka, J.; Bourgoin, V.; Boulliard, J.C.

    2016-01-01

    Roč. 28, č. 5 (2016), s. 959-967 ISSN 0935-1221 R&D Projects: GA MŠk LO1603 EU Projects: European Commission(XE) CZ.2.16/3.1.00/24510 Institutional support: RVO:68378271 Keywords : rameauite * uranyl-oxide hydroxy-hydrate * crystal structure * Raman spectrum Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.362, year: 2016

  13. Growth and structural, optical, and electrical properties of zincite crystals

    Science.gov (United States)

    Kaurova, I. A.; Kuz'micheva, G. M.; Rybakov, V. B.

    2013-03-01

    An X-ray diffraction study of ZnO crystals grown by the hydrothermal method has revealed reflections that give grounds to assign them to the sp. gr. P3 rather than to P63 mc. The distribution of Zn1, Zn2, O1, and O2 over structural positions, along with vacancies and incorporated zinc atoms, explains the dissymmetrization observed in terms of the kinetic (growth) phase transition of the order-disorder type, which is caused by ordering Zn and O atoms over structural positions. The color of crystals of refined compositions (Zn0.975□0.025)Zn i(0.015)(O0.990□0.010) (green) and (Zn0.965□0.035)Zn i(0.035)O (bright green) is related to different oxygen contents, which is confirmed by the results of electron probe X-ray microanalysis and absorption spectroscopy. The degree of the structural quality of crystals, their resistivity, and activation energy are also related to oxygen vacancies.

  14. The Synthesis and Crystal Structure of Two New Hydrazone Compounds

    Directory of Open Access Journals (Sweden)

    Li-Hua Wang

    2016-05-01

    Full Text Available Two new hydrazone compounds, 4-formylimidazole-4-hydroxybenzhydrazone dihydrate (1 and 2-nitrobenzaldehyde-2-furan formylhydrazone (2, were synthesized via the classical synthesis method. Their structure was determined via elemental analysis and X-ray single crystal diffraction analysis. Compound 1 crystallizes in triclinic, space group P-1 with a = 7.0321(14 Å, b = 7.3723(15 Å, c = 13.008(3 Å, α = 98.66(3°, β = 101.69(3°, γ = 92.25(3°, V = 651.2(2 Å3, Z = 2, Dc = 1.358 g·cm−3, μ = 0.106 mm−1, F(000 = 280, and final R1 = 0.0564, wR2 = 0.1420. Compound 2 crystallizes in monoclinic, space group P21/c with a = 17.3618(9 Å, b = 9.1506(4 Å, c = 15.5801(7 Å, β = 104.532(5°, V = 2396.05(19 Å3, Z = 8, Dc = 1.437 g·cm−3, μ = 0.111 mm−1, F(000 = 1072, and final R1 = 0.0633, wR2 = 0.1649. Compound 1 forms a 2D-layered structure via the interactions of 1D chains and Compound 2 forms a 3D network structure via the interactions of 1D chains.

  15. Growth and characterization of magnesium chloride and lanthanum chloride doped strontium tartrate crystals - gel method

    International Nuclear Information System (INIS)

    Kalaiarasi, S.; Jaikumar, D.

    2014-01-01

    Growth of single crystals of doped strontium tartrate by controlled diffusion of strontium chloride into the silica gel charged with tartaric acid at room temperature is narrated. In this study, we synthesized magnesium chloride (5% and 10%) doped strontium tartrate crystals and Lanthanum chloride (5%, 10% and 15%) doped strontium tartrate crystals are grown. The crystal structure of the compound crystals was confirmed by single crystal X-ray diffraction. The Fourier transform infrared spectrum of pure and doped crystals are recorded and analyzed. The UV-Vis-NIR spectrum analysis reveals that the optical study of the grown crystals. The second harmonic generation efficiency was measured by using Kurtz powder technique with Nd:YAG laser of wavelength 1064 nm. (author)

  16. Programmatic conversion of crystal structures into 3D printable files using Jmol

    OpenAIRE

    Scalfani, Vincent F.; Williams, Antony J.; Tkachenko, Valery; Karapetyan, Karen; Pshenichnov, Alexey; Hanson, Robert M.; Liddie, Jahred M.; Bara, Jason E.

    2016-01-01

    Background Three-dimensional (3D) printed crystal structures are useful for chemistry teaching and research. Current manual methods of converting crystal structures into 3D printable files are time-consuming and tedious. To overcome this limitation, we developed a programmatic method that allows for facile conversion of thousands of crystal structures directly into 3D printable files. Results A collection of over 30,000 crystal structures in crystallographic information file (CIF) format from...

  17. Hydrogen bonded nonlinear optical γ-glycine: Crystal growth and characterization

    Science.gov (United States)

    Narayana Moolya, B.; Jayarama, A.; Sureshkumar, M. R.; Dharmaprakash, S. M.

    2005-07-01

    Single crystals of γ-glycine(GG) were grown by solvent evaporation technique from a mixture of aqueous solutions of glycine and ammonium nitrate at ambient temperature. X-ray diffraction, thermogravimetric/differential thermal analysis, Fourier transform infrared spectral techniques were employed to characterize the crystal. The lattice parameters were calculated and they agree well with the reported values. GG exists as dipolar ions in which the carboxyl group is present as a carboxylate ion and the amino group as an ammonium ion. Due to this dipolar nature, glycine has a high decomposition temperature. The UV cutoff of GG is below 300 nm and has a wide transparency window, which is suitable for second harmonic generation of laser in the blue region. Nonlinear optical characteristics of GG were studied using Q switched Nd:YAG laser ( λ=1064 nm). The second harmonic generation conversion efficiency of GG is 1.5 times that of potassium dihydrogen phosphate . The X-ray diffraction and Fourier transform infrared spectral studies show the presence of strong hydrogen bonds which create and stabilize the crystal structure in GG. The main contributions to the nonlinear optical properties in GG results from the presence of the hydrogen bond and from the vibrational part due to very intense infrared bands of the hydrogen bond vibrations. GG is thermally stable up to 441 K.

  18. Growth, structure, Hirshfeld surface and spectroscopic properties of 2-amino-4-hydroxy-6-methylpyrimidinium-2,3-pyrazinedicorboxylate single crystal

    Science.gov (United States)

    Faizan, Mohd; Alam, Mohammad Jane; Afroz, Ziya; Rodrigues, Vítor Hugo Nunes; Ahmad, Shabbir

    2018-03-01

    The present work is focused on the crystal structure, vibrational spectroscopy and DFT calculations of hydrogen bonded 2,3-pyrazinedicorboxylic acid and 2-amino-4-hydroxy-6-methylpyrimidine (PDCA-.AHMP+) crystal. The crystal structure has been determined using single crystal X-ray diffraction analysis which shows that the crystal belongs to monoclinic space group P21/n. The PDCA-.AHMP+ crystal has been characterized by FTIR, FT-Raman and FT-NMR spectroscopic techniques. The FTIR and FT-Raman spectra of the complex have unique spectroscopic feature as compared with those of the starting material to confirm salt formation. The theoretical vibrational studies have been performed to understand the modes of the vibrations of asymmetric unit of the complex by DFT methods. Hirschfeld surface and 2D fingerprint plots analyses were carried out to investigate the intermolecular interactions and its contribution in the building of PDCA-.AHMP+ crystal. The experimental and simulated 13C and 1H NMR studies have assisted in structural analysis of PDCA-.AHMP+ crystal. The electronic spectroscopic properties of the complex were explored by the experimental as well as theoretical electronic spectra simulated using TD-DFT/IEF-PCM method at B3LYP/6-311++G (d,p) level of theory. In addition, frontier molecular orbitals, molecular electrostatic potential map (MEP) and nonlinear optical (NLO) properties using DFT method have been also presented.

