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Sample records for characterization crystal structure

  1. Preparation, structural, and calorimetric characterization of bicomponent metallic photonic crystals

    Science.gov (United States)

    Kozlov, M. E.; Murthy, N. S.; Udod, I.; Khayrullin, I. I.; Baughman, R. H.; Zakhidov, A. A.

    2007-03-01

    We report preparation and characterization of novel bicomponent metal-based photonic crystals having submicron three-dimensional (3D) periodicity. Fabricated photonic crystals include SiO2 sphere lattices infiltrated interstitially with metals, carbon inverse lattices filled with metal or metal alloy spheres, Sb inverse lattices, and Sb inverse lattices filled with Bi spheres. Starting from a face centered SiO2 lattice template, these materials were obtained by sequences of either templating and template extraction or templating, template extraction, and retemplating. Surprising high fidelity was obtained for all templating and template extraction steps. Scanning electron microscopy (SEM), small angle X-ray scattering (SAXS) and differential scanning calorimetry (DSC) were used to characterize the structure and the effects of the structure on calorimetric properties. To the best of our knowledge, SAXS data on metallic photonic crystals were collected for first time.

  2. 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.

  3. Crystal structure and characterization of pyrroloquinoline quinone disodium trihydrate

    Directory of Open Access Journals (Sweden)

    Ikemoto Kazuto

    2012-06-01

    Full Text Available Abstract Background Pyrroloquinoline quinone (PQQ, a tricarboxylic acid, has attracted attention as a growth factor, and its application to supplements and cosmetics is underway. The product used for these purposes is a water-soluble salt of PQQ disodium. Although in the past, PQQ disodiumpentahydrates with a high water concentration were used, currently, low hydration crystals of PQQ disodiumpentahydrates are preferred. Results We prepared a crystal of PQQ disodium trihydrate in a solution of ethanol and water, studied its structure, and analyzed its properties. In the prepared crystal, the sodium atom interacted with the oxygen atom of two carboxylic acids as well as two quinones of the PQQ disodium trihydrate. In addition, the hydration water of the prepared crystal was less than that of the conventional PQQ disodium crystal. From the results of this study, it was found that the color and the near-infrared (NIR spectrum of the prepared crystal changed depending on the water content in the dried samples. Conclusions The water content in the dried samples was restored to that in the trihydrate crystal by placing the samples in a humid environment. In addition, the results of X-ray diffraction (XRD and X-ray diffraction-differential calorimetry (XRD-DSC analyses show that the phase of the trihydrate crystal changed when the crystallization water was eliminated. The dried crystal has two crystalline forms that are restored to the original trihydrate crystals in 20% relative humidity (RH. This crystalline (PQQ disodium trihydrate is stable under normal environment.

  4. Synthesis and structural characterization of CsNiP crystal

    Indian Academy of Sciences (India)

    G S Gopalakrishna; B H Doreswamy; M J Mahesh; M Mahendra; M A Sridhar; J Shashidhara Prasad; K G Ashamanjari

    2004-02-01

    CsNiP crystals were synthesized by hydrothermal technique and characterized by the X-ray diffraction method. This alkaline transition metal phosphide crystallizes in the hexagonal system with space group P6$_3/mmc$ and cell parameters, = 7.173(2) Å, = 5.944(9) Å, = 264.87(7) Å3 and = 2. The final residual factor is 1 = 0.0362 for 206 reflections with > 2().

  5. STRUCTURAL CHARACTERIZATION OF POLYETHYLENES BY DSC ANALYSIS AFTER CRYSTALLIZATION SEGREGATION

    Institute of Scientific and Technical Information of China (English)

    Yu Ma; Mao Xu

    2000-01-01

    The molecular structure of polyethylene (PE) samples with various comonomers including propylene, 1-butene and 1-hexene was investigated by DSC and 13C-NMR techniques. The density of the samples varies from 0.948 g/cm3 to 0.917 g/cm3, and the molecular weight determined by the GPC method is in the range of 1~2 × 105. The branch point content of the samples was determined by 13C-NMR measurements and was found to be less than 20 per 1000 C atoms along the main chain. Crystallization segregation DSC technique (CSDSC) was used to characterize the branch point distribution or the segment length distribution of PEs. The crystallization segregation was performed in a successive annealing process at decreasing temperatures. The interval of two successive annealing temperatures was 6 K, and the time length of each annealing step was 2.5 h. The CSDSC results clearly indicate that all the PE samples used, including some metallocene PEs,more or less exhibit their non-uniformity in segment length distribution, and bimodal or multimodal CSDSC curves were usually observed. For quantitative characterization of the CSDSC curves and the segment length distribution two parameters,the average melting point, TmAV, and the root-mean-square deviation of melting temperature, (ATm2AV)1/2, were proposed.TmAV is corresponding to the average segment length due to branching and (ATm2AV)1/2 gives information about the width of the segment length distribution. Experimental results show that both the degree of average melting temperature depression and the width of the distribution seem to increase with increasing the branching content and are dependent on the type of comonomers. Very good reproducibility and additivity of the CSDSC method were evidenced experimentally. It was concluded that the CSDSC technique is a sensitive and convenient method for characterizing the segment length distribution of branched polyethylenes and will be of great interest in structure-property relationship

  6. Synthesis, single crystal structure and characterization of pentanitromonoformylhexaazaisowurtzitane.

    Science.gov (United States)

    Chen, Huaxiong; Chen, Shusen; Li, Lijie; Jiao, Qingze; Wei, Tianyu; Jin, Shaohua

    2010-03-15

    Pentanitromonoformylhexaazaisowurtzitane (PNMFIW) was synthesized by the nitrolysis of tetraacetyldiformylhexaazaisowurtzitane (TADFIW) in mixed nitric and sulfuric acids and structurally characterized by element analysis, FT-IR, MS and (1)H NMR. Single crystals of PNMFIW were grown from aqueous solution employing the technique of controlled evaporation. PNMFIW belongs to the orthorhombic system having four molecules in the unit cell, with space group P2(1)2(1)2(1) and the lattice parameters a=8.8000(18)A, b=12.534(2)A, and c=12.829(3)A. The calculated density reaches 1.977 g/cm(3) at 93 K, while the experimental density is 1.946 g/cm(3) at 20 degrees C. The calculated detonation velocity and pressure of PNMFIW according to the experimental density are 9195.76 m/s and 39.68G Pa, respectively. PNMFIW is insensitive compared with epsilon-HNIW through drop hammer impact sensitivity test. PMID:19913358

  7. A novel characterization of organic molecular crystal structures for the purpose of crystal engineering.

    Science.gov (United States)

    Thomas, Noel W

    2015-08-01

    A novel analytical approach is proposed for the characterization of organic molecular crystal structures where close packing is an important factor. It requires the identification of a unique reference axis within the crystal, along which three-dimensional space is divided into close-packed blocks (CPB) and junction zones (JZ). The degree of close packing along the reference axis is quantified by a two-dimensional packing function, ϕ2D, of symmetry determined by the space group. Values of ϕ2D reflect the degree of area-filling in planes perpendicular to this axis. The requirement of close packing within CPB allows the planar structures perpendicular to the reference axis to be analysed as tessellations of area-filling molecular-based cells (MBC), which are generally hexagonal. The form of these cells reflects the molecular shape in the cross-section, since their vertices are given by the centres of the voids between molecules. There are two basic types of MBC, Type 1, of glide or pseudo-glide symmetry, and Type 2, which is formed by lattice translations alone and generally requires a short unit-cell axis. MBC at layers of special symmetry are used to characterize the structures in terms of equivalent ellipses with parameters aell, bell and χell. The ratio aell/bell allows the established α, β, γ classification to be integrated into the current framework. The values of parameters aell and bell arising from all the structures considered, polynuclear aromatic hydrocarbons (PAH), substituted anthracenes and anthraquinones (SAA) and 2-benzyl-5-benzylidene (BBCP) are mapped onto a universal curve. The division of three-dimensional space into CPB and JZ is fundamentally useful for crystal engineering, since the structural perturbations brought about by substitution at hydrogen positions located within JZ are minimal. A contribution is also made to ongoing debate concerning the adoption of polar space groups, isomorphism and polymorphism. PMID:26208627

  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: 0.508, year: 2014

  9. Orthorhombic polymorph of ErP{sub 5}O{sub 14}, crystal structure and characterization

    Energy Technology Data Exchange (ETDEWEB)

    Katrusiak, A. [Uniwersytet Adama Mickiewicza, Poznan (Poland); Kaczmarek, F. [Uniwersytet Adama Mickiewicza, Poznan (Poland)

    1995-08-01

    Erbium pentaphosphate crystals have been characterized and the structure of the orthorhombic polymorph (type III) determined by X-rays. It has been found that the orthorhombic samples of ErP{sub 5}O{sub 14}, space group Pnma, crystallize mainly at higher temperatures and usually are much larger than monoclinic crystals, space group C2/c, obtained from lower-temperature crystallizations. Differences in fluorescence and upconversion properties between orthorhombic and monoclinic polymorphs have been detected. (orig.)

  10. Thiosaccharine disulfide: Synthesis, crystal structure, spectroscopic characterization and theoretical study

    Science.gov (United States)

    Ferullo, Ricardo M.; Granados, Alejandro; Lanterna, Anabel; Güida, Jorge A.; Piro, Oscar E.; Castellano, Eduardo E.; Dennehy, Mariana

    2013-01-01

    The title compound, (thiosaccharine disulfide), bis[1,1'dioxide-2,3-dihidro-1,2-benzoisothiazol]disulfide, (tsac)2 has been synthesized and fully characterized by UV-Visible, IR, Raman, 1H and 13C NMR spectroscopy elemental analysis and structural X-ray crystallography. A DFT theoretical study has been performed and good agreement between experimental and theoretical values of structural parameters and vibration frequencies have been achieved.

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

    International Nuclear Information System (INIS)

    Highlights: → Good quality crystals of nicotinium trifluoroacetate in monoclinic system were grown for first time. → Nicotinium trifluoroacetate crystal exhibits third order nonlinear optical properties. → The optical spectrum of nicotinium trifluoroacetate crystal reveals the wide transmission in the entire range with cutoff wavelength at 286 nm. → 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. 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.

  13. 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)

  14. Crystal structure and characterization of a novel organic optical crystal: 2-Aminopyridinium trichloroacetate

    International Nuclear Information System (INIS)

    Research highlights: → Good quality crystals of 2-aminopyridinium trichloroacetate were grown for first time. → 2-Aminopyridinium trichloroacetate crystal belongs to monoclinic crystal system with space group P21/c. → 2-Aminopyridinium trichloroacetate crystal exhibits third order nonlinear optical properties. → 2-Aminopyridinium trichloroacetate is a low dielectric constant material. -- Abstract: 2-Aminopyridinium trichloroacetate, a novel organic optical material has been synthesized and crystals were grown from aqueous solution employing the technique of controlled evaporation. 2-Aminopyridinium trichloroacetate crystallizes in monoclinic system with space group P21/c and the lattice parameters are a = 8.598(5) A, b = 11.336(2) A, c = 11.023(2) A, β = 102.83(1)o and volume = 1047.5(3) A3. High-resolution X-ray diffraction measurements were performed to analyze the structural perfection of the grown crystals. Thermal analysis shows a sharp endothermic peak at 124 oC due to melting reaction of 2-aminopyridinium trichloroacetate. UV-vis-NIR studies reveal that 2-aminopyridinium trichloroacetate has UV cutoff wavelength at 354 nm. Dielectric studies show that dielectric constant and dielectric loss decreases with increasing frequency and finally it becomes almost a constant at higher frequencies for all temperatures. The negative nonlinear optical parameters of 2-aminopyridinium trichloroacetate were derived by the Z-scan technique.

  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. Crystal structure and electrical characterization of mixed lithium ferrite ceramics.

    Directory of Open Access Journals (Sweden)

    Suresh. S. Darokar

    2015-03-01

    Full Text Available A Cobalt and Aluminium substituted Lithium ferrite ( M- type samples with the general chemical formula Li0.5Fe0.5+xAl12-2X Co xO19 were synthesized using reacting oxide by high temperature solid state reaction technique. The structural characterization of compound has been carried out from X-Ray diffraction powder pattern. The compounds are in single hexagonal phase without traces of uncertainly ambiguous reflection. From XRD pattern lattice parameters has recorded with increasing doped aluminum element in the range from a = 5.807 Å to 5.906 Å and c = 22.507 Å to 22.585 Å pertaining the space group P63/mmc (No.194. The mass density of the ferrites were found linearly varies and depends upon the mass and volume of sample. The X-Ray density has depends upon the lattice constant and molecular weight of the compounds. The average particle size was also estimated. The compounds were studies magnetically by using Guoy’s method in the temperature range 300 to 550 K, the result shows that the compounds are paramagnetic in nature.The Curie molar constant was work out.

  17. Characterization of dislocation structures in silicon carbide single crystals

    Science.gov (United States)

    Vetter, William M.

    1999-07-01

    Two types of defects in PVT-grown 6H and 4H-SiC crystals were studied: screw dislocations that follow the axial direction of the crystal and dislocations that follow directions in the crystal's basal plane. The screw dislocations possessed a range of Burgers vector magnitudes, multiples of the axial parameter c, that could be determined by x-ray topographic image analysis. Hollow cores termed "micropipes" were observed when Burgers, vectors were larger than 3c. The micropipes were studied by a variety of methods: optical microscopy, laser scanning confocal microscopy, scanning electron microscopy, transmission electron microscopy and atomic force microscopy. The micropipes were tubes 0.1 to 10mum in diameter. They were faceted, primarily along the {101¯0} planes, but also had {112¯0} facets. When encountering the growth surface of a crystal, they flared out into a trumpet-shape. Growth spirals sometimes occurred, originating from the trumpets' rims. The screw dislocations are visible in back-reflection synchrotron white beam x-ray topographs of basal-cut SiC wafers in striking contrast as black rings surrounding white circles, though such topographs are contaminated by a series of harmonic reflections, g = (0006n), where n = 3 to 16. By calculating and considering their intensities, and comparison with a g = 00018 Lang topograph taken with CuKalpha1 radiation, the g = 00024 harmonic was shown to be the most important contributor. Basal plane dislocations were seen in x-ray topographs of SiC looping from the points where screw dislocations occurred. Their extinction behavior showed they belonged to the set b = 13 . In some transmission electron micrographs, perfect dislocations with similar extinction behavior, along with partial dislocations with b = 13 , were seen originating from the micropipes' walls, curving out into the crystal a distance of 1 to 3mum, then back to terminate at the micropipe. Others led out of the field of view. Contrast is associated with

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

    International Nuclear Information System (INIS)

    Highlights: • Growth of large Al-substituted crystals BaFe12−xAlxO19. • 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 BaFe12−xAlxO19 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

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

    International Nuclear Information System (INIS)

    A novel 4-(2-meso-BOBIPY-phenoxy)phthalonitrile (6) derivative has been synthesized starting from BF3–OEt2 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, 1H and 13C 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, 1H and 13C 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, 1H and 13C 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

  20. Synthesis, spectroscopic characterizations, crystal structures and DFT studies of nalidixic acid carbonyl hydrazones derivatives

    Science.gov (United States)

    Bergamini, F. R. G.; Ribeiro, M. A.; Lancellotti, M.; Machado, D.; Miranda, P. C. M. L.; Cuin, A.; Formiga, A. L. B.; Corbi, P. P.

    2016-09-01

    This article describes the synthesis and characterization of the 1-ethyl-7-methyl-4-oxo-1,4-dihydro-1,8-naphthyridine-3-carbohydrazide (hzd) and six carbonyl hydrazones derivatives of the nalidixic with 1H-pyrrol-2-ylmethylidene (hpyrr), 1H-imidazol-2-ylmethylidene (h2imi), pyridin-2-ylmethylidene (h2py), pyridin-3-ylmethylidene (h3py), pyridin-4-ylmethylidene(h4py) and (2-hydroxyphenyl)methylidene (hsali). The carbonyl hydrazones were characterized by elemental and ESI-QTOF-MS analyses, IR and detailed NMR spectroscopic measurements. The 2D NMR experiments allowed the unambiguous assignment of the hydrogen, carbon and nitrogen atoms, which have not been reported for nalidixic acid carbonyl hydrazone derivatives so far. Crystal structures of hzd and the new carbonyl hydrazones h2imi, hpyrr and h3py were determined by X-ray diffraction studies. Although the synthesis of hzd was reported decades ago, the hzd crystal structure have not been reported yet. Geometric optimizations of all the characterized structures were performed with the aid of DFT studies. Despite the fact that the hydrazones with 2-pyridine carboxylic acid (h2py) and salicyl aldehyde (hsali) were already reported by literature, a detailed spectroscopic study followed by DFT studies are also reported for such compounds in this manuscript. Antimicrobial studies of the compounds are also presented.

  1. A hirshfeld surface analysis, crystal structure and physicochemical characterization of 1-ethylpiperazinium trichlorocadmate(II)

    Science.gov (United States)

    Soudani, S.; Jeanneau, E.; Jelsch, C.; Lefebvre, F.; Ben Nasr, C.

    2016-07-01

    A novel organic-inorganic hybrid material, C6H15N2CdCl3.H2O, was synthesized, and its structure was determined at room temperature in the monoclinic space group P21/n with the following parameters: a = 10.3829 (17), b = 7.7459 (12), c = 14.905 (2) Å, β = 98.801 (15), and Z = 4. Its crystal structure is characterized by one-dimensional polymeric chains of edge-sharing CdCl5N distorted octahedra. These chains are linked to the water molecules via Osbnd H … Cl hydrogen bonds to form layers parallel to the (b, a + c) plane. The crystal structure was stabilized by an extensive network of Nsbnd H … Cl, Osbnd H … Cl and Nsbnd H … O hydrogen bonds. The differential scanning calorimetry (DSC) reveals that the title compound is stable until 101.6 °C. The optimized geometry parameters, normal mode frequencies, and corresponding vibrational assignments of the present compound were theoretically examined by DFT/B3LYP method with the Lanl2dz basis set. The FT-IR spectrum of the polycrystalline sample was examined and compared to the calculated spectrum. The calculated results showed that the optimized geometry could well reproduce the crystal structure and that the theoretical vibrational frequency values were in good agreement with their experimental counterparts.