  19. Ab initio molecular crystal structures, spectra, and phase diagrams.

    Science.gov (United States)

    Hirata, So; Gilliard, Kandis; He, Xiao; Li, Jinjin; Sode, Olaseni

    2014-09-16

    Conspectus Molecular crystals are chemists' solids in the sense that their structures and properties can be understood in terms of those of the constituent molecules merely perturbed by a crystalline environment. They form a large and important class of solids including ices of atmospheric species, drugs, explosives, and even some organic optoelectronic materials and supramolecular assemblies. Recently, surprisingly simple yet extremely efficient, versatile, easily implemented, and systematically accurate electronic structure methods for molecular crystals have been developed. The methods, collectively referred to as the embedded-fragment scheme, divide a crystal into monomers and overlapping dimers and apply modern molecular electronic structure methods and software to these fragments of the crystal that are embedded in a self-consistently determined crystalline electrostatic field. They enable facile applications of accurate but otherwise prohibitively expensive ab initio molecular orbital theories such as Møller-Plesset perturbation and coupled-cluster theories to a broad range of properties of solids such as internal energies, enthalpies, structures, equation of state, phonon dispersion curves and density of states, infrared and Raman spectra (including band intensities and sometimes anharmonic effects), inelastic neutron scattering spectra, heat capacities, Gibbs energies, and phase diagrams, while accounting for many-body electrostatic (namely, induction or polarization) effects as well as two-body exchange and dispersion interactions from first principles. They can fundamentally alter the role of computing in the studies of molecular crystals in the same way ab initio molecular orbital theories have transformed research practices in gas-phase physical chemistry and synthetic chemistry in the last half century. In this Account, after a brief summary of formalisms and algorithms, we discuss applications of these methods performed in our group as compelling

  20. Monitoring and Characterization of Crystal Nucleation and Growth during Batch Crystallization

    NARCIS (Netherlands)

    Kadam, S.S.

    2012-01-01

    Batch crystallization is commonly used in pharmaceutical, agrochemical, specialty and fine chemicals industry. The advantages of batch crystallization lie in its ease of operation and the relatively simple equipment that can be used. On the other hand a major disadvantage associated with it is the

  1. Synthesis, crystal structure, Hirshfeld surfaces analysis and anti-ischemic activity of cinnamide derivatives

    Science.gov (United States)

    Zhong, Jian-gang; Han, Jia-pei; Li, Xiao-feng; Xu, Yi; Zhong, Yan; Wu, Bin

    2018-02-01

    Two cinnamide derivatives, namely, (E)-1-(4-(bis(4-methylphenyl)- methyl)piperazin-1-yl)-3-(3,4-diethoxyphenyl)prop-2-en-1-one (5) and (E)-1-(4-(bis- (4-fluorophenyl)methyl)piperazin-1-yl)-3-(4-methoxyphenyl)prop-2-en-1-one (6), have been synthesized and characterized by IR spectra, High resolution mass spectra, 1H NMR spectra, 13C NMR spectra. The compound 5 is a novel compound and has never been reported in the literature. Their crystal structures were studied by single-crystal X-ray diffraction. They all crystallize in the monoclinic system. The single-crystal X-ray revealed that compound 5 has infinite X-shaped 1-D polymeric chains structure and compound 6 has a layered 3-D structure by intermolecular interactions. Hirshfeld surface analysis demonstrated the presence of H⋯H, O⋯H, C⋯H, F⋯H, Csbnd H⋯π and π⋯π intermolecular interactions. In addition, the MTT assay results indicated that the compounds 5 and 6 display effective activities against neurotoxicity which is induced by glutamine in PC12 cells. The in vivo experiment indicated that the compound 6 has a good protective effect on cerebral infarction.

  2. Molecular complex of lumiflavin and 2-aminobenzoic acid: crystal structure, crystal spectra, and solution properties.

    Science.gov (United States)

    Shieh, H S; Ghisla, S; Hanson, L K; Ludwig, M L; Nordman, C E

    1981-08-04

    The molecular complex lumiflavin-2-aminobenzoic acid monohydrate (C13H12N4O2.C7H7NO2.H2O) crystallizes from from aqueous solution as red triclinic prisms. The space group is P1 with cell dimensions a = 9.660 A, b = 14.866 A, c = 7.045 A, alpha = 95.44 degrees , beta = 95.86 degrees, and gamma = 105.66 degrees . The crystal structure was solved by direct methods and refined by block-diagonal least-squares procedures to an R value of 0.050 on the basis of 1338 observed reflections. The structure is composed of stacks of alternating lumiflavin adn un-ionized (neutral) 2-aminobenzoic acid molecules. Two different modes of stacking interaction are observed. In one, 2-aminobenzoic acid overlaps all three of the isoalloxazine rings, at a mean distance of 3.36 A; in the other, 2-aminobenzoic acid interacts distance of 3.36 A; in the other, 2-aminobenzoic acid interacts with the pyrazine and dimethylbenzene moieties, at a distance of 3.42 A. Perpendicular to the stacking direction, the molecules form a continuous sheet. Each flavin is hydrogen bonded via O(2) and NH(3) to two symmetrically related aminobenzoates; the water of crystallization forms three hydrogen bonds, bridging two flavins, via O(4) and N(5), and one aminobenzoic acid. The red color of the crystals results from a charge-transfer transition involving stacked flavin and 2-aminobenzoic acid. The red color of the crystals results from a charge-transfer transition involving stacked flavin and 2-aminobenzoic acid molecules. Measurements of the polarized optical absorption spectra of crystals show that the transition moment direction for the long wavelength absorbance (beyond 530 nm) contains an out-of-plane component which can only arise from a charge-transfer interaction. Since the amino N does not make exceptionally close interactions with isoalloxazine atoms in either stacking mode (minimum interatomic distance 3.52 A), the charge transfer is presumed to involve pi orbitals of the 2-aminobenzoic acid donor.

  3. Revelation of endogenously bound Fe{sup 2+} ions in the crystal structure of ferritin from Escherichia coli

    Energy Technology Data Exchange (ETDEWEB)

    Thiruselvam, Viswanathan [Centre of Advanced Study in Crystallography and Biophysics, University of Madras, Guindy Campus, Chennai 600 025 (India); Sivaraman, Padavattan [RIKEN SPring-8 Center, Harima Institute, 1-1-1 Kouto, Sayo, Hyogo 679-5148 (Japan); Kumarevel, Thirumananseri, E-mail: kumarevel.thirumananseri@riken.jp [RIKEN SPring-8 Center, Harima Institute, 1-1-1 Kouto, Sayo, Hyogo 679-5148 (Japan); Structural Biology Laboratory, RIKEN Yokohama Institute, RIKEN, 1-7-22 Suehiro-cho, Tsurumi, Yokohama 230-0045 (Japan); Ponnuswamy, Mondikalipudur Nanjappagounder, E-mail: mnpsy2004@yahoo.com [Centre of Advanced Study in Crystallography and Biophysics, University of Madras, Guindy Campus, Chennai 600 025 (India)

    2014-10-24

    Highlights: • Crystal structure of ferritin was determined. • Endogenously expressed iron’s were identified. • Binuclear iron sites were observed at A and B active sites. - Abstract: Ferritin is an iron regulatory protein. It is responsible for storage and detoxification of excess iron thereby it regulates iron level in the body. Here we report the crystal structure of ferritin with two endogenously expressed Fe atoms binding in both the sites. The protein was purified and characterized by MALDI-TOF and N-terminal amino acid sequencing. The crystal belongs to I4 space group and it diffracted up to 2.5 Å. The structural analysis suggested that it crystallizes as hexamer and confirmed that it happened to be the first report of endogenously expressed Fe ions incorporated in both the A and B sites, situated in between the helices.

  4. Crystal structure of inactive form of Rab3B

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Wei [Hubei Key Laboratory of Genetic Regulation and Integrative Biology, College of Life Science, Huazhong Normal University, Wuhan 430079 (China); Shen, Yang [Structural Genomics Consortium, University of Toronto, 101 College St., Toronto, Ontario, Canada M5G 1L7 (Canada); Jiao, Ronghong [Department of Function Inspection, Hebei Provincial People' s Hospital, Shijiazhuang 050051 (China); Liu, Yanli; Deng, Lingfu [Hubei Key Laboratory of Genetic Regulation and Integrative Biology, College of Life Science, Huazhong Normal University, Wuhan 430079 (China); Qi, Chao, E-mail: qichao@mail.ccnu.edu.cn [Hubei Key Laboratory of Genetic Regulation and Integrative Biology, College of Life Science, Huazhong Normal University, Wuhan 430079 (China)

    2012-02-24

    Highlights: Black-Right-Pointing-Pointer This is the first structural information of human Rab3B. Black-Right-Pointing-Pointer To provides a structural basis for the GDP/GTP switch in controlling the activity of Rab3. Black-Right-Pointing-Pointer The charge distribution of Rab3B indicates its unique roles in vesicular trafficking. -- Abstract: Rab proteins are the largest family of ras-related GTPases in eukaryotic cells. They act as directional molecular switches at membrane trafficking, including vesicle budding, cargo sorting, transport, tethering, and fusion. Here, we generated and crystallized the Rab3B:GDP complex. The structure of the complex was solved to 1.9 A resolution and the structural base comparison with other Rab3 members provides a structural basis for the GDP/GTP switch in controlling the activity of small GTPase. The comparison of charge distribution among the members of Rab3 also indicates their different roles in vesicular trafficking.

  5. Crystal structure of inactive form of Rab3B

    International Nuclear Information System (INIS)

    Zhang, Wei; Shen, Yang; Jiao, Ronghong; Liu, Yanli; Deng, Lingfu; Qi, Chao

    2012-01-01

    Highlights: ► This is the first structural information of human Rab3B. ► To provides a structural basis for the GDP/GTP switch in controlling the activity of Rab3. ► The charge distribution of Rab3B indicates its unique roles in vesicular trafficking. -- Abstract: Rab proteins are the largest family of ras-related GTPases in eukaryotic cells. They act as directional molecular switches at membrane trafficking, including vesicle budding, cargo sorting, transport, tethering, and fusion. Here, we generated and crystallized the Rab3B:GDP complex. The structure of the complex was solved to 1.9 Å resolution and the structural base comparison with other Rab3 members provides a structural basis for the GDP/GTP switch in controlling the activity of small GTPase. The comparison of charge distribution among the members of Rab3 also indicates their different roles in vesicular trafficking.

  6. Synthesis of a mixed-valent tin nitride and considerations of its possible crystal structures

    International Nuclear Information System (INIS)

    Caskey, Christopher M.; Holder, Aaron; Christensen, Steven T.; Biagioni, David; Ginley, David S.; Tumas, William; Perkins, John D.; Lany, Stephan; Zakutayev, Andriy; Shulda, Sarah; Diercks, David; Pylypenko, Svitlana; Richards, Ryan M.; Schwartz, Craig P.; Nordlund, Dennis; Kukliansky, Alon; Natan, Amir; Prendergast, David; Sun, Wenhao; Orvananos, Bernardo

    2016-01-01

    Recent advances in theoretical structure prediction methods and high-throughput computational techniques are revolutionizing experimental discovery of the thermodynamically stable inorganic materials. Metastable materials represent a new frontier for these studies, since even simple binary non-ground state compounds of common elements may be awaiting discovery. However, there are significant research challenges related to non-equilibrium thin film synthesis and crystal structure predictions, such as small strained crystals in the experimental samples and energy minimization based theoretical algorithms. Here, we report on experimental synthesis and characterization, as well as theoretical first-principles calculations of a previously unreported mixed-valent binary tin nitride. Thin film experiments indicate that this novel material is N-deficient SnN with tin in the mixed II/IV valence state and a small low-symmetry unit cell. Theoretical calculations suggest that the most likely crystal structure has the space group 2 (SG2) related to the distorted delafossite (SG166), which is nearly 0.1 eV/atom above the ground state SnN polymorph. This observation is rationalized by the structural similarity of the SnN distorted delafossite to the chemically related Sn 3 N 4 spinel compound, which provides a fresh scientific insight into the reasons for growth of polymorphs of metastable materials. In addition to reporting on the discovery of the simple binary SnN compound, this paper illustrates a possible way of combining a wide range of advanced characterization techniques with the first-principle property calculation methods, to elucidate the most likely crystal structure of the previously unreported metastable materials.

  7. Synthesis of a mixed-valent tin nitride and considerations of its possible crystal structures

    Energy Technology Data Exchange (ETDEWEB)

    Caskey, Christopher M. [National Renewable Energy Laboratory, Golden, Colorado 80401 (United States); Colorado School of Mines, Golden, Colorado 80401 (United States); Larix Chemical Science, Golden, Colorado 80401 (United States); Holder, Aaron; Christensen, Steven T.; Biagioni, David; Ginley, David S.; Tumas, William; Perkins, John D.; Lany, Stephan; Zakutayev, Andriy, E-mail: andriy.zakutayev@nrel.gov [National Renewable Energy Laboratory, Golden, Colorado 80401 (United States); Shulda, Sarah; Diercks, David; Pylypenko, Svitlana; Richards, Ryan M. [Colorado School of Mines, Golden, Colorado 80401 (United States); Schwartz, Craig P.; Nordlund, Dennis [SLAC National Accelerator Laboratory, Menlo Park, California 94025 (United States); Kukliansky, Alon; Natan, Amir [Tel Aviv University, Tel Aviv-Yafo (Israel); Prendergast, David; Sun, Wenhao [Lawrence Berkeley National Laboratory, Berkley, California 94720 (United States); Orvananos, Bernardo [Massachusetts Institute of Technology, Cambridge, Massachusetts 02139 (United States); and others

    2016-04-14

    Recent advances in theoretical structure prediction methods and high-throughput computational techniques are revolutionizing experimental discovery of the thermodynamically stable inorganic materials. Metastable materials represent a new frontier for these studies, since even simple binary non-ground state compounds of common elements may be awaiting discovery. However, there are significant research challenges related to non-equilibrium thin film synthesis and crystal structure predictions, such as small strained crystals in the experimental samples and energy minimization based theoretical algorithms. Here, we report on experimental synthesis and characterization, as well as theoretical first-principles calculations of a previously unreported mixed-valent binary tin nitride. Thin film experiments indicate that this novel material is N-deficient SnN with tin in the mixed II/IV valence state and a small low-symmetry unit cell. Theoretical calculations suggest that the most likely crystal structure has the space group 2 (SG2) related to the distorted delafossite (SG166), which is nearly 0.1 eV/atom above the ground state SnN polymorph. This observation is rationalized by the structural similarity of the SnN distorted delafossite to the chemically related Sn{sub 3}N{sub 4} spinel compound, which provides a fresh scientific insight into the reasons for growth of polymorphs of metastable materials. In addition to reporting on the discovery of the simple binary SnN compound, this paper illustrates a possible way of combining a wide range of advanced characterization techniques with the first-principle property calculation methods, to elucidate the most likely crystal structure of the previously unreported metastable materials.