  2. Crystal structure and functional characterization of a light-driven chloride pump having an NTQ motif.

    Science.gov (United States)

    Kim, Kuglae; Kwon, Soon-Kyeong; Jun, Sung-Hoon; Cha, Jeong Seok; Kim, Hoyoung; Lee, Weontae; Kim, Jihyun F; Cho, Hyun-Soo

    2016-01-01

    A novel light-driven chloride-pumping rhodopsin (ClR) containing an 'NTQ motif' in its putative ion conduction pathway has been discovered and functionally characterized in a genomic analysis study of a marine bacterium. Here we report the crystal structure of ClR from the flavobacterium Nonlabens marinus S1-08(T) determined under two conditions at 2.0 and 1.56 Å resolutions. The structures reveal two chloride-binding sites, one around the protonated Schiff base and the other on a cytoplasmic loop. We identify a '3 omega motif' formed by three non-consecutive aromatic amino acids that is correlated with the B-C loop orientation. Detailed ClR structural analyses with functional studies in E. coli reveal the chloride ion transduction pathway. Our results help understand the molecular mechanism and physiological role of ClR and provide a structural basis for optogenetic applications. PMID:27554809

  3. Flexible and Asymmetric Ligand in Constructing Coordinated Complexes: Synthesis, Crystal Structures and Fluorescent Characterization

    Directory of Open Access Journals (Sweden)

    Jianhua Lin

    2010-12-01

    Full Text Available Flexible and asymmetric ligand L [L = 1-((pyridin-3-ylmethyl-1H-benzotriazole], is used as a basic backbone to construct complicated metal-organic frameworks. Two new polymers, namely, [Ag2(L2(NO32]n (1 and [Ag(L(ClO4]n (2, were synthesized and characterized by X-ray structure analysis and fluorescent spectroscopy. The complex 1 gives an “S” type double helical conformation, whereas complex 2 exhibits a 1D zigzag configuration. Different anions affect the silver coordination geometry and crystal packing topology.

  4. Synthesis, growth, structure and characterization of chalcone crystal: A novel organic NLO material

    Science.gov (United States)

    Agilandeshwari, R.; Meenatchi, V.; Meenakshisundaram, S. P.

    2016-08-01

    Single crystals of a chalcone, (E)-3-(4-bromophenyl)-1-(2-hydroxyphenyl)prop-2-en-1-one (BHP), were grown by the slow evaporation solution growth technique. The structure is elucidated by single-crystal X-ray diffraction analysis and the crystal belongs to the monoclinic system with noncentrosymmetric space group P21. Optical studies reveal that the absorption is minimum in the visible region and the cut-off wavelength is at ∼468 nm. The band-gap energy was estimated by the application of the Kubelka-Munk algorithm. The powder X-ray diffraction pattern reveals the good crystallinity of the as-grown specimen. The vibrational patterns in FT-IR are used to identify the functional groups and thermal studies indicate the stability of the material. The second harmonic generation efficiency (SHG), as estimated by Kurtz and Perry powder technique, reveals the superior nonlinear optical character of this material. Hirshfeld surface analysis is done to quantify the intermolecular interactions, responsible for developing a nonlinear atmosphere. As-grown crystals were further characterized by SEM, NMR, mass spectrometry and elemental analysis.

  5. Characterization and crystal structure of lysine insensitive Corynebacterium glutamicum dihydrodipicolinate synthase (cDHDPS) protein

    Energy Technology Data Exchange (ETDEWEB)

    Rice, E.A.; Bannon, G.A.; Glenn, K.C.; Jeong, S.S.; Sturman, E.J.; Rydel, T.J. (Monsanto)

    2008-11-21

    The lysine insensitive Corynebacterium glutamicum dihydrodipicolinate synthase enzyme (cDHDPS) was recently successfully introduced into maize plants to enhance the level of lysine in the grain. To better understand lysine insensitivity of the cDHDPS, we expressed, purified, kinetically characterized the protein, and solved its X-ray crystal structure. The cDHDPS enzyme has a fold and overall structure that is highly similar to other DHDPS proteins. A noteworthy feature of the active site is the evidence that the catalytic lysine residue forms a Schiff base adduct with pyruvate. Analyses of the cDHDPS structure in the vicinity of the putative binding site for S-lysine revealed that the allosteric binding site in the Escherichia coli DHDPS protein does not exist in cDHDPS due to three non-conservative amino acids substitutions, and this is likely why cDHDPS is not feedback inhibited by lysine.

  6. Structural and magnetic characterization of electro-crystallized magnetite nanoparticles under constant current

    International Nuclear Information System (INIS)

    Graphical abstract: Structural and magnetic properties of electro-crystallized magnetite nanoparticles under constant current were studied. All samples were characterized using XRD, SEM, VSM, and Mössbauer spectrometry. - Highlights: • The effect of applied current on morphology and properties of Fe3O4 is studied. • The particle size and morphology are controllable by adjusting the current. • The magnetization depends on particle size, type of surfactant and applied current. • The clear correlation between magnetization and the mean particle size is observed. - Abstract: The effect of applied current on the morphology, particle size, structure, and magnetic properties of magnetite nanoparticles prepared by electro-crystallization method was studied. The synthesis was performed in an electrochemical cell containing two iron electrodes and an aqueous solution of sodium sulfate, and either thiourea, sodium butanoate, or β-cyclodextrine as organic stabilizer. All the samples were characterized by XRD, SEM, VSM, and Mössbauer spectroscopy. X-ray diffraction patterns, clearly confirmed that all products have the cubic spinel Fe3O4 crystal structure. Electron microscope images of the samples showed that their mean particle size is in the range 20–80 nm, and depends critically on the applied current and type of the organic additives. Specific magnetization of the samples at room temperature ranges from 60 to 90 A m2 kg−1, depending on the growth conditions. Room temperature Mössbauer spectra are typical of nonstoichiometric Fe3−δO4, with a small excess of Fe3+, 0.06 ≤ δ ≤ 0.17

  7. Structural and magnetic characterization of electro-crystallized magnetite nanoparticles under constant current

    Energy Technology Data Exchange (ETDEWEB)

    Mosivand, Saba [Physics Department, Faculty of Science, Lorestan University, Lorestan (Iran, Islamic Republic of); Kazeminezhad, Iraj, E-mail: I.Kazeminezhad@scu.ac.ir [Physics Department, Faculty of Science, Shahid Chamran University, Ahvaz (Iran, Islamic Republic of)

    2015-10-15

    Graphical abstract: Structural and magnetic properties of electro-crystallized magnetite nanoparticles under constant current were studied. All samples were characterized using XRD, SEM, VSM, and Mössbauer spectrometry. - Highlights: • The effect of applied current on morphology and properties of Fe{sub 3}O{sub 4} is studied. • The particle size and morphology are controllable by adjusting the current. • The magnetization depends on particle size, type of surfactant and applied current. • The clear correlation between magnetization and the mean particle size is observed. - Abstract: The effect of applied current on the morphology, particle size, structure, and magnetic properties of magnetite nanoparticles prepared by electro-crystallization method was studied. The synthesis was performed in an electrochemical cell containing two iron electrodes and an aqueous solution of sodium sulfate, and either thiourea, sodium butanoate, or β-cyclodextrine as organic stabilizer. All the samples were characterized by XRD, SEM, VSM, and Mössbauer spectroscopy. X-ray diffraction patterns, clearly confirmed that all products have the cubic spinel Fe{sub 3}O{sub 4} crystal structure. Electron microscope images of the samples showed that their mean particle size is in the range 20–80 nm, and depends critically on the applied current and type of the organic additives. Specific magnetization of the samples at room temperature ranges from 60 to 90 A m{sup 2} kg{sup −1}, depending on the growth conditions. Room temperature Mössbauer spectra are typical of nonstoichiometric Fe{sub 3−δ}O{sub 4}, with a small excess of Fe{sup 3+}, 0.06 ≤ δ ≤ 0.17.

  8. Surface Structure Spread Single Crystals ((SC)-C-4): Preparation and characterization

    Energy Technology Data Exchange (ETDEWEB)

    de Alwis, A; Holsclaw, B; Pushkarev, V V; Reinicker, A; Lawton, T J; Blecher, M E; Sykes, E C. H.; Gellman, A J

    2013-02-01

    A set of six spherically curved Cu single crystals referred to as Surface Structure Spread Single Crystals (S{sup 4}Cs) has been prepared in such a way that their exposed surfaces collectively span all possible crystallographic surface orientations that can be cleaved from the face centered cubic Cu lattice. The method for preparing these S{sup 4}Cs and for finding the high symmetry pole point are described. Optical profilometry has been used to determine the true shapes of the S{sup 4}Cs and show that over the majority of the surface, the shape is extremely close to that of a perfect sphere. The local orientations of the surfaces lie within ±1{degree} of the orientation expected on the basis of the spherical shape; their orientation is as good as that of many commercially prepared single crystals. STM imaging has been used to characterize the atomic level structure of the Cu(111)±11{degree}-S{sup 4}C. This has shown that the average step densities and the average step orientations match those expected based on the spherical shape. In other words, although there is some distribution of step-step spacing and step orientations, there is no evidence of large scale reconstruction or faceting. The Cu S{sup 4}Cs have local structures based on the ideal termination of the face centered cubic Cu lattice in the direction of termination. The set of Cu S{sup 4}Cs will serve as the basis for high throughput investigations of structure sensitive surface chemistry on Cu.

  9. Crystallization and preliminary structural characterization of the two actin-depolymerization factors of the malaria parasite

    International Nuclear Information System (INIS)

    The expression, purification and crystallization of Plasmodium actin-depolymerization factors 1 and 2 are described. X-ray diffraction data were collected to 2.0 and 2.1 Å resolution, respectively, and the structures of both proteins in solution were characterized. The malaria parasite Plasmodium depends on its actin-based motor system for motility and host-cell invasion. Actin-depolymerization factors are important regulatory proteins that affect the rate of actin turnover. Plasmodium has two actin-depolymerization factors which seem to have different functions and display low sequence homology to the higher eukaryotic family members. Plasmodium actin-depolymerization factors 1 and 2 have been crystallized. The crystals diffracted X-rays to maximum resolutions of 2.0 and 2.1 Å and belonged to space groups P3121 or P3221, with unit-cell parameters a = b = 68.8, c = 76.0 Å, and P21212, with unit-cell parameters a = 111.6, b = 57.9, c = 40.5 Å, respectively, indicating the presence of one or two molecules per asymmetric unit in both cases

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

    Science.gov (United States)

    Khalaji, Aliakbar Dehno; Mogheiseh, Mohsen; Eigner, Václav; Dusek, Michal; Chow, Tahsin J.; Maddahi, Elham

    2015-10-01

    New organic compounds, cin-aa (1) and mecin-aa (2), containing cyanoacrylic acid as an acceptor were synthesized by the reaction of cinnamaldehyde or α-methylcinnamaldehyde with cyanoaceticacid in acetonitrile. The compounds 1 and 2 were characterized by elemental analyses (CHN), FT-IR, UV-Vis and 1H NMR spectroscopy, and their monoclinic centrosymmetric structures were determined by single crystal X-ray diffraction. In addition, they were tested for their potential use as photosensitizers in dye-sensitized solar cells (DSSC). Overall conversion efficiencies of 1 and 2 were determined as 0.04 and 0.09, respectively, under full sunlight irradiation. To get further insight into the molecular structure of 1 and 2, 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.

  11. Single crystal growth, structural characterization, thermal and optical properties of a novel organometallic nonlinear optical crystal: MnHg(SCN) 4(C 2H 5NO) 2

    Science.gov (United States)

    Wang, X. Q.; Cheng, X. F.; Zhang, S. J.; Xu, D.; Zhang, G. H.; Sun, Z. H.; Yu, F. P.; Liu, X. J.; Liu, W. L.; Chen, C. L.

    2010-02-01

    A novel potentially useful organometallic nonlinear optical crystal, manganese mercury thiocyanate-bis(N-methylformamide), MnHg(SCN) 4(C 2H 5NO) 2 (MMTN) has been prepared, and large highly-optical quality single crystals with dimensions up to 29×28×14 mm 3 have been grown. The structural characterization, thermal and optical properties of the grown crystals are investigated. The growth morphology was obtained by indexing the X-ray powder diffraction data and compared with that deducing from the single crystal structure data using the Bravais-Friedel-Donnay-Harker model. The thermal analysis reveals that MMTN crystal possesses good physicochemical stability. The specific heat of the crystal is 635.1 J mol -1 K -1 at 300 K. The thermal expansion coefficient along the a, b, and c axis is α1=6.18×10 -5 K -1, α2=3.91×10 -5 K -1 and α3=9.53×10 -6 K -1, respectively. The laser damage threshold of MMTN crystal is about 225.7 MW/cm 2 with pulse width of 18 ns at 1064 nm. The powder second harmonic efficiency of the crystal is about 1.1 pm/V and the UV transparency cutoff is 354 nm, which are interpreted on the basis of the crystal structure with the Molecular Orbital theory using a GAUSSIAN03 program.

  12. 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.

  13. Synthesis, Crystal Structure and Characterization of a Cobalt Coordination Polymer: [Co(suc)(L)]n

    Institute of Scientific and Technical Information of China (English)

    HONG Jun

    2008-01-01

    The title complex, [Co(suc)(L)]n 1 (L = 2-phenyl-1H-1,3,7,8-tetraazacyclopenta- [l]phenanthrene and H2suc = succinic acid) has been hydrothermally obtained and characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. It crystallizes in orthorhombic, space group Pcca with a = 13.936(3), b = 9.918(2), c = 28.670(6) (A), V = 3962.4(14) A()3, Z = 8, CoC23H16N4O4, Mr = 471.33, Dc = 1.580 g/cm3, F(000) = 1928, μ(MoKa) = 0.907 mm(1, R = 0.0543 and wR = 0.1336. Compound 1 exhibits one-dimensional chain structures which are further stacked by π-π interactions to give a supramolecular layer. Finally, the N-H…O hydrogen bonds between the nitrogen atom of L and carboxylate oxygen atom stabilize the structure of 1.

  14. Crystal Structure and Characterization of Salicylic Acid-benzene Azimide Cocrystal

    Institute of Scientific and Technical Information of China (English)

    DUAN Jiong; GUO Ping; PAN Qing-Qing; WU You; WU Xiao-Qing; LI Hui

    2013-01-01

    A new single crystal of 1∶1 salicylic acid-benzene azimide was determined and characterized.It belongs to space group P21/n with a =13.8085(13),b =5.3846(4),c =16.7063(13) (A)and β =102.331(9)°.Crystals of the title compound,C7H6O3·C6H5N3,were obtained by cocrystallization.FT-IR,Raman spectroscopy and TGA-DTA were applied to characterize the title compound as supplemental evidence to prove the formation of the crystal.Our work describes the solubility of the crystal by considering the equilibria between the crystal,components,and solution mixture.

  15. Crystal structure and characterization of a novel acentric imidazolium analog [C3N2H5+][Br

    Science.gov (United States)

    Gągor, A.; Piecha, A.; Jakubas, R.; Miniewicz, A.

    2011-02-01

    A novel nonlinear optical crystal [C3N2H5+][Br] has been synthesized and characterized by a single-crystal X-ray diffraction, calorimetric, dilatometric and dielectric measurements. Above 200 K the crystal structure is polar, with symmetry R3. It consists of a highly disordered imidazolium cations and discrete Br anions. The compound reveals a first order phase transition at 199/201 K (cooling/heating cycle) which leads to the monoclinic centrosymmetric space group P21/m. The exceptionally large increment of dielectric permittivity accompaning the structure transformation is related to the freezing of cation motions and a significant rebuilding of the anionic substructure.

  16. Crystal structure and characterization of particulate methane monooxygenase from Methylocystis species strain M.

    Science.gov (United States)

    Smith, Stephen M; Rawat, Swati; Telser, Joshua; Hoffman, Brian M; Stemmler, Timothy L; Rosenzweig, Amy C

    2011-11-29

    Particulate methane monooxygenase (pMMO) is an integral membrane metalloenzyme that oxidizes methane to methanol in methanotrophic bacteria. Previous biochemical and structural studies of pMMO have focused on preparations from Methylococcus capsulatus (Bath) and Methylosinus trichosporium OB3b. A pMMO from a third organism, Methylocystis species strain M, has been isolated and characterized. Both membrane-bound and solubilized Methylocystis sp. strain M pMMO contain ~2 copper ions per 100 kDa protomer and exhibit copper-dependent propylene epoxidation activity. Spectroscopic data indicate that Methylocystis sp. strain M pMMO contains a mixture of Cu(I) and Cu(II), of which the latter exhibits two distinct type 2 Cu(II) electron paramagnetic resonance (EPR) signals. Extended X-ray absorption fine structure (EXAFS) data are best fit with a mixture of Cu-O/N and Cu-Cu ligand environments with a Cu-Cu interaction at 2.52-2.64 Å. The crystal structure of Methylocystis sp. strain M pMMO was determined to 2.68 Å resolution and is the best quality pMMO structure obtained to date. It provides a revised model for the pmoA and pmoC subunits and has led to an improved model of M. capsulatus (Bath) pMMO. In these new structures, the intramembrane zinc/copper binding site has a different coordination environment from that in previous models. PMID:22013879

  17. Crystal Structure and Characterization of Particulate Methane Monooxygenase from Methylocystis species Strain M

    Energy Technology Data Exchange (ETDEWEB)

    Smith, Stephen M.; Rawat, Swati; Telser, Joshua; Hoffman, Brian M.; Stemmler, Timothy L.; Rosenzweig, Amy C. (WSU-MED); (NWU)

    2012-02-08

    Particulate methane monooxygenase (pMMO) is an integral membrane metalloenzyme that oxidizes methane to methanol in methanotrophic bacteria. Previous biochemical and structural studies of pMMO have focused on preparations from Methylococcus capsulatus (Bath) and Methylosinus trichosporium OB3b. A pMMO from a third organism, Methylocystis species strain M, has been isolated and characterized. Both membrane-bound and solubilized Methylocystis sp. strain M pMMO contain {approx}2 copper ions per 100 kDa protomer and exhibit copper-dependent propylene epoxidation activity. Spectroscopic data indicate that Methylocystis sp. strain M pMMO contains a mixture of Cu{sup I} and Cu{sup II}, of which the latter exhibits two distinct type 2 Cu{sup II} electron paramagnetic resonance (EPR) signals. Extended X-ray absorption fine structure (EXAFS) data are best fit with a mixture of Cu-O/N and Cu-Cu ligand environments with a Cu-Cu interaction at 2.52-2.64 {angstrom}. The crystal structure of Methylocystis sp. strain M pMMO was determined to 2.68 {angstrom} resolution and is the best quality pMMO structure obtained to date. It provides a revised model for the pmoA and pmoC subunits and has led to an improved model of M. capsulatus (Bath) pMMO. In these new structures, the intramembrane zinc/copper binding site has a different coordination environment from that in previous models.