  8. Crystal Structure of the Yeast Nicotinamidase Pnc1p

    OpenAIRE

    Hu, Gang; Taylor, Alexander B.; McAlister-Henn, Lee; Hart, P. John

    2007-01-01

    The yeast nicotinamidase Pnc1p acts in transcriptional silencing by reducing levels of nicotinamide, an inhibitor of the histone deacetylase Sir2p. The Pnc1p structure was determined at 2.9 Å resolution using MAD and MIRAS phasing methods after inadvertent crystallization during the pursuit of the structure of histidine-tagged yeast isocitrate dehydrogenase (IDH). Pnc1p displays a cluster of surface histidine residues likely responsible for its co-fractionation with IDH from Ni2+-coupled chro...

  9. Band structures in the nematic elastomers phononic crystals

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Shuai [Department of Mechanics, School of Civil Engineering, Beijing Jiaotong University, Beijing 100044 (China); School of Civil Engineering and Architecture, Anyang Normal University, Anyang 455000 (China); Liu, Ying, E-mail: yliu5@bjtu.edu.cn [Department of Mechanics, School of Civil Engineering, Beijing Jiaotong University, Beijing 100044 (China); Liang, Tianshu [Department of Mechanics, School of Civil Engineering, Beijing Jiaotong University, Beijing 100044 (China)

    2017-02-01

    As one kind of new intelligent materials, nematic elastomers (NEs) represent an exciting physical system that combines the local orientational symmetry breaking and the entropic rubber elasticity, producing a number of unique physical phenomena. In this paper, the potential application of NEs in the band tuning is explored. The band structures in two kinds of NE phononic crystals (PCs) are investigated. Through changing NE intrinsic parameters, the influence of the porosity, director rotation and relaxation on the band structures in NE PCs are analyzed. This work is a meaningful try for application of NEs in acoustic field and proposes a new intelligent strategy in band turning.

  10. Band structures in the nematic elastomers phononic crystals

    International Nuclear Information System (INIS)

    Yang, Shuai; Liu, Ying; Liang, Tianshu

    2017-01-01

    As one kind of new intelligent materials, nematic elastomers (NEs) represent an exciting physical system that combines the local orientational symmetry breaking and the entropic rubber elasticity, producing a number of unique physical phenomena. In this paper, the potential application of NEs in the band tuning is explored. The band structures in two kinds of NE phononic crystals (PCs) are investigated. Through changing NE intrinsic parameters, the influence of the porosity, director rotation and relaxation on the band structures in NE PCs are analyzed. This work is a meaningful try for application of NEs in acoustic field and proposes a new intelligent strategy in band turning.

  11. Fabrication and Characterization of Three Dimensional Photonic Crystals Generated by Multibeam Interference Lithography

    Science.gov (United States)

    Chen, Ying-Chieh

    2009-01-01

    Multibeam interference lithography is investigated as a manufacturing technique for three-dimensional photonic crystal templates. In this research, optimization of the optical setup and the photoresist initiation system leads to a significant improvement of the optical quality of the crystal, as characterized by normal incidence optical…

  12. Synthesis and characterization of hydroxyapatite crystals: a review study on the analytical methods

    NARCIS (Netherlands)

    Koutsopoulos, S.

    2002-01-01

    For the synthesis of hydroxyapatite crystals from aqueous solutions three preparation methods were employed. From the experimental processes and the characterization of the crystals it was concluded that aging and precipitation kinetics are critical for the purity of the product and its

  13. Synthesis and Single Crystal X-Ray Structure Determination of 3,3',5 ...

    African Journals Online (AJOL)

    Single crystal structure determination at 100 K revealed needle-like crystals in an orthorhombic crystal system. The asymmetric unit of the cell consists of an isolated chloride ion, one half of a tetrahedral [MnCl4]2- anion, a [H2Me4bpz]2+ dication and one half of a molecule of water. Keywords: Crystal Engineering, Hydrogen ...

  14. Influence of crystallization time on structural and morphological characteristics the precursor of zeolite MCM-22

    International Nuclear Information System (INIS)

    Barbosa, A.S.; Lima, L.A.; Sousa, B.V.; Santos, Everton R.F. dos; Rodrigues, M.G.F.

    2009-01-01

    The zeolite MCM-22 has been studied extensively as a promising catalyst because of the high thermal stability and high activity for acid catalysis and selectivity of molecular shape. The synthesis of MCM-22 is carried out by hydrothermal treatment and long times required for complete crystallization gradual growth of crystals of 10-14 days for the synthesis of static. This work aims to synthesize the precursor of zeolite MCM-22 using the method of hydrothermal synthesis with a reduction in crystallization time of 8 and 9 days. The precursor of zeolite MCM-22 was obtained using sources of silica, soda, deionized water and the director of structures hexametilenoimina (HMI). The samples were synthesized at 150° C for 8 to 9 days, with the following molar composition: 0.511 SiO 2 : 0.039 NaOH: 0.024 Al 2 O 3 : 23.06 H 2 O and subjected to characterizations by X-ray diffraction (XRD), scanning electron microscopy ( SEM) and energy dispersive (EDX). According to tests carried out showed that the hydrothermal treatment used to synthesize the precursor of zeolite MCM-22 was effective during times of crystallization of 8 and 9 days. The results for the micrographs showed that the samples consist of clusters and / or aggregates of small crystals. (author)

  15. Cloning and characterization of an insecticidal crystal protein gene ...

    Indian Academy of Sciences (India)

    Unknown

    The sequence of the cloned crystal protein gene showed almost complete homology with a mosquitocidal toxin gene from Bacillus .... diet or by topical application on food substrates as .... has very high similarity (99.74%) at DNA level with.

  16. Natural Cr3+-rich ettringite: occurrence, properties, and crystal structure

    Science.gov (United States)

    Seryotkin, Yurii V.; Sokol, Ella V.; Kokh, Svetlana N.; Murashko, Mikhail N.

    2017-08-01

    Cr3+-rich ettringite with Cr3+→Al substitution and Cr/(Cr + Al) ratios up to 0.40-0.50 was found in mineral assemblages of the Ma'aleh Adumim area of Mottled Zone (Judean Desert). The Cr3+-rich compositions were the latest in the thaumasite → ettringite-thaumasite solid solution → ettringite → ettringite-bentorite solid solution series. The mineral-forming solution was enriched in Cr3+ and had a pH buffered by afwillite at 11-12. Chromium was inherited from larnite rocks produced by high-temperature combustion metamorphic alteration of bioproductive calcareous sediments. The Cr/(Cr + Al) ratios are within 0.10-0.15 in most of the analysed crystals. This degree of substitution imparts pink colouration to the crystals, but does not affect their habit (a combination of monohedra and a prism). The habit changes to pyramid faces in coarse and later Cr3+-bearing crystals as Cr/(Cr + Al) ratios increase abruptly to 0.40-0.50. Single-crystal XRD analysis of one Cr-free and two Cr3+-rich samples and their structure determination and refinement indicate that the Cr-rich crystals (with Cr/(Cr + Al) to 0.3) preserve the symmetry and metrics of ettringite. The Ca-O bonding network undergoes differentiation with increase of Cr3+ concentration at octahedral M sites. The compression of Ca2 and expansion of Ca1 polyhedra sub-networks correlates with the degree of Cr3+→Al substitution.