  18. Crystal structure and functional characterization of a light-driven chloride pump having an NTQ motif

    Science.gov (United States)

    Kim, Kuglae; Kwon, Soon-Kyeong; Jun, Sung-Hoon; Cha, Jeong Seok; Kim, Hoyoung; Lee, Weontae; Kim, Jihyun F.; Cho, Hyun-Soo

    2016-01-01

    A novel light-driven chloride-pumping rhodopsin (ClR) containing an ‘NTQ motif' in its putative ion conduction pathway has been discovered and functionally characterized in a genomic analysis study of a marine bacterium. Here we report the crystal structure of ClR from the flavobacterium Nonlabens marinus S1-08T determined under two conditions at 2.0 and 1.56 Å resolutions. The structures reveal two chloride-binding sites, one around the protonated Schiff base and the other on a cytoplasmic loop. We identify a ‘3 omega motif' formed by three non-consecutive aromatic amino acids that is correlated with the B–C loop orientation. Detailed ClR structural analyses with functional studies in E. coli reveal the chloride ion transduction pathway. Our results help understand the molecular mechanism and physiological role of ClR and provide a structural basis for optogenetic applications. PMID:27554809

  19. Synthesis and Crystal Structural Characterization of a Thiosemicarbazone Derived from 4-Acylpyrazolone

    Institute of Scientific and Technical Information of China (English)

    LIU Guang-Fei; LIU Lang; HU Xin; JIA Dian-Zeng; YU Kai-Bei

    2006-01-01

    The reaction of 4-(p-fluobenzoyl)-2,5-dihydro-3-methyl-1-phenyl pyrazol-5-one with thiosemicarbazide in MeOH followed by recrystallization in EtOH gave rise to yellowish lamellar crystals of 4(p-fluo-α-aminothiocarbonyl hydrazonobenzal)-2,5-dihydro-3-methyl- 1 -phenyl pyrazol-5-one 1. It crystallizes in orthorhombic, space group Pbca with a = 18.445(4), b = 11.987(2),c = 19.249(4) (A), V= 4256.1(18) (A)3, Z = 8, Mr = 415.49, Dc= 1.297 g/cm3, T= 296(2) K, F(000) =1744, μ(MoKα) = 0.186 cm-1, R = 0.0521 and wR = 0.1211 for 1661 observed reflections with I >2σ(I). The compound was structurally characterized by elemental analyses, IR and 1H NMR. The intermolecular hydrogen bonds are present and a two-dimensional framework is formed by two intermolecular hydrogen bonds in the (001) plane.

  20. Crystal Structures of Furazanes

    Directory of Open Access Journals (Sweden)

    Thomas M. Klapötke

    2015-09-01

    Full Text Available Several nitrogen-rich salts of 3-nitramino-4-nitrofurazane and dinitraminoazoxyfurazane were synthesized and characterized by various spectroscopic methods. The crystal structures were determined by low temperature single crystal X-ray diffraction. Moreover the sensitivities toward thermal and mechanical stimuli were determined by differential thermal analysis (DTA and BAM (Bundesanstalt für Materialforschung und -prüfung methods. The standard enthalpies of formation were calculated for all compounds at the CBS-4M level of theory, and the energetic performance was predicted with the EXPLO5 V6.02 computer code.

  1. Investigation on growth, structure and characterization of succinate salt of 8-hydroxyquinoline: An organic NLO crystal

    Science.gov (United States)

    Thirumurugan, R.; Babu, B.; Anitha, K.; Chandrasekaran, J.

    2015-04-01

    8-Hydroxyquinolinium succinate (8-HQSU) has been synthesized and single crystals were grown from ethanol solvent by employing the technique of slow evaporation at room temperature. The structure of the grown crystal has been elucidated by single crystal X-ray diffraction analysis. It reveals that 8-HQSU crystallizes in monoclinic system with non-centro symmetric space group P21. FTIR, 1H and 13C NMR spectral investigations have been carried out to identify the vibrational modes of various functional groups and placement of proton and carbon in the 8-HQSU compound, respectively. UV-vis-NIR transmission spectrum shows the cutoff wavelength around 357 nm. In addition, a photoluminescence spectral analysis was carried out for 8-HQSU crystals. The thermal properties of crystals were evaluated from TGA and DTA techniques and the crystal was found to be stable up to 145 °C. The dielectric studies show that the dielectric constant and dielectric loss decrease exponentially with frequency at different temperatures. Photoconductivity studies were carried out on the grown crystals it reveals the positive photo conducting nature. Powder second harmonic generation property of the crystal was confirmed by Kurtz and Perry powder SHG technique and it is found to be 1.3 times greater than that of KDP.

  2. Crystal Structure and Characterization of a New Eight Coordinated Cadmium Complex

    International Nuclear Information System (INIS)

    In this work, a new cadmium complex [Cd(L)(CH3COO)2]-2H2O (1) with the ligand L, N,N'-bis(2-pyridinecar-boxalidene)-1,2-cyclohexanediamine was prepared and identified by elemental analysis, FT-IR, Raman, 1H NMR spectroscopy and single-crystal X-ray diffraction. The cadmium atom in the crystal structure of 1 has distorted triangular dodecahedral geometry by coordination of the four nitrogen atoms of L and four oxygen atoms of the two acetate ions. Two water molecules are also incorporated in the crystal network. The O-H···O hydrogen bonds present in the crystal structure of 1. In this work, three structural surveys including coordination numbers of the cadmium atom, coordination modes of L and resonance in pyridine-2-ylmethanimine-based compounds are presented

  3. Crystal Structure and Characterization of a New Eight Coordinated Cadmium Complex

    Energy Technology Data Exchange (ETDEWEB)

    Hakimi, Mohammad; Moeini, Keyvan; Mardani, Zahra; Khorrami, Farzaneh [Payame Noor Univ., Tehran (Iran, Islamic Republic of)

    2013-06-15

    In this work, a new cadmium complex [Cd(L)(CH{sub 3}COO){sub 2}]-2H{sub 2}O (1) with the ligand L, N,N'-bis(2-pyridinecar-boxalidene)-1,2-cyclohexanediamine was prepared and identified by elemental analysis, FT-IR, Raman, {sup 1}H NMR spectroscopy and single-crystal X-ray diffraction. The cadmium atom in the crystal structure of 1 has distorted triangular dodecahedral geometry by coordination of the four nitrogen atoms of L and four oxygen atoms of the two acetate ions. Two water molecules are also incorporated in the crystal network. The O-H···O hydrogen bonds present in the crystal structure of 1. In this work, three structural surveys including coordination numbers of the cadmium atom, coordination modes of L and resonance in pyridine-2-ylmethanimine-based compounds are presented.

  4. 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

  5. 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.

  6. Synthesis, crystal structure and characterization of [C9H11N4] H2PO4

    Science.gov (United States)

    Chtourou, A.; Boujelbene, M.; Allouch, F.; Mhiri, T.

    2014-04-01

    Chemical preparation crystal structure and spectroscopic investigations are given for a new organic-cation dihydrogenomonophosphate (C9H11N4) H2PO4 in the solid state. This compound crystallizes in the monoclinic space group P 21 with the following unit cell parameters: a = 9.640 (5) Ǻ. b = 4.582 (5) Ǻ. c = 14.094 (5) Ǻ, β = 106.979 (5)°, Z = 2, V = 595.4 (7) Å3. Crystal structure was solved with a final R = 0.054 for 2077 independent reflections. The atomic arrangement can be described as inorganic layers of HPO4- anions between which are located the organic groups. Solid-state 13C and 31P MAS-NMR spectroscopies are in agreement with the X-ray structure. Ab initio calculations allow the attribution of the phosphorous and carbon signals to the independent crystallographic sites and to the various atoms of the organic groups.

  7. 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.

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

    Science.gov (United States)

    Khalaji, A. D.; Maddahi, E.; Dusek, M.; Fejfarova, K.; Chow, T. J.

    2015-12-01

    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, 1H-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.

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

    International Nuclear Information System (INIS)

    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, 1H-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

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

    International Nuclear Information System (INIS)

    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

  11. Characterizing protein crystal nucleation

    Science.gov (United States)

    Akella, Sathish V.

    We developed an experimental microfluidic based technique to measure the nucleation rates and successfully applied the technique to measure nucleation rates of lysozyme crystals. The technique involves counting the number of samples which do not have crystals as a function of time. Under the assumption that nucleation is a Poisson process, the fraction of samples with no crystals decays exponentially with the decay constant proportional to nucleation rate and volume of the sample. Since nucleation is a random and rare event, one needs to perform measurements on large number of samples to obtain good statistics. Microfluidics offers the solution of producing large number of samples at minimal material consumption. Hence, we developed a microfluidic method and measured nucleation rates of lysozyme crystals in supersaturated protein drops, each with volume of ˜ 1 nL. Classical Nucleation Theory (CNT) describes the kinetics of nucleation and predicts the functional form of nucleation rate in terms of the thermodynamic quantities involved, such as supersaturation, temperature, etc. We analyzed the measured nucleation rates in the context of CNT and obtained the activation energy and the kinetic pre-factor characterizing the nucleation process. One conclusion is that heterogeneous nucleation dominates crystallization. We report preliminary studies on selective enhancement of nucleation in one of the crystal polymorprhs of lysozyme (spherulite) using amorphous mesoporous bioactive gel-glass te{naomi06, naomi08}, CaO.P 2O5.SiO2 (known as bio-glass) with 2-10 nm pore-size diameter distribution. The pores act as heterogeneous nucleation centers and claimed to enhance the nucleation rates by molecular confinement. The measured kinetic profiles of crystal fraction of spherulites indicate that the crystallization of spherulites may be proceeding via secondary nucleation pathways.

  12. 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: 1.602, year: 2014

  13. Structural characterization of Lu1.8Y0.2SiO5 crystals

    Science.gov (United States)

    Chiriu, Daniele; Faedda, Nicola; Lehmann, Alessandra Geddo; Ricci, Pier Carlo; Anedda, Alberto; Desgreniers, Serge; Fortin, Emery

    2007-08-01

    The structural and vibrational properties of Lu1.8Y0.2SiO5 (LYSO) single crystals were investigated by means of Raman spectroscopy and x-ray diffraction measurements. Unit cell parameters and bond lengths were determined by Rietveld refinement of the collected x-ray diffraction powder spectra. By comparison with the vibrational spectra of the parent compounds Lu2SiO5 and Y2SiO5 and by using polarized Raman measurements, we propose the assignment of the principal vibrational modes of LYSO crystals. The strict connection of Raman spectra of the LYSO solid solution and of the pure lutetium and yttrium crystals, as well as the analysis of the polarized measurements, confirms that LYSO structure adopts the C2/c space group symmetry. The structural analogies of LYSO with the pure compound Lu2SiO5 are further shown by means of high pressure Raman spectroscopy, and the possibility of considering the LYSO crystal analogous to the LSO structure with a tensile stress between 0.25 and 0.80GPa is discussed.

  14. Structural, thermal and optical characterization of an organic NLO material—Benzaldehyde thiosemicarbazone monohydrate single crystals

    Science.gov (United States)

    Santhakumari, R.; Ramamurthi, K.

    2011-02-01

    Single crystals of the organic NLO material, benzaldehyde thiosemicarbazone (BTSC) monohydrate, were grown by slow evaporation method. Solubility of BTSC monohydrate was determined in ethanol at different temperatures. The grown crystals were characterized by single crystal X-ray diffraction analysis to determine the cell parameters and by FT-IR technique to study the presence of the functional groups. Thermogravimetric and differential thermal analyses reveal the thermal stability of the crystal. UV-vis-NIR spectrum shows excellent transmission in the region of 200-1100 nm. Theoretical calculations were carried out to determine the linear optical constants such as extinction coefficient and refractive index. Further the optical nonlinearities of BTSC have been investigated by Z-scan technique with He-Ne laser radiation of wavelength 632.8 nm. Mechanical properties of the grown crystal were studied using Vickers microhardness tester. Second harmonic generation efficiency of the powdered BTSC monohydrate was tested using Nd:YAG laser and it is found to be ˜5.3 times that of potassium dihydrogen orthophosphate.

  15. Crystal structure and characterization of a novel luminescent 2D metal-organic framework, poly[aquaitaconatocalcium(II)] possessing an open framework structure with hydrophobic channels

    Science.gov (United States)

    Nair, Remya M.; Sudarsanakumar, M. R.; Suma, S.; Prathapachandra Kurup, M. R.

    2016-02-01

    A novel 2D metal-organic framework poly[aquaitaconatocalcium(II)] with an open framework structure has been successfully grown by single gel diffusion technique. Sodium metasilicate was used for gel preparation. The structure was determined by single crystal X-ray diffraction. The compound crystallizes in monoclinic space group P21/c with hydrophobic 1D channels. The obtained crystals were further characterized by elemental analysis, FT-IR and UV-Visible spectroscopy, powder X-ray diffraction and thermogravimetry. The luminescent property of the complex was also discussed.

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

    International Nuclear Information System (INIS)

    Dimethyltin dichloride react with 2-ac ethylpyridine benzophenone azine (apba) in refluxing dry hexane to give (SnMe2 Cl2 (apba)) where the azine ligand acts as a bidentate N-N chelating ligand. The complex has been characterized by IR spectroscopy, 1H and 13C 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

  17. Synthesis, Crystal Structure, and Characterization of Ternary Copper(II Complex Derived from N-(salicylidene-L-valine

    Directory of Open Access Journals (Sweden)

    Sundaramurthy Santha Lakshmi

    2016-01-01

    Full Text Available Ternary Schiff base copper(II complex [CuL(tmpda] (where H2L is N-(salicylidene-L-valine; tmpda is N,N,N′,N′-tetramethyl-1,3-propanediamine has been characterized by UV-Vis., FTIR, and single crystal XRD. The crystal structure displays a distorted square pyramidal geometry in which Schiff base is bonded to the Cu(II ion via phenolate oxygen, imine nitrogen, and an oxygen atom of the carboxylate group through the basal plane and the chelating diamine, N,N,N′,N′-tetramethyl-1,3-propanediamine, displays an axial and equatorial mode of binding via NN-donor atoms.

  18. Synthesis, structure, thermal and NLO characterization of 4-hydroxy tetramethylpiperazinium picrate crystals

    Indian Academy of Sciences (India)

    T Dhanabal; G Amirthaganesan; M Dhandapani; Samar K Das

    2012-07-01

    Good quality single crystals of 4-hydroxy tetramethylpiperazinium picrate (TMPP) were grown by slow evaporation solution growth method at room temperature. The average dimensions of the grown crystals were 0.6 × 0.2 × 0.2 cm3. The solubility of the compound was estimated using methanol and acetone. The elemental analysis confirms the formation of the compound in the stoichiometric proportion. The UV-visible transmittance study indicates that the crystal possesses minimum transmittance at 370 nm and no absorption at 470-900 nm. The Bragg peaks obtained in the powder X-ray diffraction pattern confirm its crystallinity. The thermal behaviour of the crystal was investigated using thermogravimetric (TG) and differential thermal analysis (DTA) techniques. The structure of the compound was determined by using single crystal X-ray diffraction method. The compound was found to be crystallize in the monoclinic space group P2(1)/c (a = 6.9513(8)Å, b = 11.8016(14)Å, c = 22.018(2)Å, = 90.00°, = 92.575(2)°, = 90.00°). The thermal anomalies observed in the differential scanning calorimetry (DSC) heating and cooling cycles indicate the occurrence of first order phase transition. Fourier transform infrared (FTIR) and polarized Raman spectral analyses were used to confirm the presence of various functional groups in the compound. The nonlinear optical property (NLO) of the crystal was analysed by Kurtz-Perry powder technique and found that the compound has SHG efficiency 1.5 times greater that of potassium dihydrogen phosphate (KDP).

  19. Synthesis, crystal structure, spectral characterization and fluorescence studies of salts of α-mangostin with APIs

    Science.gov (United States)

    Satyanarayana Reddy, J.; Ravikumar, N.; Gaddamanugu, Gopikrishna; Naresh, K. N.; Rajan, S. S.; Anand Solomon, K.

    2013-05-01

    α-Mangostin is a naturally occurring oxygenated xanthonoid isolated from the mangosteen tree (Garcinia mangostana). We report the molecular salts of α-mangostin with the active pharmaceutical ingredients (APIs) metformin (anti-diabetic) and piperazine (anti-helminthic) obtained by solvent assisted grinding method as well as solution crystallization method based on the ΔpKa criterion. The synergistic pharmaceutically active α-mangostin-metformin molecular salt and α-mangostin-hemipiperazine ethanol solvate were characterized by the single crystal X-ray diffraction (SCXRD), vibrational spectroscopy (FT-IR) and differential scanning calorimetry (DSC). The fluorescence properties of the molecular salts are obtained by fluorescence spectroscopy. The molecules in both the crystal forms are stabilized by N+sbnd H⋯N, Osbnd H⋯O-, N+sbnd H⋯O and N+sbnd H⋯O-, Osbnd H⋯O hydrogen bonding interactions. In the FT-IR spectra characteristic peaks are observed for the protonated amine (sbnd NH2+) group piperazinium dication (sbnd NH+) respectively indicating formation salts.

  20. A new strontium antimonateIII Sr5Sb22O38: Synthesis, crystal structure and characterizations

    International Nuclear Information System (INIS)

    A new strontium antimonateIII, Sr5Sb22O38, has been hydrothermally synthesized and structurally characterized by single crystal X-ray diffraction. It crystallizes in the P21/n space group of the monoclinic system with a=11.739(9) Å, b=12.014(10) Å, c=16.412(13) Å, β=91.460(8)°, V=2314.0(3) Å3. The crystal structure is built of seven trigonal–pyramidal SbO3 and four sphenoid SbO4 polyhedra which are connected through sharing corner-oxygen atoms to form the complex three-dimensional ∞3[Sb22O38]10− anionic network with two different intersectant tunnels along the [111-bar ] and [11-bar 1-bar ] directions accommodating the electric charge balanced Sr2+ cations. First-principles electronic structure calculations based on the density functional theory (DFT) and the UV–vis diffuse reflectance spectroscopy measurements both indicate that the compound belongs to a direct band insulator with an optical gap value of 3.3 eV. - Graphical abstract: The 2D Sb–O slabs are stacked through sharing oxygen atoms to form the 3D network structure of the new strontium antimonateIII Sr5Sb22O38. - Highlights: • A new strontium antimonateIII, Sr5Sb22O38, has been hydrothermally synthesized. • The single crystal structure was determined by X-ray diffraction. • The powder XRD and UV–vis absorption spectroscopy were studied. • Theoretical studies interpret the relationships between optical absorption and crystal structure

  1. Synthesis, crystal structures, spectroscopic characterization and in vitro antidiabetic studies of new Schiff base Copper(II) complexes

    Indian Academy of Sciences (India)

    SUNDARAMURTHY SANTHA LAKSHMI; KANNAPPAN GEETHA; M GAYATHRI; GANESH SHANMUGAM

    2016-07-01

    Two new Schiff base copper(II) complexes, [CuL¹(tmen)] (1) and [Cu₂L₂² (tmen)] (2) {where, H₂L¹ = N-(salicylidene)-L-valine, H₂L² = N-(3,5-dichlorosalicylidene)-L-valine and tmen = N,N,N',N'- tetramethylethylene-1,2-diamine} have been synthesized and characterized by molar conductance, elemental analyses, VSM-RT, UV-Vis, FTIR, EPR, and CD spectra. Both the complexes were structurally characterized by single crystal XRD. The crystal structure of complex 1 displays a distorted square pyramidal geometry in which Schiff base is coordinated to the Cu(II) ion via ONO-donor in the axial mode, whereas, the chelating diamine displays axial and equatorial mode of binding via NN-donor atoms. The crystal structure of the complex 2 reveals a syn-anti mode of carboxylate bridged dinuclear complex, in which, the coordination geometry around Cu(1) is square pyramid and distorted square planar around Cu(2). The target complexes were screened for in vitro antidiabetic activity. Both the complexes showed good inhibitory activity for α-amylase and α-glucosidase.

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

    OpenAIRE

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

    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 ...

  3. Synthesis, Crystal Structures and Characterization of Ba5LiTiNb9O30

    Institute of Scientific and Technical Information of China (English)

    LIU,Han-Xing(刘韩星); ZOU,Long(邹龙); ZHOU,Jian(周建); FANG,Liang(方亮); ZHANG,Gao-Ke(张高科); OUYANG,Shi-Xi(欧阳世翕)

    2004-01-01

    A new niobate compound with the chemical composition of Ba5LiTiNb9O30 was synthesized by doping Li+ into the system BaO-TiO2-Nb2O5 in conventional solid state reaction method.The crystalline structure was determined by X-ray diffraction analysis (XRD).The results showed that crystal structure of Ba5LiTiNb9O30 belongs to tetragonal tungsten bronze structure with space group P4bn and its unit cell parameters:a=b=l.2512(2) nm,c=0.4008(5) nm.The microstructure of reaction products was observed by scanning electron microscopy (SEM).

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

    International Nuclear Information System (INIS)

    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. - 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 [NH2(CH2)4NH][BF4], phase IV. The dashed lines stand for the hydrogen bonds. The hydrogen bonds to BF4 groups are not included for the picture quality Highlights:

  5. Synthesis, characterization, and crystal structure of 2-iodo-3,4,5-trimethoxybenzoic acid

    Science.gov (United States)

    Kolev, Iliyan N.; Petrova, Svetlana P.; Nikolova, Rositsa P.; Dimowa, Louiza T.; Shivachev, Boris L.

    2013-02-01

    This work describes the synthesis of 2-iodo-3,4,5-trimethoxybenzoic acid. The combination of iodine and silver trifluoroacetate (AgTFA) reagents was used successfully for the iodination of 3,4,5-trimetoxybenzoic acid. To improve the efficiency of the synthetic process a significant modification on the experimental design was also performed. The main structural features of the obtained aryl iodide were investigated by a single crystal X-ray diffraction analysis, FTIR, 1H and 13C NMR spectroscopy.

  6. Three new bismuth(III) pyridine-2,6-dicarboxylate compounds: Synthesis, characterization and crystal structures

    Science.gov (United States)

    Hakimi, Mohammad; Motieiyan, Elham; Bertolotti, Federica; Marabello, Domenica; Nunes Rodrigues, Vitor Hugo

    2015-11-01

    Three new metal-organic compounds containing bismuth and pyridine-2,6-dicarboxylate (pydc) formulated as (2-apyH)2[Bi(pydc)2(pydcH)]·2H2O, 1, (4-apyH)[Bi(pydc) (pydcH)2].4H2O, 2 and (pipzeaH)[Bi2(pydc)3(pydcH) (H2O)2]·5H2O, 3, (2-apy = 2-aminopyridine, 4-apy = 4-aminopyridine, pipzea = 2-piperazin-1-ylethanamine), have been synthesized in deionized water and characterized by elemental analysis (C, H and N), spectral (UV-Vis, IR), 1H NMR spectroscopy, TGA and single crystal X-ray diffraction. These compounds were obtained via proton transfer methodology. Compounds 1 and 2 have similar monomeric bismuth coordination units, whereas compound 3 has a dimeric bismuth coordination unit. The compounds are anionic in 1 and 2 and they are connected non-covalently to 2-apyH and 4-apyH, respectively. In 3, two molecules are present, one neutral and one anionic, and both are connected non-covalently to pipzeaH cations. Five different coordination modes of Bi-pydc exist in 1, 2 and 3. These compounds are stabilized in the solid state by a complex network of hydrogen bonds between crystallization water molecules, anionic, cationic and neutral fragments, forming 3D-supramolecular arrays.

  7. Synthesis, characterization and crystal structure of 1-ferrocenesulfonyl-2-1ong carbon chain alkyl benzimidazole

    Institute of Scientific and Technical Information of China (English)

    Junzhen ZHANG; Bingqin YANG; Yating YANG; Binglin ZHANG

    2009-01-01

    Six new 1-ferrocenesulfonyl-2-benzimidazole derivatives were prepared by the reaction of ferrocene-sulfonyl chloride with benzimidazole derivatives in the presence of dichloromethane and n-tetrabutylammonia bromide. The yields of these six new ferrocenesulfonyl benzimidazole derivatives were about 80%. The structures characteristic were confirmed by IR, 1H-NMR, Elemental analysis and MS. The crystal structure of compound a2 was determined via X-ray single crystal diffraction and it belongs to monoclinic system with space group C2/c,and the unit cell parameters are a=2.8252(2)nm, b=0.97696(7)nm, c=1.64828(12)nm, a=90°, β=92.053(2)°,y = 90°, V= 4.5466(6) nm3, Z= 8, F(000) =2024, Mr=481.40, Dc=l.407g/cm3, μ=0.784mm-1,R1=0.0495, wR2=0.1517. The results show that the reactions of 2-alkylbenzimidazoles containing active hydrogen with ferrocenesulfonyl chloride gave 1-ferrocenesulfonyl-2-alkylbenzimidazoles in good yields.

  8. Crystal Structure and Biochemical Characterization of Tetrahydrodipicolinate N-Succinyltransferase from Corynebacterium glutamicum.

    Science.gov (United States)

    Sagong, Hye-Young; Kim, Kyung-Jin

    2015-12-16

    Tetrahydrodipicolinate N-succinyltransferase (DapD) is an enzyme involved in the biosynthesis of l-lysine by converting tetrahydrodipicolinate into N-succinyl-l-2-amino-6-oxopimelate, using succinyl-CoA as a cofactor. We determined the crystal structure of DapD from Corynebacterium glutamicum (CgDapD). CgDapD functions as a trimer, and each monomer consists of three domains: an N-terminal helical domain (NTD), a left-handed β-helix (LβH) domain, and a β C-terminal domain (CTD). The mode of cofactor binding to CgDapD, elucidated by determining the structure in complex with succinyl-CoA, reveals that the position of the CTD changes slightly as the cofactor binds to the enzyme. The superposition of this structure with that of Mycobacterium tuberculosis shows differences in residues that make up cofactor-binding sites. Moreover, we determined the structure of CgDapD in complex with the substrate analogue 2-aminopimelate and revealed that the analogue was stabilized by conserved residues. The catalytic and substrate binding sites of CgDapD were confirmed by site-directed mutagenesis experiments. PMID:26602189

  9. Syntheses, characterization and crystal structures of potassium and barium complexes of a Schiff base ligand with different anions

    Indian Academy of Sciences (India)

    Bhavesh Parmar; Kamal Kumar Bisht; Pratyush Maiti; Parimal Paul; Eringathodi Suresh

    2014-09-01

    New pseudopolymorph of a O,N,N′-donor hydrazone ligand, 2-pyridylcarboxaldehyde isonicotinoylhydrazone (L) and its discrete complexes with K+ and Ba2+ have been reported. L forms isostructural dinuclear complexes with K+ when bromide and iodide were employed as counter anions. However, a monomeric complex in the case of Ba2+ with existence of coordinated as well as lattice perchlorate counter anions was observed. All compounds were characterized by single crystal X-ray analysis and other physicochemical techniques. Structural analysis and spectral features of all compounds are described in detail.

  10. Structural characterization of wavelength-dependent Raman scattering and laser-induced crystallization of silicon thin films

    International Nuclear Information System (INIS)

    In this report, we present a detailed structural characterization of hydrogenated amorphous silicon (a-Si:H) and microcrystalline silicon (μc-Si:H) thin films grown using high working pressure plasma-enhanced chemical vapor deposition. It is shown that the volumetric crystalline fraction of deposited μc-Si:H thin films measured by Raman scattering differs significantly for three different excitation laser wavelengths (514.5, 632.8, and 785.0 nm) owing to differences in penetration depth due to absorption, and optical confocal depth. The results demonstrate that selection of the correct excitation wavelength for Raman experiments is a highly important factor for gaining an accurate understanding of the relationship between internal microstructures and solar cell performance. In addition, the use of a high power laser was found to induce the crystallization of a-Si:H thin films due to local sample heating during the Raman measurements, which was characterized by the appearance of a sharp peak around 500 cm−1. It was found that both photon energy (laser wavelength) and photon flux (laser power) were important factors in inducing crystallization of the films. - Highlights: • We present wavelength-dependent Raman scattering of silicon thin films. • Thin films were grown by using high working pressure PECVD. • The crystallinity of deposited thin films was measured by Raman scattering. • The crystallinity differs significantly for three different excitation wavelengths. • Photon energy is an important factor in inducing crystallization of the films

  11. Crystal structure, spectroscopy, DFT studies and thermal characterization of Cobalt(II) complex with 2-protonated aminopyridinium cation as ligand

    Science.gov (United States)

    Mhadhbi, Noureddine; Saïd, Salem; Elleuch, Slim; Naïli, Houcine

    2016-03-01

    Single crystals of a new organic-inorganic hybrid compound (2-HAMP)2[CoBr4], (2-HAMP = 2-protonated aminopyridinium cation) was synthesized and characterized by X-Ray diffraction at room temperature, DTA-TG measurement, FT-IR and FT-Raman spectroscopies and optical absorption. Its crystal structure is a packing of alternated organic and inorganic layers parallel to (a, b) plane. The different components are connected by a network of N/C-H⋯Br hydrogen bonds and halogen⋯halogen interactions. These hydrogen bonds give notable vibrational effects. Theoretical calculations were performed using density functional theory (DFT) for studying the molecular structure, vibrational spectra and optical properties of the investigated molecule in the ground state. The optimized geometrical parameters obtained by DFT calculations are in good agreement with single crystal XRD data. The energy and oscillator strength calculated by Time-Dependent Density Functional Theory (TD-DFT) results complements with the experimental findings. The simulated spectra satisfactorily coincide with the experimental UV-Visible spectrum. The results show good consistent with the experiment and confirm the contribution of metal orbital to the HOMO-LUMO boundary. Thermal analysis studies indicate the presence of three phase transitions at 68, 125 and 172 °C, which are confirmed by X-ray powder diffraction as a function of temperature.

  12. 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

  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

    2016-04-01

    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.

  14. Crystal structure and characterization of a novel ferroelastic ionic crystal: 1-Aminopyridinium iodide (C5H7N2)+I-

    Science.gov (United States)

    Owczarek, M.; Jakubas, R.; Kinzhybalo, V.; Medycki, W.; Kruk, D.; Pietraszko, A.; Gałazka, M.; Zieliński, P.

    2012-06-01

    1-Aminopyridinium iodide (API) undergoes a reversible first-order phase transition (PT) II → I at 384 K. The single-crystal X-ray diffraction studies have been carried out at 110, 280 and 401 K. The compound crystallizes in the monoclinic space group P21/c (phase II) and exhibits ferroelastic properties. High temperature paraelastic phase (I) is described by the trigonal symmetry (space group R3¯m) with the 6-site cations disorder. The mechanism of PT is governed by both cationic dynamics and shifts of the I- anions. The conductivity that emerges when approaching the PT temperature is believed to be associated with the charge transfer from I- anion to the 1-aminopyridinium cation.

  15. Synthesis, Crystal Structure, and Characterization of a New Organic-Inorganic Hybrid Material:

    OpenAIRE

    Hela Ferjani; Habib Boughzala; Ahmed Driss

    2013-01-01

    The title compound is an organic-inorganic hybrid material. The single crystal X-ray diffraction investigation reveals that the studied compound crystallizes in the orthorhombic system, space group Pbca with the following lattice parameters:  (4) Å,  (3) Å,  (6) Å, and . The crystal lattice is composed of a discrete anion surrounded by piperazinium cations, chlorine anions, and water molecules. Complex hydrogen bonding interactions between , , organic cations, and water molecules form a three...

  16. Novel Lanthanide Complexes of Ciprofloxacin: Synthesis, Characterization, Crystal Structure and in vitro Antibacterial Activity Studies

    Institute of Scientific and Technical Information of China (English)

    LI,Jia-Bin; YANG,Pin; GAO,Fei; HAN,Gao-Yi; YU,Kai-Bei

    2001-01-01

    Novel lanthanide coordinatlon compounds with ciprofloxacin (CPFX), including eleven complexes Ln(CPFX)2Cl(H2O)n (Ln= Pr,Nd,Sm,Eu,Gd,To,Dy,Ho,Er,Tm, Yb; n =7,8, 9) and crystalline [Ce(CPFX)2(H2O)4]Cl· (H2O)3.25(C2H5- OH)0.25, were synthesized. The crystal is of triclinic space group Pi with a= 1.3865(2) nm, b = 1.3899(3) nm, c = 1.6505(2) nm, α= 92.73(1)°, β= 114.39(1)°, γ= 115.55 (1)°, Z = 2 and R = 0.0449.FT-IR, electronic spectroscopy and X-ray diffraction were employed to show that the lan thanide ion, which displays an eight-coordinate structure, is chelated by 3-carboxyl and 4-keto oxygen donors of CPFX and two six- membered chelate rings are formed. Test of in vitro antibacterial activity against E. coli, P. aeruginosa and S. aureus indicated that the in vitro antibacterial activity of the ligand can be improved by complexation with Ce(Ⅲ).

  17. cis-Dioxomolybdenum(VI) complexes of a new ONN chelating thiosemicarbazidato ligand; Synthesis, characterization, crystal, molecular structures and antioxidant activities

    Science.gov (United States)

    İlhan Ceylan, Berat; Deniz, Nahide Gulsah; Kahraman, Sibel; Ulkuseven, Bahri

    2015-04-01

    5-Chloro-4-methyl-2-hydroxybenzophenone S-propyl-4-phenyl-thiosemicarbazone (H2L) and its cis-dioxomolybdenum(VI) complexes, in the general formula [MoO2(L)R-OH)] (R: methyl, 1; ethyl, 2; n-propyl, 3; n-butyl, 4; n-pentyl, 5), were synthesized and characterized by micro analysis, electronic, infrared and 1H and 13C NMR spectra. The crystal structures of complexes, 1 and 3, have been solved by direct methods (SIR92) and refined to the residual indexes R1 = 0.098 and R1 = 0.052 respectively. Complexes 1 and 3 are crystallized in the triclinic space group P-1 with Z = 2. The crystal study of complex 1 showed the first example of intermolecular hydrogen bond for this type of molybdenum-thiosemicarbazone complexes. The hydrogen bond is between the hydroxyl proton of attached alcohol and an oxo oxygen (in MoO22+ unit) of another complex molecule, and its bond distance (1.767(1) Å) is shorter than from the σ-coordination bonds in complex 1. Antioxidant activities of the compounds were determined by using 1,1-diphenyl-2-picrylhydrazyl (DPPH) method. Ligand showed 23.61% DPPH radical scavenging activity at 250 mg/L concentration. Cupric Reducing Antioxidant Capacity (CUPRAC) was also evaluated and trolox-equivalent antioxidant capacity (TEAC) values were found for ligand, 1 and 3 as 0.51, 0.33 and 0.30 respectively.

  18. Synthesis, crystal structure, spectral characterization and biological exploration of water soluble Cu(II) complexes of vitamin B6 derivative.

    Science.gov (United States)

    Annaraj, B; Neelakantan, M A

    2015-09-18

    The synthesis and characterization of Copper(II) complexes of a Schiff base derived from vitamin B6 component (pyridoxal) and ethanol amine [CuL2] (1), and its mixed ligand complexes [Cu(L)(N,N')]NO3, where N,N' is bipyridine (2) and 1,10-phenanthroline (3) are reported, including the X-ray crystal structures of [CuL2] (1). The crystal structure of 1 has square planar geometry with ligand to the metal ratio 2:1. The molecules are assembled in 3D supramolecular structure through hydrogen bonding interactions. DNA is considered as the major pharmacological target of metal based drugs, the objective of the present work includes the understanding of DNA binding mode of the synthesized compounds. The complexes bind with DNA through non intercalative interaction has been evidenced from the results of UV-Visible and fluorescence spectral titrations. It is further validated by molecular docking studies. Bovine serum albumin (BSA) binding studies revealed that the complexes can strongly quench the intrinsic fluorescence of BSA through a static quenching mechanism. The complexes promote the DNA cleavage even in the absence of additives which follows the order 2 > 1 > 3. Further, the complexes show potential cytotoxicity towards human breast cancer cell MCF-7 and induce the cell death. PMID:26241872

  19. Crystal growth, structure and characterizations of a new semiorganic nonlinear optical material-β-Alanine zinc chloride

    International Nuclear Information System (INIS)

    The title compound, β-alanine zinc chloride-a new semiorganic nonlinear optical crystal was grown by slow evaporation technique. Single crystals of β-alanine zinc chloride have been subjected to X-ray diffraction analysis to determine the crystal structure. The powder X-ray diffractogram of the crystal has also been recorded. The amount of carbon, nitrogen and hydrogen in the crystals was also estimated. Fourier Transform Infrared and Raman spectral measurements have been carried out on the grown crystals in order to identify the functional groups. The presence of hydrogen and carbon in the β-alanine zinc chloride was confirmed by using proton and carbon nuclear magnetic resonance spectral analyses. The percentage of zinc in the crystal was determined by atomic absorption spectroscopy. Optical behavior such as ultraviolet-vis-near infrared transmittance spectrum and second harmonic generation has been investigated. The mechanical strength and thermal behavior of the grown crystal have been analyzed.