  17. Crystal structures of two eukaryotic nucleases involved in RNA metabolism

    DEFF Research Database (Denmark)

    Jonstrup, Anette Thyssen; Midtgaard, Søren Fuglsang; Van, Lan Bich

    RNA serves a number of functions in the cell: mRNAs are the carriers of information between gene and protein, tRNAs and rRNAs are involved in the synthesis of proteins, whereas a number of additional RNA species are responsible for other functions in the cell. The quality of the different RNAs...... RNAs. We have solved the structures of two nucleases involved in 3'-5' degradation of RNA; the S. pombe Pop2p and the S. cerevisiae Rrp6p. Pop2p is part of the main cytoplasmatic deadenylation complex in yeast, which also contains the nuclease Ccr4p. Deadenylation, where the poly(A)-tail is removed...... specific transcripts. Here, we present the crystal structure of the S. pombe Pop2p protein to 1.4 Å resolution. The high resolution structure provides a clear picture of the active site architecture. Structural alignment of single nucleotides and poly(A)-oligonucleotides from earlier co-crystal structures...

  18. The crystal structure of human GDP-L-fucose synthase.

    Science.gov (United States)

    Zhou, Huan; Sun, Lihua; Li, Jian; Xu, Chunyan; Yu, Feng; Liu, Yahui; Ji, Chaoneng; He, Jianhua

    2013-09-01

    Human GDP-l-fucose synthase, also known as FX protein, synthesizes GDP-l-fucose from its substrate GDP-4-keto-6-deoxy-d-mannose. The reaction involves epimerization at both C-3 and C-5 followed by an NADPH-dependent reduction of the carbonyl at C-4. In this paper, the first crystal structure of human FX protein was determined at 2.37 Å resolution. The asymmetric unit of the crystal structure contains four molecules which form two homodimers. Each molecule consists of two domains, a Rossmann-fold NADPH-binding motif and a carboxyl terminal domain. Compared with the Escherichia coli GDP-l-fucose synthase, the overall structures of these two enzymes have four major differences. There are four loops in the structure of human FX protein corresponding to two α-helices and two β-sheets in that of the E. coli enzyme. Besides, there are seven different amino acid residues binding with NAPDH comparing human FX protein with that from E. coli. The structure of human FX reveals the key catalytic residues and could be useful for the design of drugs for the treatment of inflammation, auto-immune diseases, and possibly certain types of cancer.

  19. Magnetic activity at infrared frequencies in structured metallic photonic crystals

    International Nuclear Information System (INIS)

    O'Brien, S.; Pendry, J.P.

    2002-01-01

    We derive the effective permeability and permittivity of a nanostructured metallic photonic crystal by analysing the complex reflection and transmission coefficients for slabs of various thicknesses. These quantities were calculated using the transfer matrix method. Our results indicate that these structures could be used to realize a negative effective permeability, at least up to infrared frequencies. The origin of the negative permeability is a resonance due to the internal inductance and capacitance of the structure. We also present an analytic model for the effective permeability of the crystal. The model reveals the importance of the inertial inductance due to the finite mass of the electrons in the metal. We find that this contribution to the inductance has implications for the design of metallic magnetic structures in the optical region of the spectrum. We show that the magnetic activity in the structure is accompanied by the concentration of the incident field energy into very small volumes within the structure. This property will allow us to considerably enhance non-linear effects with minute quantities of material. (author)

  20. Relation between photochromic properties and molecular structures in salicylideneaniline crystals.

    Science.gov (United States)

    Johmoto, Kohei; Ishida, Takashi; Sekine, Akiko; Uekusa, Hidehiro; Ohashi, Yuji

    2012-06-01

    The crystal structures of the salicylideneaniline derivatives N-salicylidene-4-tert-butyl-aniline (1), N-3,5-di-tert-butyl-salicylidene-3-methoxyaniline (2), N-3,5-di-tert-butyl-salicylidene-3-bromoaniline (3), N-3,5-di-tert-butyl-salicylidene-3-chloroaniline (4), N-3,5-di-tert-butyl-salicylidene-4-bromoaniline (5), N-3,5-di-tert-butyl-salicylidene-aniline (6), N-3,5-di-tert-butyl-salicylidene-4-carboxyaniline (7) and N-salicylidene-2-chloroaniline (8) were analyzed by X-ray diffraction analysis at ambient temperature to investigate the relationship between their photochromic properties and molecular structures. A clear correlation between photochromism and the dihedral angle of the two benzene rings in the salicylideneaniline derivatives was observed. Crystals with dihedral angles less than 20° were non-photochromic, whereas those with dihedral angles greater than 30° were photochromic. Crystals with dihedral angles between 20 and 30° could be either photochromic or non-photochromic. Inhibition of the pedal motion by intra- or intermolecular steric hindrance, however, can result in non-photochromic behaviour even if the dihedral angle is larger than 30°.

  1. Molecular and crystal structure of 2-((E)-[(4-Methylphenyl)imino]methyl)-4-nitrophenol: A redetermination

    International Nuclear Information System (INIS)

    Kaynar, Nihal Kan; Tanak, Hasan; Şahin, Songul; Dege, Necmi; Ağar, Erbil; Yavuz, Metin

    2016-01-01

    The crystal structure of the title compound, C_1_4H_1_2N_2O_3, was recently determined as a mixture of its neutral (OH containing) and zwitterionic (NH containing) forms, in a 0.60 (4): 0.40 (4) ratio using the X-ray determination. In this study, the title compound has been characterized by FT-IR and X-ray diffraction. The redetermination showed that the title compound has only enol (OH) form because of lack of the NH stretching vibration in FT-IR spectrum. In addition, the molecular structure and tautomerism of the title compound have been discussed.

  2. Molecular and crystal structure of 2-((E)-[(4-Methylphenyl)imino]methyl)-4-nitrophenol: A redetermination

    Energy Technology Data Exchange (ETDEWEB)

    Kaynar, Nihal Kan, E-mail: nihal-kan84@windowslive.com [Ondokuz Mayıs University, Department of Physics, Faculty of Arts and Sciences (Turkey); Tanak, Hasan [Amasya University, Department of Physics, Faculty of Arts and Sciences (Turkey); Şahin, Songul [Ondokuz Mayıs University, Department of Chemistry, Faculty of Arts and Sciences (Turkey); Dege, Necmi [Ondokuz Mayıs University, Department of Physics, Faculty of Arts and Sciences (Turkey); Ağar, Erbil [Ondokuz Mayıs University, Department of Chemistry, Faculty of Arts and Sciences (Turkey); Yavuz, Metin [Ondokuz Mayıs University, Department of Physics, Faculty of Arts and Sciences (Turkey)

    2016-03-15

    The crystal structure of the title compound, C{sub 14}H{sub 12}N{sub 2}O{sub 3}, was recently determined as a mixture of its neutral (OH containing) and zwitterionic (NH containing) forms, in a 0.60 (4): 0.40 (4) ratio using the X-ray determination. In this study, the title compound has been characterized by FT-IR and X-ray diffraction. The redetermination showed that the title compound has only enol (OH) form because of lack of the NH stretching vibration in FT-IR spectrum. In addition, the molecular structure and tautomerism of the title compound have been discussed.