  20. Synthesis and structural characterization of Na2MnP2O7 crystal

    Indian Academy of Sciences (India)

    N K Lokanath; M A Sridhar; J Shashidhara Prasad; G S Gopalakrishna; K G Ashamanjari

    2000-06-01

    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, $\\bar{1}$, = 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, = 2, ρcal = 2, 3.121 g/cm3, = 3.121 mm–1, 000 = 244, goodness-of-fit on = 1.348, final indices with [ > 3()] = 0.051 and = 0.065.

  1. Synthesis of two new azo-azomethines; spectral characterization, crystal structures, computational and fluorescence studies

    Science.gov (United States)

    Eskikanbur, Sevgi; Sayin, Koray; Kose, Muhammet; Zengin, Huseyin; McKee, Vickie; Kurtoglu, Mukerrem

    2015-08-01

    This study describes the preparation, characterization and the photoluminescence properties of novel azo-azomethines (2-{(E)-[(4-ethylphenyl)imino]methyl}-4-[(E)-phenyldiazenyl]phenol, HL1 and 2-{(E)-[(3-ethylphenyl)imino]methyl}-4-[(E)-phenyldiazenyl]phenol, HL2 dyes). The dyes were characterized by elemental analysis, spectroscopic studies such as IR, 1H and 13C NMR, mass and fluorescence spectra. Molecular structures of the dyes were examined by X-ray diffraction analysis. The molecular structures are mostly similar, differing mainly in the position of the ethyl group and dihedral angles between aromatic rings. X-ray data revealed that both HL1 and HL2 favor phenol-imine tautomer in the solid state. An intramolecular phenol-imine hydrogen bond (O1⋯N1) were observed in both compounds resulting in a S(6) hydrogen bonding motif. Molecular packing of both compounds are determined by π⋯π interactions. Quantum chemical investigation of mentioned molecules were performed by using DFT hybrid function (B3LYP) with 6-31+G(d) basis set. The compounds HL1 and HL1 gave intense light emissions upon irradiation by Ultra-Violet light. The photoluminescence quantum yields and long excited-state lifetimes of the compounds HL1 and HL2 were measured. The azo-azomethine dyes HL1 and HL2 have photoluminescence quantum yields of 34% and 32% and excited-state lifetimes of 3.21 and 2.98 ns, respectively. The photoluminescence intensities and quantum yields of these dyes were dependent on the position of alkyl group on the phenyl ring.

  2. 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.

  3. Incommensurability in crystal structures

    International Nuclear Information System (INIS)

    Incommensurate or modulated crystal structures (TaS2, Srsub(1-p)Cr2Sesub(4-p), etc.) are examined and compared with superstructures (TaSe2, Basub(1-p)Cr2Sesub(4-p)). Observed and calculated structure factors are given for Eusub(1-p)Cr2Sesub(4-p). (C.F.)

  4. Crystal structure, complexation, spectroscopic characterization and antimicrobial evaluation of 3,4-dihydroxybenzylidene isonicotinyl-hydrazone

    Science.gov (United States)

    Jeragh, Bakir; Ali, Mayada S.; El-Asmy, Ahmed A.

    2015-06-01

    A single crystal of 3,4-dihydroxybenzylidene isonicotinylhydrazone, HBINH, has been grown and solved by X-ray crystallography. The VO2+, Zr4+, Co2+, Ni2+, Cu2+, Zn2+, Cd2+, Hg2+ and Pd2+ complexes of HBINH have been prepared and spectroscopically characterized. The data confirmed the formulae [Co(HBINH)(H2O)Cl]Cl·H2O, [Pd(HBINH)Cl2], [Zn(HBINH)2Cl2], [Cd(HBINH)(H2O)2Cl2]·1½H2O, [(VO)2(HBINH-3H)(OH)(H2O)], [Ni2(HBINH)(H2O)6Cl2]Cl2, [Cu2(HBINH-3H)(H2O)2(OAc)]·3H2O, [Zr2(HBINH-3H)Cl4]Cl, [Hg2(HBINH)Cl4] and the dimer {[Cu(HBINH)Cl]Cl}2. Most of the complexes have intense colors and high melting points and some are electrolytes in DMSO solution. The ligand behaves as a neutral bidentate in the Co(II), Cu(II), Pd(II), Zn(II) and Cd(II) complexes; dibasic tetradentate in [Ni2(HBINH)(H2O)6Cl2]Cl2 and tribasic tetradentate in [Cu2(HBINH-3H)(OAc)]·5H2O, [(VO)2(HBINH-3H)(OH)(H2O)] and [Zr2(HBINH-3H)Cl4]Cl by the loss of 3H+ due to the deprotonation of the two hydroxyl groups and the enolization of the amide (Odbnd CNH) group. A tetrahedral geometry was proposed for the Co(II), Cu(II), Zn(II) and Hg(II) complexes; square-planar for the Pd(II) complex; square-pyramid for the VO2+ complex and octahedral for the Ni(II) and Cd(II) complexes. The complexes [Cd(HBINH)(H2O)2Cl2]·1½H2O, [(VO)2(HBINH-3H)(OH)(H2O)] and [Cu2(HBINH-3H)-(H2O)2(OAc)]·3H2O have activities against Bacillus sp. M3010, Candida albicans, Escherichia coli, Staphylococcus aureus and Slamonella sp. PA393.

  5. Photonic Crystal Laser Accelerator Structures

    OpenAIRE

    Cowan, Benjamin; Javanmard, Mehdi; Siemann, Robert H.

    2003-01-01

    Photonic crystals have great potential for use as laser-driven accelerator structures. A photonic crystal is a dielectric structure arranged in a periodic geometry. Like a crystalline solid with its electronic band structure, the modes of a photonic crystal lie in a set of allowed photonic bands. Similarly, it is possible for a photonic crystal to exhibit one or more photonic band gaps, with frequencies in the gap unable to propagate in the crystal. Thus photonic crystals can confine an optic...

  6. Studies on bulk growth, structural and microstructural characterization of 4-aminobenzophenone single crystal grown from vertical Bridgman technique

    Indian Academy of Sciences (India)

    S P Prabhakaran; R Ramesh Babu; G Bhagavannarayana; K Ramamurthi

    2014-02-01

    Bulk single crystal of 4-aminobenzophenone with a size of 25 mm dia. and 35 mm length has been grown by vertical Bridgman technique. The crystal system of the grown crystal was confirmed by X-ray diffraction analysis. Crystalline perfection was analysed by high resolution X-ray diffraction studies. Chemical etching was carried out for the first time in 4-aminobenzophenone single crystal to study the defects presented in the grown crystal and the growth mechanism involved. Several organic etchants were employed with different etching time to select suitable etchant for studying dislocation pattern and other structural defects existing in the grown crystal. Etch patterns such as spirals and striations observed for the selective etchants provide considerable information on growth mechanism of the crystal.

  7. 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 this is...

  8. cis-Dioxomolybdenum(VI) complexes of a new ONN chelating thiosemicarbazidato ligand; synthesis, characterization, crystal, molecular structures and antioxidant activities.

    Science.gov (United States)

    İlhan Ceylan, Berat; Deniz, Nahide Gulsah; Kahraman, Sibel; Ulkuseven, Bahri

    2015-04-15

    5-Chloro-4-methyl-2-hydroxybenzophenone S-propyl-4-phenyl-thiosemicarbazone (H2L) and its cis-dioxomolybdenum(VI) complexes, in the general formula [MoO2(L)R-OH)] (R: methyl, 1; ethyl, 2; n-propyl, 3; n-butyl, 4; n-pentyl, 5), were synthesized and characterized by micro analysis, electronic, infrared and (1)H and (13)C NMR spectra. The crystal structures of complexes, 1 and 3, have been solved by direct methods (SIR92) and refined to the residual indexes R1=0.098 and R1=0.052 respectively. Complexes 1 and 3 are crystallized in the triclinic space group P-1 with Z=2. The crystal study of complex 1 showed the first example of intermolecular hydrogen bond for this type of molybdenum-thiosemicarbazone complexes. The hydrogen bond is between the hydroxyl proton of attached alcohol and an oxo oxygen (in MoO2(2+) unit) of another complex molecule, and its bond distance (1.767(1)Å) is shorter than from the σ-coordination bonds in complex 1. Antioxidant activities of the compounds were determined by using 1,1-diphenyl-2-picrylhydrazyl (DPPH) method. Ligand showed 23.61% DPPH radical scavenging activity at 250 mg/L concentration. Cupric Reducing Antioxidant Capacity (CUPRAC) was also evaluated and trolox-equivalent antioxidant capacity (TEAC) values were found for ligand, 1 and 3 as 0.51, 0.33 and 0.30 respectively. PMID:25681810

  9. CALYPSO: a method for crystal structure prediction

    OpenAIRE

    Wang, Yanchao; Lv, Jian; Zhu, Li; Ma, Yanming

    2012-01-01

    We have developed a software package CALYPSO (Crystal structure AnaLYsis by Particle Swarm Optimization) to predict the energetically stable/metastable crystal structures of materials at given chemical compositions and external conditions (e.g., pressure). The CALYPSO method is based on several major techniques (e.g. particle-swarm optimization algorithm, symmetry constraints on structural generation, bond characterization matrix on elimination of similar structures, partial random structures...

  10. 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.

  11. Synthesis, characterization, and crystal structure of sulfonamide chalcone: ( E)-4-methoxy- N-(4-(3-(3,4,5-trimethoxyphenyl)acryloyl)phenyl)-benzenesulfonamide

    Science.gov (United States)

    Kobkeatthawin, T.; Chantrapromma, S.; Chidan Kumar, C. S.; Fun, H.-K.

    2015-12-01

    The title sulfonamide chalcone derivative was synthesized by condensation reaction of N-(4-acetylphenyl)-4-methoxybenzenesulfonamide and 3,4,5-trimethoxybenzaldehyde in basic solution. The structure was determined using FT-IR, 1H-NMR and UV-Vis spectroscopy. The crystal structure was characterized by single crystal X-ray structure analysis: triclinic system, sp. gr. P overline 1, Z = 2; a = 7.9273(5), b = 9.3159(6), c = 18.0174(12) Å, α = 94.6420(18)°, β = 93.0310(17)°, γ = 114.9200(15)°. In crystal packing, the molecules are linked by N-H···O hydrogen bonds into chains along the [100] direction. The crystal is further stabilized by weak C-H···O and C-H···π interactions.

  12. Growth, structural and optical characterization of L-histidine 4-nitrophenolate (LHPNP) single crystals for NLO applications

    Energy Technology Data Exchange (ETDEWEB)

    Mahadevan, M., E-mail: devanphysics@gmail.com [Department of Physics, Adhiparasakthi Engineering College, Melmaruvathur - 603319 (India); Ramachandran, K., E-mail: ramach76@yahoo.com [Department of Physics, SRM University - Vadapalani Campus, Chennai -600026 (India); Anandan, P., E-mail: anandantcet@gmail.com [Department of Physics, Thiruvalluvar College of Engineering and Technology, Vandavasi-604 505, India and Research Institute of Electronics, Shizuoka University, 3-5-1 Johoku, Naka-Ku, Hamamatsu 432-8011 (Japan); Arivanandhan, M., E-mail: arivucz@gmail.com, E-mail: royhaya@ipc.shizuoka.ac.jp; Hayakawa, Y., E-mail: arivucz@gmail.com, E-mail: royhaya@ipc.shizuoka.ac.jp [Research Institute of Electronics, Shizuoka University, 3-5-1 Johoku, Naka-Ku, Hamamatsu 432-8011 (Japan)

    2014-10-15

    Using slow evaporation solution growth technique, single crystals of L-histidine-4-nitro phenolate has been grown from the solution. Structural analyses were carried out by powder x-ray diffraction, FT-Raman, Fourier Transform Infrared and Nuclear Magnetic Resonance spectral methods to conform the grown crystals. Thermal stability of the grown crystals was studied by thermo-gravimetric (TG) and differential thermal analyses (DTA). UV-Vis spectral analysis has been carried out to find the transparency of the grown crystal. Nonlinear optical property has been confirmed by Kurtz powder technique. The PL measurements were carried out in Perkin Elmer LS 55 Luminescence spectrometer using 410 nm as excitation wavelength. The observed properties have confirmed that the grown crystal is suitable for nonlinear optical applications.

  13. Growth of NBT-BT single crystals by flux method and their structural, morphological and electrical characterizations

    Science.gov (United States)

    Kanuru, Sreenadha Rao; Baskar, K.; Dhanasekaran, R.; Kumar, Binay

    2016-05-01

    In this paper, one of the important, eco-friendly polycrystalline material, (1-x)(Na0.5Bi0.5)TiO3 (NBT) - xBaTiO3 (BT) of different compositions (x=0.07, 0.06 and 0.05 wt%) around the morphotropic phase boundary (MPB) were synthesized by solid state reaction technique. And the single crystals with 13×7×7 mm3, 12×12×7 mm3 and 10×7×4 mm3 dimensions were grown by self flux method. The morphology, crystal structure and unit-cell parameters have been studied and the monoclinic phase has been identified for 0.07 wt% of BT. Higher BT concentration changes the crystal habit and the mechanism has been studied clearly. Raman spectroscopy at room-temperature confirms the presence of functional groups. The quality of the as grown single crystals was examined by high resolution x-ray diffraction analysis. The dielectric properties of the as grown crystals were investigated in the frequency range of 20 Hz-2 MHz from room temperature to 450 °C. The broad dielectric peak and frequency dispersion demonstrates the relaxor behavior of grown crystals. The dielectric constant (εr), transition temperature (Tm), and depolarization temperature (Td) of the grown crystals are found to be comparatively good. The diffusive factor (γ) from Curie-Weiss law confirms the as grown NBT-BT single crystals are relaxor in nature.

  14. Electron diffraction tomography and dynamical refinement for crystal-structure characterization of nanocrystalline materials

    Czech Academy of Sciences Publication Activity Database

    Correa, Cinthia Antunes; Klementová, Mariana; Palatinus, Lukáš

    Warsaw : Polish Academy of Sciences, 2015, s. 651-653. ISSN 0587-4246. [International Symposium on Physics of Materials /13./. Praha (CZ), 31.08.2014-04.09.2014] R&D Projects: GA ČR GA13-25747S Institutional support: RVO:68378271 Keywords : dynamical diffraction * nanocrystal * structure analysis Subject RIV: BM - Solid Matter Physics ; Magnetism

  15. Syntheses, crystal structures and characterizations of two new bismuth(III) arsenites

    International Nuclear Information System (INIS)

    Two new bismuth arsenites with two different structural types, namely, Bi2O(AsO3)Cl (1), Bi8O6(AsO3)2(AsO4)2 (2), have been synthesized by the solid-state reactions. Compound 1 exhibits novel 2D bismuth arsenite layers with Bi4O4 rings capped by oxide anions, which are further interconnected by Bi–Cl–Bi bridges into a 3D network. Compound 2 contains both arsenite and arsenate anions, its 3D structures are based on 1D bismuth arsenite and 1D bismuth arsenate chains both along b-axis, which are interconnected by oxide anions via Bi–O–Bi bridges, forming 1D tunnels of Bi4As4 8-membered rings (MRs) along b-axis, the lone pairs of the arsenite groups are orientated toward the centers of the above tunnels. Thermogravimetric analysis indicated that both compounds display high thermal stability. Optical property measurements revealed that they are wide band-gap semiconductors. Both compounds display broad green-light emission bands centered at 506 nm under excitation at 380 and 388 nm. - Graphical abstract: Solid state reactions of Bi2O3 (BiCl3) and As2O3 yielded two new compounds with two different structural types, namely, Bi2O(AsO3)Cl (1), Bi8O6(AsO3)2(AsO4)2 (2). They represent the first examples of bismuth arsenates. Highlights: ► Solid state reactions of Bi2O3 (BiCl3) and As2O3 yielded two new phases. ► They represent the first examples of bismuth arsenites. ► The two compounds exhibit two different structural types.

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

    International Nuclear Information System (INIS)

    Three new organically templated or organically bonded zinc selenates, namely, {H2bipy}Zn(SeO4)2(H2O)2 1 (bipy=4,4'-bipyridine), {H2pip}{Zn(SeO4)2(H2O)4}·2H2O 2 (pip=piprazine), and Zn(SeO4)(phen)(H2O)2 3 (phen=1,10-phenanthroline) have been synthesized by hydrothermal reactions. The structure of compound 1 features a 1D chain composed of [Zn(SeO4)2(H2O)2]2- anions. Compound 2 has a 2D layer structure built from {Zn(SeO4)2(H2O)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(SeO4)(phen)(H2O)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

  17. Gold(III) bis-thiosemicarbazonato complexes: synthesis, characterization, radiochemistry and X-ray crystal structure analysis

    Energy Technology Data Exchange (ETDEWEB)

    Bottenus, Brienne N. [Department of Chemistry, University of Missouri, Columbia, MO 65211 (United States); Harry S Truman Memorial VA Hospital, Columbia, MO 65201 (United States); Kan, Para [Department of Chemistry, University of Missouri, Columbia, MO 65211 (United States); University of Missouri Research Reactor (MURR), University of Missouri, Columbia, MO 65211 (United States); Jenkins, Tyler; Ballard, Beau [Department of Chemistry, University of Missouri, Columbia, MO 65211 (United States); Rold, Tammy L. [Department of Internal Medicine, University of Missouri, Columbia, MO 65211 (United States); Harry S Truman Memorial VA Hospital, Columbia, MO 65201 (United States); Barnes, Charles [Department of Chemistry, University of Missouri, Columbia, MO 65211 (United States); Cutler, Cathy [University of Missouri Research Reactor (MURR), University of Missouri, Columbia, MO 65211 (United States); Hoffman, Timothy J. [Department of Chemistry, University of Missouri, Columbia, MO 65211 (United States); Department of Internal Medicine, University of Missouri, Columbia, MO 65211 (United States); Harry S Truman Memorial VA Hospital, Columbia, MO 65201 (United States); Green, Mark A. [School of Pharmacy, Purdue University, West Lafayette, IN 47907 (United States); Jurisson, Silvia S. [Department of Chemistry, University of Missouri, Columbia, MO 65211 (United States); University of Missouri Research Reactor (MURR), University of Missouri, Columbia, MO 65211 (United States); Harry S Truman Memorial VA Hospital, Columbia, MO 65201 (United States)], E-mail: jurissons@missouri.edu

    2010-01-15

    Introduction: A variety of (bis)thiosemicarbazone-based ligand systems have been investigated as chelating agents for Au(III) complexes with potential radiotherapeutic applications. Ligand systems containing an ethyl, propyl or butyl backbone between the two imine N donors have been synthesized to evaluate chelate ring size effects on the resultant Au(III) complex stability at the macroscopic and radiotracer levels. Methods: The Au(III) complexes were synthesized and characterized by NMR, electrospray ionization mass spectra, elemental analysis and X-ray crystallography. The {sup 198}Au complexes were evaluated in vitro at the tracer level for stability in phosphate-buffered saline at pH 7.4 and 37 deg. C. One of these complexes [{sup 198}Au(3,4-HxTSE)] showed high in vitro stability and was further evaluated in vivo in normal mice. Results: [Au(ATSM)]AuCl{sub 4}.2CH{sub 3}OH, (ATSM=diacetyl-bis(N{sup 4}-methylthiosemicarbazone)) H{sub 14}C{sub 8}N{sub 6}O{sub 2}S{sub 2}Cl{sub 4}Au{sub 2}.2CH{sub 3}OH, crystallized from methanol in the monoclinic space group P21/n with a=14.7293(13) A, b=7.7432(7) A, c=20.4363(18) A, {beta}=100.140(2){sup o}, V=2294.4 (4) A{sup 3}, Z=4; [Au(3,4-HxTSE)]Cl.CH{sub 3}CH{sub 2}OH/AuCl{sub 2}, (3,4-HxTSE=3,4-hexanedione-bis(N{sup 4}-ethylthiosemicarbazone)) H{sub 26}C{sub 13.6}N{sub 6}O{sub 0.8}S{sub 2}Cl{sub 1.2}Au{sub 1.2}, crystallized from ethanol in the monoclinic space group P21/c with a=10.1990(10) A, b=13.8833(14) A, c=15.1752(15) A, {beta}=99.353(2){sup o}, V=2120.2 (4) A{sup 3}, Z=4. Conclusions: These studies revealed poor stability of the [{sup 198}Au][Au(3,4-HxTSE)]{sup +} complex; however, crystal structure data suggest potential alterations to the ligand backbone may increase stability.

  18. 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

  19. Syntheses, crystal structures and characterizations of two new bismuth(III) arsenites

    Energy Technology Data Exchange (ETDEWEB)

    Liu Junhui [State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002 (China); Graduate School of the Chinese Academy of Sciences, Beijing 100039 (China); Kong Fang [State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002 (China); Gai Yanli [State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002 (China); Graduate School of the Chinese Academy of Sciences, Beijing 100039 (China); Mao Jianggao, E-mail: mjg@fjirsm.ac.cn [State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002 (China)

    2013-01-15

    Two new bismuth arsenites with two different structural types, namely, Bi{sub 2}O(AsO{sub 3})Cl (1), Bi{sub 8}O{sub 6}(AsO{sub 3}){sub 2}(AsO{sub 4}){sub 2} (2), have been synthesized by the solid-state reactions. Compound 1 exhibits novel 2D bismuth arsenite layers with Bi{sub 4}O{sub 4} rings capped by oxide anions, which are further interconnected by Bi-Cl-Bi bridges into a 3D network. Compound 2 contains both arsenite and arsenate anions, its 3D structures are based on 1D bismuth arsenite and 1D bismuth arsenate chains both along b-axis, which are interconnected by oxide anions via Bi-O-Bi bridges, forming 1D tunnels of Bi{sub 4}As{sub 4} 8-membered rings (MRs) along b-axis, the lone pairs of the arsenite groups are orientated toward the centers of the above tunnels. Thermogravimetric analysis indicated that both compounds display high thermal stability. Optical property measurements revealed that they are wide band-gap semiconductors. Both compounds display broad green-light emission bands centered at 506 nm under excitation at 380 and 388 nm. - Graphical abstract: Solid state reactions of Bi{sub 2}O{sub 3} (BiCl{sub 3}) and As{sub 2}O{sub 3} yielded two new compounds with two different structural types, namely, Bi{sub 2}O(AsO{sub 3})Cl (1), Bi{sub 8}O{sub 6}(AsO{sub 3}){sub 2}(AsO{sub 4}){sub 2} (2). They represent the first examples of bismuth arsenates. Highlights: Black-Right-Pointing-Pointer Solid state reactions of Bi{sub 2}O{sub 3} (BiCl{sub 3}) and As{sub 2}O{sub 3} yielded two new phases. Black-Right-Pointing-Pointer They represent the first examples of bismuth arsenites. Black-Right-Pointing-Pointer The two compounds exhibit two different structural types.

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

    International Nuclear Information System (INIS)

    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 memory, in which physics participates in the elaboration of geometric complexes and chiral biomolecules that serve to build bodies with embryoid print as it develops during gestation. Reversal mechanisms in biology are intimately

  1. Characterization of some amino acid derivatives of benzoyl isothiocyanate: Crystal structures and theoretical prediction of their reactivity

    Science.gov (United States)

    Odame, Felix; Hosten, Eric C.; Betz, Richard; Lobb, Kevin; Tshentu, Zenixole R.

    2015-11-01

    The reaction of benzoyl isothiocyanate with L-serine, L-proline, D-methionine and L-alanine gave 2-[(benzoylcarbamothioyl)amino]-3-hydroxypropanoic acid (I), 1-(benzoylcarbamothioyl)pyrrolidine-2-carboxylic acid (II), 2-[(benzoylcarbamothioyl)amino]-4-(methylsulfanyl)butanoic acid (III) and 2-[(benzoylcarbamothioyl)amino]propanoic acid (IV), respectively. The compounds have been characterized by IR, NMR, microanalyses and mass spectrometry. The crystal structures of all the compounds have also been discussed. Compound II showed rotamers in solution. DFT calculations of the frontier orbitals of the compounds have been carried out to ascertain the groups that contribute to the HOMO and LUMO, and to study their contribution to the reactivity of these compounds. The calculations indicated that the carboxylic acid group in these compounds is unreactive hence making the conversion to benzimidazoles via cyclization on the carboxylic acids impractical. This has been further confirmed by the reaction of compounds I-IV, respectively, with o-phenylene diamine which was unsuccessful but gave compound V.

  2. 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: 1.221, year: 2014

  3. Crystal growth and structural analysis of zirconium sulphoselenide single crystals

    Indian Academy of Sciences (India)

    K R Patel; R D Vaidya; M S Dave; S G Patel

    2008-08-01

    A series of zirconium sulphoselenide (ZrSSe3–, where = 0, 0.5, 1, 1.5, 2, 2.5, 3) single crystals have been grown by chemical vapour transport technique using iodine as a transporting agent. The optimum condition for the growth of these crystals is given. The stoichiometry of the grown crystals were confirmed on the basis of energy dispersive analysis by X-ray (EDAX) and the structural characterization was accomplished by X-ray diffraction (XRD) studies. The crystals are found to possess monoclinic structure. The lattice parameters, volume, particle size and X-ray density have been carried out for these crystals. The effect of sulphur proportion on the lattice parameter, unit cell volume and X-ray density in the series of ZrSSe3– single crystals have been studied and found to decrease in all these parameters with rise in sulphur proportion. The grown crystals were examined under optical zoom microscope for their surface topography study. Hall effect measurements were carried out on grown crystals at room temperature. The negative value of Hall coefficient implies that these crystals are -type in nature. The conductivity is found to decrease with increase of sulphur content in the ZrSSe3– series. The electrical resistivity parallel to c-axis as well as perpendicular to -axis have been carried out in the temperature range 303–423 K. The results obtained are discussed in detail.

  4. Synthesis, Characterization, Crystal Structure, and Biological Studies of a Cadmium(II) Complex with a Tridentate Ligand 4'-Chloro-2,2':6',2''-Terpyridine.

    Science.gov (United States)

    Saghatforoush, L A; Valencia, L; Chalabian, F; Ghammamy, Sh

    2011-01-01

    A new Cd(II) complex with the ligand 4'-chloro-2,2'6',2''-terpyridine (Cltpy), [Cd(Cltpy)(I)(2)], has been synthesized and characterized by CHN elemental analysis, (1)H-NMR, (13)C-NMR, and IR spectroscopy and structurally analyzed by X-ray single-crystal diffraction. The single-crystal X-ray analyses show that the coordination number in complex is five with three terpyridine (Cltpy) N-donor atoms and two iodine atoms. The antibacterial activities of Cltpy and its Cd(II) complex are tested against different bacteria. PMID:21738495

  5. Crystal structures of two peptide-HLA-B*1501 complexes; structural characterization of the HLA-B62 supertype

    DEFF Research Database (Denmark)

    Roder, G; Blicher, Thomas; Justesen, Sune Frederik Lamdahl;

    2006-01-01

    would be a major undertaking to address each of these specificities individually. Based upon their peptide binding specificity, they are currently subdivided into 12 supertypes. Several of these HLA supertypes have not yet been described at the structural level. To support a comprehensive understanding...... of human immune responses, the structure of at least one member of each supertype should be determined. Here, the structures of two immunogenic peptide-HLA-B*1501 complexes are described. The structure of HLA-B*1501 in complex with a peptide (LEKARGSTY, corresponding to positions 274-282 in the...... Epstein-Barr virus nuclear antigen-3A) was determined to 2.3 A resolution. The structure of HLA-B*1501 in complex with a peptide (ILGPPGSVY) derived from human ubiquitin-conjugating enzyme-E2 corresponding to positions 91-99 was solved to 1.8 A resolution. Mutual comparisons of these two structures with...

  6. A new supramolecular compound of chrome(III): Synthesis, spectroscopic characterization, X-ray crystal structure, DFT, and solution studies

    Science.gov (United States)

    Eshtiagh-Hosseini, Hossein; Yousefi, Zakieh; Mirzaei, Masoud; Chen, Ya-Guang; Ali Beyramabadi, S.; Shokrollahi, Ardeshir; Aghaei, Roghayyeh

    2010-06-01

    A new supramolecular compound of Cr(III) atom was synthesized and characterized by using elemental analysis, FTIR spectroscopy, UV-vis, and single crystal X-ray diffraction method. The chemical formula and space group of the resulting compound is (2-apymH)[Cr(pydc) 2]·2H 2O ( 1) (pydc = 2,6-pyridinedicarboxylate, 2-apym = 2-aminopyrimidine) and P2 1/ c where the final R value is 0.0157 for 3896 reflections collected. The [Cr(pydc) 2] - anions and the (2-apymH) + moiety form a three-dimensional solid state structure by a variety of noncovalent interactions such as ion pairing and hydrogen bonds interactions. On the basis of crystallographic data, it can be seen that Cr(III) atom is six-coordinated by two (pydc) 2- groups. With respect to bond lengths and angles, it is observed that coordination sphere around Cr(III) atom is a distorted octahedral. Furthermore, DFT calculation and solution study have been completely performed on 1 where corresponding data showed that obtained results from DFT and solution studies have good agreement with X-ray crystallography results. The optimized geometry confirms that the C-O (bonded) bond length of (pydc) 2- ligand in its complex form has been increased compared with the free ligand. The evidence shows that C-O (bonded) is weakened upon formation of complex, while C dbnd O (free) converted to double bond. Anionic complex possesses 90 occupied molecular orbitals and 3 half-occupied ones (91-93). A comparison between the stoichiometry of the crystalline complex in pydcH 2-2-apym-Cr system and the results obtained from solution studies clearly revealed that the CrL 2QH is the most abundant species existing in aqueous solution possesses a stoichiometry similar to that of the complex which was obtained in the solid state.

  7. Single crystal growth, structural characterization, thermal and optical properties of a novel organometallic nonlinear optical crystal: MnHg(SCN){sub 4}(C{sub 2}H{sub 5}NO){sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Wang, X.Q., E-mail: xqwang@sdu.edu.c [State Key Laboratory of Crystal Materials and Institute of Crystal Materials, Shandong University, Jinan 250100 (China); Cheng, X.F.; Zhang, S.J.; Xu, D.; Zhang, G.H.; Sun, Z.H.; Yu, F.P.; Liu, X.J. [State Key Laboratory of Crystal Materials and Institute of Crystal Materials, Shandong University, Jinan 250100 (China); Liu, W.L. [School of Materials Science and Engineering, Shandong Institute of Light Industry, Jinan 250353 (China); Chen, C.L. [Hydrology Bureau of Liaocheng, Shandong 252055 (China)

    2010-02-15

    A novel potentially useful organometallic nonlinear optical crystal, manganese mercury thiocyanate-bis(N-methylformamide), MnHg(SCN){sub 4}(C{sub 2}H{sub 5}NO){sub 2} (MMTN) has been prepared, and large highly-optical quality single crystals with dimensions up to 29x28x14 mm{sup 3} have been grown. The structural characterization, thermal and optical properties of the grown crystals are investigated. The growth morphology was obtained by indexing the X-ray powder diffraction data and compared with that deducing from the single crystal structure data using the Bravais-Friedel-Donnay-Harker model. The thermal analysis reveals that MMTN crystal possesses good physicochemical stability. The specific heat of the crystal is 635.1 J mol{sup -1} K{sup -1} at 300 K. The thermal expansion coefficient along the a, b, and c axis is alpha{sub 1}=6.18x10{sup -5} K{sup -1}, alpha{sub 2}=3.91x10{sup -5} K{sup -1} and alpha{sub 3}=9.53x10{sup -6} K{sup -1}, respectively. The laser damage threshold of MMTN crystal is about 225.7 MW/cm{sup 2} with pulse width of 18 ns at 1064 nm. The powder second harmonic efficiency of the crystal is about 1.1 pm/V and the UV transparency cutoff is 354 nm, which are interpreted on the basis of the crystal structure with the Molecular Orbital theory using a GAUSSIAN03 program.

  8. Inorganic Crystal Structure Database (ICSD)

    Science.gov (United States)

    SRD 84 FIZ/NIST Inorganic Crystal Structure Database (ICSD) (PC database for purchase)   The Inorganic Crystal Structure Database (ICSD) is produced cooperatively by the Fachinformationszentrum Karlsruhe(FIZ) and the National Institute of Standards and Technology (NIST). The ICSD is a comprehensive collection of crystal structure data of inorganic compounds containing more than 140,000 entries and covering the literature from 1915 to the present.

  9. Crystal structure of propaquizafop

    Directory of Open Access Journals (Sweden)

    Youngeun Jeon

    2014-12-01

    Full Text Available The title compound, C22H22ClN3O5 {systematic name: 2-(propan-2-ylideneaminooxyethyl (R-2-[4-(6-chloroquinoxalin-2-yloxyphenoxy]propionate}, is a herbicide. The asymmetric unit comprises two independent molecules in which the dihedral angles between the phenyl ring and the quinoxaline ring plane are 75.93 (7 and 82.77 (8°. The crystal structure features C—H...O, C—H...N, and C—H...Cl hydrogen bonds, as well as weak π–π interactions [ring-centroid separation = 3.782 (2 and 3.5952 (19 Å], resulting in a three-dimensional architecture.

  10. Crystal structure of dimethomorph

    Directory of Open Access Journals (Sweden)

    Gihaeng Kang

    2015-09-01

    Full Text Available In the title compound, C21H22ClNO4 [systematic name: (E-3-(4-chlorophenyl-3-(3,4-dimethoxyphenyl-1-(morpholin-4-ylprop-2-en-1-one], which is the morpholine fungicide dimethomorph, the dihedral angles between the mean planes of the central chlorophenyl and the terminal benzene and morpholine (r.m.s. deviation = 0.2233 Å rings are 71.74 (6 and 63.65 (7°, respectively. In the crystal, molecules are linked via C—H...O hydrogen bonds and weak Cl...π interactions [3.8539 (11 Å], forming a three-dimensional structure.

  11. Obtention of good quality Ba2NaNb5O15 crystals: growth characterization and structure of Nd3+-doped single-crystal fibres

    International Nuclear Information System (INIS)

    The obtention of good quality and crackless Ba2NaNb5O15 (BNN) single crystals doped with different amounts of Nd2O3 is reported. The crystals were grown as monocrystalline fibres by the Laser Heated Pedestal Growth technique (L.H.P.G.). A new determination of the crystallographic structure of BNN has been performed on 1 at % Nd3+ -doped fibres. It was found orthorhombic with the space group Pba2 instead of Cmm2. The well known twinning of BNN disturbing the optical properties and due to the exchange of the a and b axis of the unit cell is shown to decrease as the neodymium content of the increases. Above 3% Nd3+ doping, BNN fibres were found tetragonal. (authors). 22 refs., 8 figs., 3 tabs

  12. Potential antidiabetic drug involving a zinc anionic complex of dipic and metformin as counter ions: Synthesis, characterization, crystal structure and electrochemical studies

    Science.gov (United States)

    Ghasemi, Khaled; Rezvani, Ali Reza; Rosli, Mohd Mustaqim; Abdul Razak, Ibrahim; Moghimi, Abolghasem; Ghasemi, Fatemeh

    2014-09-01

    The new complex [H2Met][Zn(dipic)2]·3H2O (1) (dipicH2 = 2,6-pyridinedicarboxylic acid) and Met = metformin (N,N-dimethylebiguanidine), was synthesized and characterized by elemental analysis, FTIR, 1H NMR, 13C NMR and UV-Vis spectroscopy and single crystal X-ray method. The crystal system is triclinic with space group Pī. The unit cell dimensions for ZnII complex is a = 9.3817(5), b = 10.0714(5), c = 12.4917(6). In this complex, metformin is diprotonated and acts as counter ion. The intra and intermolecular hydrogen bonds stabilize the crystal structure of compound. The redox behavior of the complex was investigated by cyclic voltammetry.

  13. Second harmonic chalcone crystal: Synthesis, growth and characterization

    Energy Technology Data Exchange (ETDEWEB)

    D' Silva, E.D., E-mail: deepak.dsilva@gmail.co [Department of studies in Physics, Mangalore University, Mangalagangotri, Mangalore 574199 (India); Narayan Rao, D. [School of Physics, University of Hyderabad, Hyderabad 500046 (India); Philip, Reji [Light and Matter Physics Group, Raman Research Institute, Bangalore 560080 (India); Butcher, Ray J. [Department of Chemistry, Howard University, Washington, DC 20059 (United States); Rajnikant [Department of Physics and Electronics, University of Jammu, Jammu Tawi 180006 (India); Dharmaprakash, S.M. [Department of studies in Physics, Mangalore University, Mangalagangotri, Mangalore 574199 (India)

    2011-05-15

    The novel nonlinear optical chalcone derivative (2E)-3-[4-(methylsulfanyl)phenyl]-1-(3-bromophenyl)prop-2-en-1-one (3Br4MSP) crystals have been grown by slow evaporation technique at ambient temperature. The crystal was subjected to different types of characterization method in order to study its possible application in nonlinear optics. The structure determination of the grown crystal was done by single crystal X-ray diffraction study. The morphology of the crystal is studied. The crystal was subjected to thermal analysis to find its thermal stability. The grown crystals were characterized for their optical transmission and mechanical hardness. The second harmonic generation (SHG) efficiency of the crystal is obtained by classical powdered technique. The laser damage threshold for 3Br4MSP crystal was determined using Q-switched Nd:YAG laser.