  3. Crystal structure of bile salt hydrolase from Lactobacillus salivarius.

    Science.gov (United States)

    Xu, Fuzhou; Guo, Fangfang; Hu, Xiao Jian; Lin, Jun

    2016-05-01

    Bile salt hydrolase (BSH) is a gut-bacterial enzyme that negatively influences host fat digestion and energy harvesting. The BSH enzyme activity functions as a gateway reaction in the small intestine by the deconjugation of glycine-conjugated or taurine-conjugated bile acids. Extensive gut-microbiota studies have suggested that BSH is a key mechanistic microbiome target for the development of novel non-antibiotic food additives to improve animal feed production and for the design of new measures to control obesity in humans. However, research on BSH is still in its infancy, particularly in terms of the structural basis of BSH function, which has hampered the development of BSH-based strategies for improving human and animal health. As an initial step towards the structure-function analysis of BSH, C-terminally His-tagged BSH from Lactobacillus salivarius NRRL B-30514 was crystallized in this study. The 1.90 Å resolution crystal structure of L. salivarius BSH was determined by molecular replacement using the structure of Clostridium perfringens BSH as a starting model. It revealed this BSH to be a member of the N-terminal nucleophile hydrolase superfamily. Crystals of apo BSH belonged to space group P21212, with unit-cell parameters a = 90.79, b = 87.35, c = 86.76 Å (PDB entry 5hke). Two BSH molecules packed perfectly as a dimer in one asymmetric unit. Comparative structural analysis of L. salivarius BSH also identified potential residues that contribute to catalysis and substrate specificity.

  4. Crystal growth and characterization of a semiorganic nonlinear optical single crystal of gamma glycine

    International Nuclear Information System (INIS)

    Prakash, J. Thomas Joseph; Kumararaman, S.

    2008-01-01

    Gamma glycine has been successfully synthesized by taking glycine and potassium chloride and single crystals have been grown by solvent evaporation method for the first time. The grown single crystals have been analyzed with XRD, Fourier transform infrared (FTIR), and thermo gravimetric and differential thermal analyses (TG/DTA) measurements. Its mechanical behavior has been assessed by Vickers microhardness measurements. Its nonlinear optical property has been tested by Kurtz powder technique. Its optical behavior was examined by UV-vis., and found that the crystal is transparent in the region between 240 and 1200 nm. Hence, it may be very much useful for the second harmonic generation (SHG) applications

  5. Path-integral and Ornstein-Zernike study of quantum fluid structures on the crystallization line

    International Nuclear Information System (INIS)

    Sesé, Luis M.

    2016-01-01

    Liquid neon, liquid para-hydrogen, and the quantum hard-sphere fluid are studied with path integral Monte Carlo simulations and the Ornstein-Zernike pair equation on their respective crystallization lines. The results cover the whole sets of structures in the r-space and the k-space and, for completeness, the internal energies, pressures and isothermal compressibilities. Comparison with experiment is made wherever possible, and the possibilities of establishing k-space criteria for quantum crystallization based on the path-integral centroids are discussed. In this regard, the results show that the centroid structure factor contains two significant parameters related to its main peak features (amplitude and shape) that can be useful to characterize freezing.

  6. Path-integral and Ornstein-Zernike study of quantum fluid structures on the crystallization line

    Energy Technology Data Exchange (ETDEWEB)

    Sesé, Luis M., E-mail: msese@ccia.uned.es [Departamento de Ciencias y Técnicas Fisicoquímicas, Universidad Nacional de Educación a Distancia, Paseo Senda del Rey 9, 28040 Madrid (Spain)

    2016-03-07

    Liquid neon, liquid para-hydrogen, and the quantum hard-sphere fluid are studied with path integral Monte Carlo simulations and the Ornstein-Zernike pair equation on their respective crystallization lines. The results cover the whole sets of structures in the r-space and the k-space and, for completeness, the internal energies, pressures and isothermal compressibilities. Comparison with experiment is made wherever possible, and the possibilities of establishing k-space criteria for quantum crystallization based on the path-integral centroids are discussed. In this regard, the results show that the centroid structure factor contains two significant parameters related to its main peak features (amplitude and shape) that can be useful to characterize freezing.

  7. Crystal structures and conformers of CyMe4-BTBP

    Directory of Open Access Journals (Sweden)

    Lyczko Krzysztof

    2015-12-01

    Full Text Available The crystal structure of new conformation of the CyMe4-BTBP ligand (ttc has been presented. The ttt conformer of this compound in a form of THF solvate has been also crystallized. The geometries of six possible conformations (ttt, ttc, tct, tcc, ctc and ccc of the CyMe4-BTBP ligand have been modeled in the gas phase and in solutions (MeOH and H2O by DFT calculations using B3LYP/6-31G(d,p method. According to the calculations, in the three different media the conformers with trans orientation of the N atoms in the bipyridyl moiety are the most stable.

  8. Crystal structure of dichloridobis(dimethyl N-cyanodithioiminocarbonatecobalt(II

    Directory of Open Access Journals (Sweden)

    Mouhamadou Birame Diop

    2016-01-01

    Full Text Available The structure of the mononuclear title complex, [{(H3CS2C=NC[triple-bond] N}2CoCl2], consists of a CoII atom coordinated in a distorted tetrahedral manner by two Cl− ligands and the terminal N atoms of two dimethyl N-cyanodithioiminocarbonate ligands. The two organic ligands are almost coplanar, with a dihedral angle of 5.99 (6° between their least-squares planes. The crystal packing features pairs of inversion-related complexes that are held together through C—H...Cl and C—H...S interactions and π–π stacking [centroid-to-centroid distance = 3.515 (su? Å]. Additional C—H...Cl and C—H...S interactions, as well as Cl...S contacts < 3.6 Å, consolidate the crystal packing.

  9. Crystal Structure of Na3MoCl6

    Directory of Open Access Journals (Sweden)

    Martin Beran

    2011-07-01

    Full Text Available The ternary chloride Na3MoCl6 is obtained as red crystals from a disproportionation reaction of molybdenum dichloride, {Mo6}Cl12, in an acidic NaCl/AlCl3 melt at 350 °C. The crystal structure (trigonal, P-31c, a = 687.1(1, c = 1225.3(2 pm, Z = 2, V = 501,0(1 106 pm3 is that of Na3CrCl6: within a hexagonal closest-packing of chloride ions two thirds of the octahedral voids are filled between the AB double layers with Na+/Mo3+, and between the BA layers with Na+.

  10. Crystal growth and characterization of bulk Sb2Te3 topological insulator

    Science.gov (United States)

    Sultana, Rabia; Gurjar, Ganesh; Patnaik, S.; Awana, V. P. S.