  14. Second harmonic chalcone crystal: Synthesis, growth and characterization

    Science.gov (United States)

    D'silva, E. D.; Narayan Rao, D.; Philip, Reji; Butcher, Ray J.; Rajnikant; Dharmaprakash, S. M.

    2011-05-01

    The novel nonlinear optical chalcone derivative (2 E)-3-[4-(methylsulfanyl)phenyl]-1-(3-bromophenyl)prop-2-en-1-one (3Br4MSP) crystals have been grown by slow evaporation technique at ambient temperature. The crystal was subjected to different types of characterization method in order to study its possible application in nonlinear optics. The structure determination of the grown crystal was done by single crystal X-ray diffraction study. The morphology of the crystal is studied. The crystal was subjected to thermal analysis to find its thermal stability. The grown crystals were characterized for their optical transmission and mechanical hardness. The second harmonic generation (SHG) efficiency of the crystal is obtained by classical powdered technique. The laser damage threshold for 3Br4MSP crystal was determined using Q-switched Nd:YAG laser.

  15. Characterization and Crystal Structures of Two Copper(Ⅱ) Complexes Constructed by a Flexible Double Betaine Ligand

    Institute of Scientific and Technical Information of China (English)

    JIANG Ning-Yi; LI Song-Lin

    2007-01-01

    A flexible double betaine 1,4-bis(pyridinil-4-carboxylato)-1,4-dimethylbenzene L has been used to generate two Cu(Ⅱ)-containing metal complexes that exhibit different polymeric structures: [Cu(H2O)2 L]·2NO3 1 and [Cu(H2O)3 L]·2Cl·H2O 2. The crystal structures of 1 and 2have been determined by single-crystal X-ray diffraction method. Crystal data for 1: triclinic, space group P1-, a = 5.253(2), b = 7.406(3), c = 14.792(5) (A), α = 84.195(5), β = 80.014(5), γ =78.053(5)°, V = 553.2(3) (A)3, Z = 1, F(000) = 293, Dc = 1.717 g/cm3, the final R = 0.0385 and wR =0.1079 for 1883 observed reflections (I> 2σ(Ⅰ)); and those for 2: monoclinic, space group P21/c, a =10.222(3), b = 25.287(7), c = 9.277(3) (A),β = 93.572(5)°, V = 2393.2(12) (A)3, Z = 4, F(000) = 1140,Dc = 1.540 g/cm3, the final R = 0.0472 and wR = 0.0956 for 3204 observed reflections (I >2σ(Ⅰ)).

  16. Crystallization, phase evolution and corrosion of Fe-based metallic glasses: An atomic-scale structural and chemical characterization study

    International Nuclear Information System (INIS)

    Understanding phase changes, including their formation and evolution, is critical for the performance of functional as well as structural materials. We analyze in detail microstructural and chemical transformations of the amorphous steel Fe50Cr15Mo14C15B6 during isothermal treatments at temperatures ranging from 550 to 800 °C. By combining high-resolution transmission electron microscopy and Rietveld analyses of X-ray diffraction patterns together with the local chemical data obtained by atom probe tomography, this research provides relevant information at the atomic scale about the mechanisms of crystallization and the subsequent phases evolution. During the initial stages of crystallization a stable (Fe,Cr)23(C,B)6 precipitates as well as two metastable intermediates of M3(C,B) and the intermetallic χ-phase. When full crystallization is reached, only a percolated nano-scale Cr-rich (Fe,Cr)23(C,B)6 and Mo-rich η-Fe3Mo3C structure is detected, with no evidence to suggest that other phases appear at any subsequent time. Finally, the corrosion behavior of the developed phases is discussed from considerations of the obtained atomic information

  17. A new strontium antimonate{sup III} Sr{sub 5}Sb{sub 22}O{sub 38}: Synthesis, crystal structure and characterizations

    Energy Technology Data Exchange (ETDEWEB)

    Geng, Lei, E-mail: lgeng.cn@gmail.com [Department of Physics and Electronic Information, Huaibei Normal University, Huaibei, Anhui 235000 (China); Meng, Chang-Yu [Department of Chemistry and Materials, Yulin Normal University, Yulin, Guangxi 537000 (China); Lin, Chen-Sheng [State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002 (China); Cheng, Wen-Dan, E-mail: cwd@fjirsm.ac.cn [State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002 (China)

    2013-07-15

    A new strontium antimonate{sup III}, Sr{sub 5}Sb{sub 22}O{sub 38}, has been hydrothermally synthesized and structurally characterized by single crystal X-ray diffraction. It crystallizes in the P2{sub 1}/n space group of the monoclinic system with a=11.739(9) Å, b=12.014(10) Å, c=16.412(13) Å, β=91.460(8)°, V=2314.0(3) Å{sup 3}. The crystal structure is built of seven trigonal–pyramidal SbO{sub 3} and four sphenoid SbO{sub 4} polyhedra which are connected through sharing corner-oxygen atoms to form the complex three-dimensional {sub ∞}{sup 3}[Sb{sub 22}O{sub 38}]{sup 10−} anionic network with two different intersectant tunnels along the [111-bar ] and [11-bar 1-bar ] directions accommodating the electric charge balanced Sr{sup 2+} cations. First-principles electronic structure calculations based on the density functional theory (DFT) and the UV–vis diffuse reflectance spectroscopy measurements both indicate that the compound belongs to a direct band insulator with an optical gap value of 3.3 eV. - Graphical abstract: The 2D Sb–O slabs are stacked through sharing oxygen atoms to form the 3D network structure of the new strontium antimonate{sup III} Sr{sub 5}Sb{sub 22}O{sub 38}. - Highlights: • A new strontium antimonate{sup III}, Sr{sub 5}Sb{sub 22}O{sub 38}, has been hydrothermally synthesized. • The single crystal structure was determined by X-ray diffraction. • The powder XRD and UV–vis absorption spectroscopy were studied. • Theoretical studies interpret the relationships between optical absorption and crystal structure.

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

    International Nuclear Information System (INIS)

    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)(C4H10NO+,C7H6NO2−), 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.

  19. 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

  20. Prediction of molecular crystal structures

    CERN Document Server

    Beyer, T

    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 parac...

  1. Synchrotron white beam x-ray topography characterization of structural defects in microgravity and ground-based CdZnTe crystals

    Energy Technology Data Exchange (ETDEWEB)

    Chung, H.; Raghothamachar, B.; Dudley, M.; Larson, D.J. Jr. [SUNY, Stony Brook, NY (United States). Dept. of Materials Science and Engineering

    1996-12-31

    In a microgravity environment, gravity-dependent effects such as buoyancy, convection and hydrostatic pressure are minimized, providing an ideal environment for investigating diffusion-controlled, nonwetting crystal growth processes. To evaluate the influence of microgravity on the resultant crystal quality, Synchrotron White Beam X-ray Topography (SWBXT) is applied to characterize defect structures in both flight and ground-based CdZnTe single crystals. Transmission X-ray topographs recorded from one flight sample revealed regions of very low dislocation density with individual dislocations clearly resolved. Dislocations of very high density arrayed in a mosaic pattern were observed in all ground-base samples grown under identical growth conditions except for the gravity conditions. This observation indicates that the flight samples have much higher structural perfection than the ground-based samples. On the other hand, studies of defect configurations in a different flight sample revealed that structural defects and distributions can be strongly influenced by rapid cooling, thermal gradients, and constrained growth. Large thermal stresses induced by rapid cooling can be multiplied by wall contact leading to the formation of extensive slip bands and small angle tilt boundaries starting at the crystal periphery and propagating into the interior of the sample. It is concluded that an optimization of post solidification cooling rate is important to minimize the occurrence of slip.

  2. 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.

  3. Preparation and crystal structure characterization of CuNiGaSe3 and CuNiInSe3 quaternary compounds

    Indian Academy of Sciences (India)

    G E Delgado; A J Mora; P Grima-Gallardo; S Durán; M Muñoz; M Quintero

    2010-10-01

    Samples of the quaternary chalcogenide compounds, CuNiGaSe3 and CuNiInSe3, prepared by direct fusion and annealing method, were characterized by X-ray powder diffraction. In each case, the crystal structure was refined using the Rietveld method. Both compounds were found to crystallize in the tetragonal system, space group $\\bar{4}$2 (N°112), with unit cell parameter values = 5.6213(1) Å, = 11.0282(3) Å, = 348.48(1) Å3 and = 5.7857(2) Å, = 11.6287(5) Å, = 389.26(3) Å3 for CuNiGaSe3 and CuNiInSe3, respectively. These compounds have a normal adamantane structures and are isostructural with CuFeInSe3.

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

    International Nuclear Information System (INIS)

    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 Km, Vmax, and Kcat values of 11.58 μM, 1.5 μmol/min, and 102.18 s−1, respectively, and the catalytic and substrate binding sites of ReBktB were further confirmed by site-directed mutagenesis experiments

  5. 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

  6. Crystal structure, characterization and magnetic properties of a 1D copper(II) polymer incorporating a Schiff base with carboxylate side arm

    Indian Academy of Sciences (India)

    SHYAMAPADA SHIT; MADHUSUDAN NANDY; CORRADO RIZZOLI; CÉDRIC DESPLANCHES; SAMIRAN MITRA

    2016-06-01

    A new 1D polymeric copper(II) complex [{Cu(L)$(CF_{3}COO)}2]_{n}$ has been synthesized using apotentially tetradentate Schiff base ligand, HL, ((E)-2-((pyridin-2-yl)methyleneamino)-5-chlorobenzoic acid)and characterized by different spectroscopic methods. Single crystal X-ray structural characterization revealsthat the side arm carboxylate group of the coordinated Schiff base exhibits a $μ_{1,3}$ -bridging mode and connectsthe neighbouring copper(II) ions leading to a zigzag 1D chain structure where the copper(II) ions displaydistorted square pyramidal geometries. Variable temperature magnetic susceptibility measurement reveals aweak antiferromagnetic exchange (J = −0.47±0.01 $cm_{−1}) prevails between copper(II) ions in the chainmediated by the bridging carboxylate group, is also supported by the room temperature EPR spectral study.Electrochemical property of the complex is also reported.

  7. X-Ray Characterization of Structural Defects in Seeded and Self-Seeded ZnSe Crystal Grown by PVT in Horizontal and Vertical Configurations

    Science.gov (United States)

    Raghothamachar, B.; Dudley, M.; Su, C.-H.; Volz, H. M.; Matyi, R.; Whitaker, Ann F. (Technical Monitor)

    2001-01-01

    As part of a pre-flight ground based investigation of crystal growth of II-VI compound semiconductors, a number of ZnSe boules have been grown by physical vapor transport (PVT) at Marshall Space Flight Center. Boules were grown in both horizontal and vertical configurations and seeded and self-seeded growth techniques were employed. As-grown and/or cleaved boules were examined by a combination of synchrotron white beam x-ray topography (SWBXT) and high resolution triple axis diffraction (HRTXD) to characterized the structural defects and correlate them with the growth conditions. Horizontal grown boules tend to grow away from the ampoule wall (contactless growth) and generally exhibit large (110) facets parallel to the gravity vector. Vertical grown boules grew to the full diameter of the ampoule and exhibited no faceting. X-ray topography combined with back reflection x-ray diffraction revealed the presence of lamellar twins (180 deg type about the [111] axis) in horizontal grown boules while vertically grown boules contain a few large grains, some of which are twinned. X-ray topographs and reciprocal space maps recorded from the boules show the better crystal quality of horizontal grown boules. The relationship between crystal quality and gravity vector is investigated. Further, an attempt is made to extend the Hurle theory of twin nucleation in Czochralski grown crystals to explain the twinning mechanisms in horizontal grown boules.

  8. Synthesis, crystal growth, structural and magnetic characterization of NH4MCl2(HCOO), M=(Fe, Co, Ni)

    Science.gov (United States)

    Greenfield, Joshua T.; Ovidiu Garlea, V.; Kamali, Saeed; Chen, Michael; Kovnir, Kirill

    2016-04-01

    An ambient-pressure solution route and an improved solvothermal synthetic method have been developed to produce polycrystalline powders and large single crystals of NH4MCl2(HCOO) (M=Fe, Co, Ni). The magnetic structure of the 1D linear chain compound NH4FeCl2(HCOO) has been determined by low-temperature neutron powder diffraction, revealing ferromagnetic intra-chain interactions and antiferromagnetic inter-chain interactions. The newly-reported Co and Ni analogs are isostructural with NH4FeCl2(HCOO), but there are significant differences in the magnetic properties of each compound; the Ni analog behaves similarly to the Fe compound but with stronger magnetic coupling, exhibiting antiferromagnetic ordering (TN=8.5 K) and a broad metamagnetic transition between 2 and 5 T, while the Co analog does not order magnetically above 2 K, despite strong antiferromagnetic nearest-neighbor interactions.

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

    International Nuclear Information System (INIS)

    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

  10. Prediction of molecular crystal structures

    International Nuclear Information System (INIS)

    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 structures

  11. 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

  12. Crystal structure of benzobicyclon

    Directory of Open Access Journals (Sweden)

    Gihaeng Kang

    2015-12-01

    Full Text Available In the title compound, C22H19ClO4S2 [systematic name: 3-(2-chloro-4-mesylbenzoyl-4-(phenylsulfanylbicyclo[3.2.1]oct-3-en-2-one], which is an unclassified herbicide, the dihedral angle between the plane of the phenyl and chlorobenzene rings is 19.9 (2°. In the crystal, C—H...O hydrogen bonds link adjacent molecules, generating two-dimensional networks extending parellel to (011.

  13. Characterization of a Trifunctional Mimivirus mRNA Capping Enzyme and Crystal Structure of the RNA Triphosphatase Domain

    Energy Technology Data Exchange (ETDEWEB)

    Benarroch,D.; Smith, P.; Shuman, S.

    2008-01-01

    The RNA triphosphatase (RTPase) components of the mRNA capping apparatus are a bellwether of eukaryal taxonomy. Fungal and protozoal RTPases belong to the triphosphate tunnel metalloenzyme (TTM) family, exemplified by yeast Cet1. Several large DNA viruses encode metal-dependent RTPases unrelated to the cysteinyl-phosphatase RTPases of their metazoan host organisms. The origins of DNA virus RTPases are unclear because they are structurally uncharacterized. Mimivirus, a giant virus of amoeba, resembles poxviruses in having a trifunctional capping enzyme composed of a metal-dependent RTPase module fused to guanylyltransferase (GTase) and guanine-N7 methyltransferase domains. The crystal structure of mimivirus RTPase reveals a minimized tunnel fold and an active site strikingly similar to that of Cet1. Unlike homodimeric fungal RTPases, mimivirus RTPase is a monomer. The mimivirus TTM-type RTPase-GTase fusion resembles the capping enzymes of amoebae, providing evidence that the ancestral large DNA virus acquired its capping enzyme from a unicellular host.

  14. Crystal structure and functional characterization of the complement regulator MBL/ficolin-associated protein-1 (MAP-1)

    DEFF Research Database (Denmark)

    Skjoedt, Mikkel-Ole; Roversi, Pietro; Hummelshøj, Tina;

    2012-01-01

    The human lectin complement pathway activation molecules comprise MBL, ficolin-1, -2 and -3, in complex with associated serine proteases MASP-1, -2 and -3, and the non-enzymatic sMAP. Recently, a novel plasma protein named MBL/ficolin associated protein-1 (MAP-1) was identified in humans. This...... protein is the result of a differential splicing of the MASP1 gene and includes the major part of the heavy chain, but lacks the serine protease domain. We investigated the direct interactions of MAP-1 and MASP-3 with ficolin-3 and MBL using surface plasmon resonance and found affinities around 5 nM and 2.......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...

  15. Synthesis, crystal structure and characterization of Na3H(SO4)1.78(SeO4)0.22

    Science.gov (United States)

    Ben Hassen, C.; Boujelbene, M.; Mhiri, T.

    2013-05-01

    Synthesis, crystal structure, Raman, IR and TG/DTA characterization are given for Trisodium hydrogen bisulfate selenite Na3H(SO4)1.78(SeO4)0.22. This compound crystallizes in the monoclinic system with space group P21/c and cell parameters: a = 8.6787 (4) Å, b = 9.6631 (6) Å, c = 9.2070 (5) Å, ß = 108.825 (4)°, Z = 4 and V = 730.83 (7) Å3. The refinement of 2492 observed reflections (I > 2σ(I)) leads to R1 = 0.045 and wR2 = 0.125. The structure is characterized by S/SeO4 tetrahedra which are linked into isolated pairs by hydrogen bonds which form dimers of composition [H(SO)2]. The existence of O-H and (S/Se)-O bonds in the structure at room temperature has been confirmed by IR and Raman spectroscopy in the frequency ranges 50-1300 and 500-4000 cm-1, respectively. Thermogravimetric analysis (TGA) and differential thermal analysis (DTA) measurements have been carried out on Na3H(SO4)1.78(SeO4)0.22 crystal in the temperature range between 50 and 600 °C. Water evolution and major thermal decomposition take place with onset temperatures of approximately 282 °C and 395 °C, respectively. A Raman study of the decomposition of Na3H(SO4)1.78(SeO4)0.22 as a function of temperature supports a reaction sequence and possible intermediates during the process.

  16. Characterization of pore and crystal structure of synthesized LiBOB with varying quality of raw materials as electrolyte for lithium-ion battery

    Science.gov (United States)

    Lestariningsih, Titik; Ratri, Christin Rina; Wigayati, Etty Marty; Sabrina, Qolby

    2016-02-01

    Characterization of pore structure and crystal structure of the LiB(C2O4)2H2O or LIBOB compound has been performed in this study. These recent years, research regarding LiBOB electrolyte salt have been performed using analytical-grade raw materials, therefore this research was aimed to synthesized LiBOB electrolyte salt using the cheaper and abundant technical-grade raw materials. Lithium hydroxide (LiOH), oxalic acid dihydrate (H2C2O4.2H2O), and boric acid (H3BO3) both in technical-grade and analytical-grade quality were used as raw materials for the synthesis of LiBOB. Crystal structure characterization results of synthesized LiBOB from both technical-grade and analytical-grade raw materials have shown the existence of LiBOB and LiBOB hydrate phase with orthorombic structure. These results were also confirmed by FT-IR analysis, which showed the functional groups of LiBOB compounds. SEM analysis results showed that synthesized LiBOB has spherical structure, while commercial LiBOB has cylindrical structure. Synthesized LiBOB has a similar pore size of commercial LiBOB, i.e. 19 nm (mesoporous material). Surface area of synthesized LiBOB from analytical-grade raw materials and technical-grade materials as well as commercial LIBOB were 88.556 m2/g, 41.524 m2/g, and 108.776 m2/g, respectively. EIS analysis results showed that synthesized LiBOB from technical-grade raw materials has lower conductivity than synthesized LiBOB from analytical-grade raw materials.