    2018-04-01

    The Sb2Te3 crystals are grown using the conventional self flux method via solid state reaction route, by melting constituent elements (Sb and Te) at high temperature (850 °C), followed by slow cooling (2 °C/h). As grown Sb2Te3 crystals are analysed for various physical properties by x-ray diffraction (XRD), Raman Spectroscopy, Scanning Electron Microscopy (SEM) coupled with Energy Dispersive x-ray Spectroscopy (EDAX) and electrical measurements under magnetic field (6 Tesla) down to low temperature (2.5 K). The XRD pattern revealed the growth of synthesized Sb2Te3 sample along (00l) plane, whereas the SEM along with EDAX measurements displayed the layered structure with near stoichiometric composition, without foreign contamination. The Raman scattering studies displayed known ({{{{A}}}1{{g}}}1, {{{{E}}}{{g}}}2 and {{{{A}}}1{{g}}}2) vibrational modes for the studied Sb2Te3. The temperature dependent electrical resistivity measurements illustrated the metallic nature of the as grown Sb2Te3 single crystal. Further, the magneto—transport studies represented linear positive magneto-resistance (MR) reaching up to 80% at 2.5 K under an applied field of 6 Tesla. The weak anti localization (WAL) related low field (±2 Tesla) magneto-conductance at low temperatures (2.5 K and 20 K) has been analysed and discussed using the Hikami—Larkin—Nagaoka (HLN) model. Summarily, the short letter reports an easy and versatile method for crystal growth of bulk Sb2Te3 topological insulator (TI) and its brief physical property characterization.

  11. Enzyme catalysis captured using multiple structures from one crystal at varying temperatures

    Directory of Open Access Journals (Sweden)

    Sam Horrell

    2018-05-01

    Full Text Available High-resolution crystal structures of enzymes in relevant redox states have transformed our understanding of enzyme catalysis. Recent developments have demonstrated that X-rays can be used, via the generation of solvated electrons, to drive reactions in crystals at cryogenic temperatures (100 K to generate `structural movies' of enzyme reactions. However, a serious limitation at these temperatures is that protein conformational motion can be significantly supressed. Here, the recently developed MSOX (multiple serial structures from one crystal approach has been applied to nitrite-bound copper nitrite reductase at room temperature and at 190 K, close to the glass transition. During both series of multiple structures, nitrite was initially observed in a `top-hat' geometry, which was rapidly transformed to a `side-on' configuration before conversion to side-on NO, followed by dissociation of NO and substitution by water to reform the resting state. Density functional theory calculations indicate that the top-hat orientation corresponds to the oxidized type 2 copper site, while the side-on orientation is consistent with the reduced state. It is demonstrated that substrate-to-product conversion within the crystal occurs at a lower radiation dose at 190 K, allowing more of the enzyme catalytic cycle to be captured at high resolution than in the previous 100 K experiment. At room temperature the reaction was very rapid, but it remained possible to generate and characterize several structural states. These experiments open up the possibility of obtaining MSOX structural movies at multiple temperatures (MSOX-VT, providing an unparallelled level of structural information during catalysis for redox enzymes.

  12. Crystal structure of homoserine O-acetyltransferase from Leptospira interrogans

    International Nuclear Information System (INIS)

    Wang Mingzhu; Liu Lin; Wang Yanli; Wei Zhiyi; Zhang Ping; Li Yikun; Jiang Xiaohua; Xu Hang; Gong Weimin

    2007-01-01

    Homoserine O-acetyltransferase (HTA, EC 2.3.1.31) initiates methionine biosynthesis pathway by catalyzing the transfer of acetyl group from acetyl-CoA to homoserine. This study reports the crystal structure of HTA from Leptospira interrogans determined at 2.2 A resolution using selenomethionyl single-wavelength anomalous diffraction method. HTA is modular and consists of two structurally distinct domains-a core α/β domain containing the catalytic site and a helical bundle called the lid domain. Overall, the structure fold belongs to α/β hydrolase superfamily with the characteristic 'catalytic triad' residues in the active site. Detailed structure analysis showed that the catalytic histidine and serine are both present in two conformations, which may be involved in the catalytic mechanism for acetyl transfer

  13. Crystal structure of isoflavone reductase from alfalfa (Medicago sativa L.).

    Science.gov (United States)

    Wang, Xiaoqiang; He, Xianzhi; Lin, Jianqiao; Shao, Hui; Chang, Zhenzhan; Dixon, Richard A

    2006-05-19

    Isoflavonoids play important roles in plant defense and exhibit a range of mammalian health-promoting activities. Isoflavone reductase (IFR) specifically recognizes isoflavones and catalyzes a stereospecific NADPH-dependent reduction to (3R)-isoflavanone. The crystal structure of Medicago sativa IFR with deletion of residues 39-47 has been determined at 1.6A resolution. Structural analysis, molecular modeling and docking, and comparison with the structures of other NADPH-dependent enzymes, defined the putative binding sites for co-factor and substrate and potential key residues for enzyme activity and substrate specificity. Further mutagenesis has confirmed the role of Lys144 as a catalytic residue. This study provides a structural basis for understanding the enzymatic mechanism and substrate specificity of IFRs as well as the functions of IFR-like proteins.

  14. Crystal structure and thin film morphology of BBL ladder polymer

    Energy Technology Data Exchange (ETDEWEB)

    Song, H H [Department of Macromolecular Science, Han Nam University, Taejon (Korea, Republic of); Fratini, A V [Department of Chemistry, University of Dayton, Dayton, OH (United States); Chabinyc, M [Department of Chemistry, University of Dayton, Dayton, OH (United States); Price, G E [University of Dayton Research, Dayton, OH (United States); Agrawal, A K [Systran Corporation, Dayton, OH (United States); Wang, C S [University of Dayton Research, Dayton, OH (United States); Burkette, J [University of Dayton Research, Dayton, OH (United States); Dudis, D S [Materials Directorate, Wright Laboratory, Wright-Patterson Air Force Base, OH (United States); Arnold, F E [Materials Directorate, Wright Laboratory, Wright-Patterson Air Force Base, OH (United States)

    1995-03-01

    Crystal structure and morphology of poly[7-oxo-7H-benz(d,e)imidazo(4`,5`:5,6)-benzimidazo(2,1-a)isoquinoline-3,4:10,11-tetrayl-10-carbonyl] (BBL) ladder-like polymer were studied. The polymer forms a two-dimensional lattice of nematic liquid crystalline structure. An orthorhombic unit cell with cell parameters of a=7.87 b=3.37 c=11.97A was determined from the fiber diffraction pattern. In thin films, the rigid chains spontaneously form a layered structure across the film thickness, but in a very unusual manner, i.e. the very large molecular plane is standing perpendicularly to the film surface plane. The results are identical to our recent results of poly(p-phenylene benzobisthiazole) (PBT) film [7]. The polymer, however, lost its anisotropic order upon extrusion into a film and resulted in a fiber-like structure. (orig.)

  15. Synthesis, crystal structure and electronic structure of the binary phase Rh{sub 2}Cd{sub 5}

    Energy Technology Data Exchange (ETDEWEB)

    Koley, Biplab [Department of Chemistry, Indian Institute of Technology Kharagpur, Kharagpur 721302 (India); Chatterjee, S. [Department of Physics, Indian Institute of Technology Kharagpur, Kharagpur 721302 (India); Jana, Partha P., E-mail: ppj@chem.iitkgp.ernet.in [Department of Chemistry, Indian Institute of Technology Kharagpur, Kharagpur 721302 (India)

    2017-02-15

    A new phase in the Rh-Cd binary system - Rh{sub 2}Cd{sub 5} has been identified and characterized by single crystal X-ray diffraction and Energy dispersive X-ray analysis. The stoichiometric compound Rh{sub 2}Cd{sub 5} crystallizes with a unit cell containing 14 atoms, in the orthorhombic space group Pbam (55). The crystal structure of Rh{sub 2}Cd{sub 5} can be described as a defect form of the In{sub 3}Pd{sub 5} structure with ordered vacancies, formed of two 2D atomic layers with the stacking sequence: ABAB. The A type layers consist of (3.6.3.6)-Kagomé nets of Cd atoms while the B type layers consist of (3{sup 5}) (3{sup 7})- nets of both Cd and Rh atoms. The stability of this line phase is investigated by first principle electronic structure calculations on the model of ordered Rh{sub 2}Cd{sub 5}. - Graphical abstract: (3.6.3.6)-Kagomé nets of cadmium atoms (top) and (3{sup 5}) (3{sup 7})- nets of both cadmium and rhodium atoms (bottom) in the structure of Rh{sub 2}Cd{sub 5}.

  16. Lead(ii) soaps: crystal structures, polymorphism, and solid and liquid mesophases.

    Science.gov (United States)

    Martínez-Casado, F J; Ramos-Riesco, M; Rodríguez-Cheda, J A; Redondo-Yélamos, M I; Garrido, L; Fernández-Martínez, A; García-Barriocanal, J; da Silva, I; Durán-Olivencia, M; Poulain, A

    2017-07-05

    The long-chain members of the lead(ii) alkanoate series or soaps, from octanoate to octadecanoate, have been thoroughly characterized by means of XRD, PDF analysis, DSC, FTIR, ssNMR and other techniques, in all their phases and mesophases. The crystal structures at room temperature of all of the members of the series are now solved, showing the existence of two polymorphic forms in the room temperature crystal phase, different to short and long-chain members. Only nonanoate and decanoate present both forms, and this polymorphism is proven to be monotropic. At higher temperature, these compounds present a solid mesophase, defined as rotator, a liquid crystal phase and a liquid phase, all of which have a similar local arrangement. Since some lead(ii) soaps appear as degradation compounds in oil paintings, the solved crystal structures of lead(ii) soaps can now be used as fingerprints for their detection using X-ray diffraction. Pair distribution function analysis on these compounds is very similar in the same phases and mesophases for the different members, showing the same short range order. This observation suggests that this technique could also be used in the detection of these compounds in disordered phases or in the initial stages of formation in paintings.

  17. Ionothermal synthesis, crystal structure, and magnetic study of Co2PO4OH isostructural with caminite.

    Science.gov (United States)

    Wang, Guangmei; Valldor, Martin; Spielberg, Eike T; Mudring, Anja-Verena

    2014-03-17

    A new framework cobalt(II) hydroxyl phosphate, Co2PO4OH, was prepared by ionothermal synthesis using 1-butyl-4-methyl-pyridinium hexafluorophosphate as the ionic liquid. As the formation of Co2PO4F competes in the synthesis, the synthesis conditions have to be judiciously chosen to obtain well-crystallized, single phase Co2PO4OH. Single-crystal X-ray diffraction analyses reveal Co2PO4OH crystallizes with space group I41/amd (a = b = 5.2713(7) Å, c = 12.907(3) Å, V = 358.63(10) Å(3), and Z = 4). Astonishingly, it does not crystallize isotypically with Co2PO4F but rather isotypically with the hydroxyl minerals caminite Mg1.33[SO4(OH)0.66(H2O)0.33] and lipscombite Fe(2–y)PO4(OH) (0 ≤ y ≤ 2/3). Phosphate tetrahedra groups interconnect four rod-packed face-sharing ∞(1){CoO(6/2)} octahedra chains to form a three-dimensional framework structure. The compound Co2PO4OH was further characterized by powder X-ray diffraction, Fourier transform–infrared, and ultraviolet–visible spectroscopy, confirming the discussed structure. The magnetic measurement reveals that Co2PO4OH undergoes a magnetic transition and presents at low temperatures a canted antiferromagnetic spin order in the ground state.

  18. Crystal structure of the Japanese encephalitis virus envelope protein.

    Science.gov (United States)

    Luca, Vincent C; AbiMansour, Jad; Nelson, Christopher A; Fremont, Daved H

    2012-02-01

    Japanese encephalitis virus (JEV) is the leading global cause of viral encephalitis. The JEV envelope protein (E) facilitates cellular attachment and membrane fusion and is the primary target of neutralizing antibodies. We have determined the 2.1-Å resolution crystal structure of the JEV E ectodomain refolded from bacterial inclusion bodies. The E protein possesses the three domains characteristic of flavivirus envelopes and epitope mapping of neutralizing antibodies onto the structure reveals determinants that correspond to the domain I lateral ridge, fusion loop, domain III lateral ridge, and domain I-II hinge. While monomeric in solution, JEV E assembles as an antiparallel dimer in the crystal lattice organized in a highly similar fashion as seen in cryo-electron microscopy models of mature flavivirus virions. The dimer interface, however, is remarkably small and lacks many of the domain II contacts observed in other flavivirus E homodimers. In addition, uniquely conserved histidines within the JEV serocomplex suggest that pH-mediated structural transitions may be aided by lateral interactions outside the dimer interface in the icosahedral virion. Our results suggest that variation in dimer structure and stability may significantly influence the assembly, receptor interaction, and uncoating of virions.

  19. Crystal Structure of Rat Carnitine Palmitoyltransferase II (CPT-II)

    Energy Technology Data Exchange (ETDEWEB)

    Hsiao,Y.; Jogl, G.; Esser, V.; Tong, L.

    2006-01-01

    Carnitine palmitoyltransferase II (CPT-II) has a crucial role in the {beta}-oxidation of long-chain fatty acids in mitochondria. We report here the crystal structure of rat CPT-II at 1.9 Angstroms resolution. The overall structure shares strong similarity to those of short- and medium-chain carnitine acyltransferases, although detailed structural differences in the active site region have a significant impact on the substrate selectivity of CPT-II. Three aliphatic chains, possibly from a detergent that is used for the crystallization, were found in the structure. Two of them are located in the carnitine and CoA binding sites, respectively. The third aliphatic chain may mimic the long-chain acyl group in the substrate of CPT-II. The binding site for this aliphatic chain does not exist in the short- and medium-chain carnitine acyltransferases, due to conformational differences among the enzymes. A unique insert in CPT-II is positioned on the surface of the enzyme, with a highly hydrophobic surface. It is likely that this surface patch mediates the association of CPT-II with the inner membrane of the mitochondria.

  20. Synthesis and crystal structure of chromium-bearing anhydrous wadsleyite

    Science.gov (United States)

    Sirotkina, E. A.; Bindi, L.; Bobrov, A. V.; Aksenov, S. M.; Irifune, T.

    2018-04-01

    A chromium-bearing wadsleyite (Cr- Wad) was synthesized in the model system Mg2SiO4-MgCr2O4 at 14 GPa and 1600 °C and studied from the chemical and structural point of views. Microprobe data gave the formula Mg1.930Cr0.120Si0.945O4, on the basis of 4 oxygen atoms. The crystal structure has been studied by single-crystal X-ray diffraction. The orthorhombic unit-cell parameters are: a = 5.6909(5) Å, b = 11.4640(10) Å, c = 8.2406(9) Å, V = 537.62(9) Å3, Z = 8. The structure, space group Imma, was refined to R 1 = 5.99% in anisotropic approximation using 1135 reflections with F o > 4σ( F o) and 43 parameters. Chromium was found to substitute for both Mg at the octahedral sites and Si at the tetrahedral site, according to the reaction VIMg2+ + IVSi4+ = VICr3+ + IVCr3+. On the whole, the structural topology is nearly identical to that of pure wadsleyite. The successful synthesis of Cr- Wad may be important for the thermobarometry of mantle phase associations.