  17. Isoxazole derivatives of alpha-pinene isomers: Synthesis, crystal structure, spectroscopic characterization (FT-IR/NMR/GC-MS) and DFT studies

    Science.gov (United States)

    Eryılmaz, Serpil; Gül, Melek; İnkaya, Ersin; Taş, Murat

    2016-03-01

    In this paper, the alpha-pinene isoxazole derivatives (3a-b-c, 4a-b) were synthesized via 1,3-dipolar cycloaddition and characterized with FT-IR, 1H NMR, 13C NMR and GC-MS. Isoxazole (C21H23NO) compound (4a) 6,6,7a,-trimethyl-3-(naphthalen-2-yl)-3a,4,5,6,7,7a-hexahydro-5,7-methanobenzo[d] was characterized by X-ray single crystal diffraction technique. The compound crystallizes in the monoclinic space group P 212121, with Z = 4. The molecular geometry of the compound was optimized by applying Density Functional Theory (DFT/B3LYP) method with 6-31G(d,p) and 6-311 + G(d,p) basis sets in the ground state and geometric parameters were compared with the X-ray analysis results of the structure. Results of the experimental FT-IR and NMR spectral analysis were examined in order to determine the compliance with vibrational frequencies, 1H NMR and 13C NMR chemical shifts values by using the Gauge-Independent Atomic Orbital (GIAO) method calculated over the optimized structure. Besides molecular electrostatic potential (MEP), frontier molecular orbitals (FMOs), some global reactivity descriptors, thermodynamic properties, non-linear optical (NLO) behaviour and Mulliken charge analysis of the (4a) compound were computed with the same method in gas phase, theoretically.

  18. Synthesis, crystal structure, spectroscopic characterization and nonlinear optical properties of manganese (II) complex of picolinate: A combined experimental and computational study

    Science.gov (United States)

    Tamer, Ömer; Avcı, Davut; Atalay, Yusuf; Çoşut, Bünyemin; Zorlu, Yunus; Erkovan, Mustafa; Yerli, Yusuf

    2016-02-01

    A novel manganese (II) complex with picolinic acid (pyridine 2-carboxylic acid, Hpic), namely, [Mn(pic)2(H2O)2] was prepared and its crystal structure was fully characterized by using single crystal X-ray diffraction. Picolinate (pic) ligands were coordinated to the central manganese(II) ion as bidentate N,O-donors through the nitrogen atoms of pyridine rings and the oxygen atoms of carboxylate groups forming five-membered chelate rings. The spectroscopic characterization of Mn(II) complex was performed by the applications of FT-IR, Raman, UV-vis and EPR techniques. In order to support these studies, density functional theory (DFT) calculations were carried out by using B3LYP level. IR and Raman spectra were simulated at B3LYP level, and obtained results indicated that DFT calculations generally give compatible results to the experimental ones. The electronic structure of the Mn(II) complex was predicted using time dependent DFT (TD-DFT) method with polarizable continuum model (PCM). Molecular stability, hyperconjugative interactions, intramolecular charge transfer (ICT) and bond strength were investigated by applying natural bond orbital (NBO) analysis. Nonlinear optical properties of Mn(II) complex were investigated by the determining of molecular polarizability (α) and hyperpolarizability (β) parameters.

  19. Crystal structure of triclopyr

    OpenAIRE

    Seonghwa Cho; Jineun Kim; Youngeun Jeon; Tae Ho Kim

    2014-01-01

    In the title compound {systematic name: 2-[(3,5,6-trichloropyridin-2-yl)oxy]acetic acid}, the herbicide triclopyr, C7H4Cl3NO3, the asymmetric unit comprises two independent molecules in which the dihedral angles between the mean plane of the carboxylic acid group and the pyridyl ring plane are 79.3 (6) and 83.8 (5)°. In the crystal, pairs of intermolecular O—H...O hydrogen bonds form dimers through an R22(8) ring motif and are extended into chains along [100] by weak π–π interactions [ring ce...

  20. 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.

  1. Crystal structure of pencycuron

    OpenAIRE

    Gihaeng Kang; Jineun Kim; Eunjin Kwon; Tae Ho Kim

    2015-01-01

    In the title compound [systematic name: 1-(4-chlorobenzyl)-1-cyclopentyl-3-phenylurea], C19H21ClN2O, which is a urea fungicide, the cyclopentyl ring adopts an envelope conformation, with one of the methylene C atoms adjacent to the C atom bonding to the N atom as the flap. The dihedral angles between the mean planes of the central cyclopentyl ring (all atoms) and the chlorobenzyl and phenyl rings are 77.96 (6) and 57.77 (7)°, respectively. In the crystal, N—H...O hydrogen bonds link adjacent ...

  2. Crystal structure of fenclorim

    OpenAIRE

    Eunjin Kwon; Jineun Kim; Gihaeng Kang; Tae Ho Kim

    2015-01-01

    In the title compound, C10H6Cl2N2 (systematic name: 4,6-dichloro-2-phenylpyrimidine), which is used commercially as the herbicide safener, fenclorim, the dihedral angle between the dichloropyrimidyl and phenyl rings is 9.45 (10)°. In the crystal, C—H...N hydrogen bonds link adjacent molecules, forming chains along the c-axis direction. In addition, weak intermolecular C—Cl...π [3.6185 (10) Å] and π–π [3.8796 (11) Å] interactions are present, forming a three-dimensional network....

  3. Crystal structure of fenclorim

    Directory of Open Access Journals (Sweden)

    Eunjin Kwon

    2015-10-01

    Full Text Available In the title compound, C10H6Cl2N2 (systematic name: 4,6-dichloro-2-phenylpyrimidine, which is used commercially as the herbicide safener, fenclorim, the dihedral angle between the dichloropyrimidyl and phenyl rings is 9.45 (10°. In the crystal, C—H...N hydrogen bonds link adjacent molecules, forming chains along the c-axis direction. In addition, weak intermolecular C—Cl...π [3.6185 (10 Å] and π–π [3.8796 (11 Å] interactions are present, forming a three-dimensional network.

  4. Crystal structure of metobromuron

    OpenAIRE

    Gihaeng Kang; Jineun Kim; Eunjin Kwon; Tae Ho Kim

    2015-01-01

    The title compound [systematic name: 3-(4-bromophenyl)-1-methoxy-1-methylurea], C9H11BrN2O2, is a phenylurea herbicide. The dihedral angle between the plane of the urea group and that of the bromophenyl ring is 39.13 (10)°. In the crystal, N—H...O and C—H...O hydrogen bonds and weak C—H...π interactions link adjacent molecules, forming chains along the a-axis direction. In addition, short intermolecular Br...Br contacts [3.648 (4) Å] are present, resulting in a two-dimensional network extendi...

  5. Crystal structure of azimsulfuron

    OpenAIRE

    Youngeun Jeon; Jineun Kim; Eunjin Kwon; Tae Ho Kim

    2015-01-01

    The title compound {systematic name: 1-(4,6-dimethoxypyrimidin-2-yl)-3-[1-methyl-4-(2-methyl-2H-tetrazol-5-yl)pyrazol-5-ylsulfonyl]urea}, C13H16N10O5S, is a sulfonylurea herbicide. In this compound, the dihedral angles between the planes of the central pyrazole and the terminal dimethoxypyrimidine and tetrazole rings are 79.10 (8) and 17.21 (16)°, respectively. In the crystal, N—H...O hydrogen bonds link adjacent molecules, forming R22(8) inversion dimers. In addition, weak C—H...O and C—H......

  6. Crystal structure of dimethomorph

    OpenAIRE

    Gihaeng Kang; Jineun Kim; Eunjin Kwon; Tae Ho Kim

    2015-01-01

    In the title compound, C21H22ClNO4 [systematic name: (E)-3-(4-chlorophenyl)-3-(3,4-dimethoxyphenyl)-1-(morpholin-4-yl)prop-2-en-1-one], which is the morpholine fungicide dimethomorph, the dihedral angles between the mean planes of the central chlorophenyl and the terminal benzene and morpholine (r.m.s. deviation = 0.2233 Å) rings are 71.74 (6) and 63.65 (7)°, respectively. In the crystal, molecules are linked via C—H...O hydrogen bonds and weak Cl...π interactions [3.8539 (11) Å], forming a t...

  7. Crystal structure of triclopyr

    Directory of Open Access Journals (Sweden)

    Seonghwa Cho

    2014-09-01

    Full Text Available In the title compound {systematic name: 2-[(3,5,6-trichloropyridin-2-yloxy]acetic acid}, the herbicide triclopyr, C7H4Cl3NO3, the asymmetric unit comprises two independent molecules in which the dihedral angles between the mean plane of the carboxylic acid group and the pyridyl ring plane are 79.3 (6 and 83.8 (5°. In the crystal, pairs of intermolecular O—H...O hydrogen bonds form dimers through an R22(8 ring motif and are extended into chains along [100] by weak π–π interactions [ring centroid separations = 3.799 (4 and 3.810 (4 Å]. In addition, short intermolecular Cl...Cl contacts [3.458 (2 Å] connect the chains, yielding a two-dimensional architecture extending parallel to (020. The crystal studied was found to be non-merohedrally twinned with the minor component being 0.175 (4.

  8. Crystal structure of triclopyr.

    Science.gov (United States)

    Cho, Seonghwa; Kim, Jineun; Jeon, Youngeun; Kim, Tae Ho

    2014-09-01

    In the title compound {systematic name: 2-[(3,5,6-tri-chloro-pyridin-2-yl)-oxy]acetic acid}, the herbicide triclopyr, C7H4Cl3NO3, the asymmetric unit comprises two independent mol-ecules in which the dihedral angles between the mean plane of the carb-oxy-lic acid group and the pyridyl ring plane are 79.3 (6) and 83.8 (5)°. In the crystal, pairs of inter-molecular O-H⋯O hydrogen bonds form dimers through an R 2 (2)(8) ring motif and are extended into chains along [100] by weak π-π inter-actions [ring centroid separations = 3.799 (4) and 3.810 (4) Å]. In addition, short inter-molecular Cl⋯Cl contacts [3.458 (2) Å] connect the chains, yielding a two-dimensional architecture extending parallel to (020). The crystal studied was found to be non-merohedrally twinned with the minor component being 0.175 (4). PMID:25309266

  9. Growth, structural, spectral, mechanical and dielectric characterization of RbCl-doped L-alanine hydrogen chloride monohydrate single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Lucia Rose, A.S.J., E-mail: luciarose_osm@yahoo.co.i [Department of Physics, St. Mary' s College, Thoothukudi 628 001 (India); Selvarajan, P. [Department of Physics, Aditanar College of Arts and Science, Tiruchendur 628216 (India); Perumal, S. [Physics Research Centre, S.T. Hindu College, Nagercoil 629003 (India)

    2011-02-01

    Pure (undoped) and RbCl-doped LAHC single crystals were grown successfully by the solution method with the slow evaporation technique at room temperature. The grown crystals were colourless and transparent. The solubility of the grown samples were found out at various temperatures. The lattice parameters of the grown crystals were determined by the single crystal X-ray diffraction technique and the diffracting planes were indentified by recording the powder X-ray diffraction pattern. UV-visible transmittance studies were carried out for the grown samples. Chemical analysis and atomic absorption studies indicate the presence of rubidium in the doped LAHC crystals. Nonlinear optical studies reveal that the SHG efficiency increases when the LAHC crystal is doped with rubidium chloride (RbCl). From microhardness studies, it is observed that the RbCl-doped LAHC crystal is harder than the pure sample. It is observed that the dielectric properties of the LAHC crystal are altered when it is doped with rubidium chloride.

  10. Crystal structure of triclopyr

    OpenAIRE

    Cho, Seonghwa; Kim, Jineun; Jeon, Youngeun; Kim, Tae Ho

    2014-01-01

    In the title compound {systematic name: 2-[(3,5,6-tri­chloro­pyridin-2-yl)­oxy]acetic acid}, the herbicide triclopyr, C7H4Cl3NO3, the asymmetric unit comprises two independent mol­ecules in which the dihedral angles between the mean plane of the carb­oxy­lic acid group and the pyridyl ring plane are 79.3 (6) and 83.8 (5)°. In the crystal, pairs of inter­molecular O—H⋯O hydrogen bonds form dimers through an R 2 2(8) ring motif and are extended into chains along [100] by weak π–π inter­actions ...

  11. Crystal structure of flumioxazin

    OpenAIRE

    Hyunjin Park; Jineun Kim; Eunjin Kwon; Tae Ho Kim

    2015-01-01

    The title compound {systematic name: 2-[7-fluoro-3,4-dihydro-3-oxo-4-(prop-2-yn-1-yl)-2H-1,4-benzoxazin-6-yl]-4,5,6,7-tetrahydro-1H-isoindole-1,3(2H)-dione}, C19H15FN2O4, is a dicarboximide herbicide. The dihedral angle between the maleimide and benzene ring planes is 66.13 (5)°. In the crystal, C—H...O and C—H...F hydrogen bonds and weak C—H...π interactions [3.5601 (19) Å] link adjacent molecules, forming two-dimensional networks extending parallel to the (110) plane.

  12. Crystal structure of pyrazoxyfen

    OpenAIRE

    Kwon, Eunjin; Kim, Jineun; Kang, Gihaeng; Kim, Tae Ho

    2015-01-01

    The title compound, C20H16Cl2N2O3 (systematic name: 2-{[4-(2,4-di­chloro­benzo­yl)-1,3-di­methyl­pyrazol-5-yl}­oxy}-1-phenyl­ethan-1-one), is the benzoyl­pyrazole herbicide pyrazoxyfen. The asymmetric unit comprises two independent mol­ecules, A and B, in which the pyrazole ring makes dihedral angles of 80.29 (10) and 61.70 (10)° and 87.60 (10) and 63.92 (8)°, respectively, with the di­chloro­phenyl and phenyl rings. In the crystal, C—H⋯O and C—H⋯N hydrogen bonds, and C—H⋯π and π–π [3.646 (2)...

  13. Crystal structure of flumioxazin

    Directory of Open Access Journals (Sweden)

    Hyunjin Park

    2015-10-01

    Full Text Available The title compound {systematic name: 2-[7-fluoro-3,4-dihydro-3-oxo-4-(prop-2-yn-1-yl-2H-1,4-benzoxazin-6-yl]-4,5,6,7-tetrahydro-1H-isoindole-1,3(2H-dione}, C19H15FN2O4, is a dicarboximide herbicide. The dihedral angle between the maleimide and benzene ring planes is 66.13 (5°. In the crystal, C—H...O and C—H...F hydrogen bonds and weak C—H...π interactions [3.5601 (19 Å] link adjacent molecules, forming two-dimensional networks extending parallel to the (110 plane.

  14. Crystal structure of fenclorim

    OpenAIRE

    Kwon, Eunjin; Kim, Jineun; Kang, Gihaeng; Kim, Tae Ho

    2015-01-01

    In the title compound, C10H6Cl2N2 (systematic name: 4,6-di­chloro-2-phenyl­pyrimidine), which is used commercially as the herbicide safener, fenclorim, the dihedral angle between the di­chloro­pyrimidyl and phenyl rings is 9.45 (10)°. In the crystal, C—H⋯N hydrogen bonds link adjacent mol­ecules, forming chains along the c-axis direction. In addition, weak inter­molecular C—Cl⋯π [3.6185 (10) Å] and π–π [3.8796 (11) Å] inter­actions are present, forming a three-dimensional network....

  15. Crystal structure of cyproconazole

    OpenAIRE

    Gihaeng Kang; Jineun Kim; Eunjin Kwon; Tae Ho Kim

    2015-01-01

    The title compound [systematic name: 2-(4-chlorophenyl)-3-cyclopropyl-1-(1H-1,2,4-triazol-1-yl)butan-2-ol], C15H18ClN3O, is a conazole fungicide. The asymmetric unit comprises two enantiomeric pairs (molecules A and B) in which the dihedral angles between the chlorophenyl and triazole rings are 46.54 (9) (molecule A) and 67.03 (8)° (molecule B). In the crystal, C—H...O, O—H...N and C—H...Cl hydrogen bonds and weak C—H...π interactions [3.473 (2) Å] link adjacent molecules, forming columns alo...

  16. Crystal structure of pencycuron

    Directory of Open Access Journals (Sweden)

    Gihaeng Kang

    2015-08-01

    Full Text Available In the title compound [systematic name: 1-(4-chlorobenzyl-1-cyclopentyl-3-phenylurea], C19H21ClN2O, which is a urea fungicide, the cyclopentyl ring adopts an envelope conformation, with one of the methylene C atoms adjacent to the C atom bonding to the N atom as the flap. The dihedral angles between the mean planes of the central cyclopentyl ring (all atoms and the chlorobenzyl and phenyl rings are 77.96 (6 and 57.77 (7°, respectively. In the crystal, N—H...O hydrogen bonds link adjacent molecules, forming C(4 chains propagating along the b-axis direction. The chains are linked by weak π–π interactions between the chlorobenzene rings [centroid–centroid separation = 3.9942 (9 Å], resulting in two-dimensional networks extending parellel to the (110 plane.

  17. Crystal structure of pyrazoxyfen

    OpenAIRE

    Eunjin Kwon; Jineun Kim; Gihaeng Kang; Tae Ho Kim

    2015-01-01

    The title compound, C20H16Cl2N2O3 (systematic name: 2-{[4-(2,4-dichlorobenzoyl)-1,3-dimethylpyrazol-5-yl}oxy}-1-phenylethan-1-one), is the benzoylpyrazole herbicide pyrazoxyfen. The asymmetric unit comprises two independent molecules, A and B, in which the pyrazole ring makes dihedral angles of 80.29 (10) and 61.70 (10)° and 87.60 (10) and 63.92 (8)°, respectively, with the dichlorophenyl and phenyl rings. In the crystal, C—H...O and C—H...N hydrogen bonds, and C—H...π and π–π [3.646 (2) Å] i...

  18. Crystal structure of metobromuron

    OpenAIRE

    Kang, Gihaeng; Kim, Jineun; Kwon, Eunjin; Kim, Tae Ho

    2015-01-01

    The title compound [systematic name: 3-(4-bromo­phen­yl)-1-meth­oxy-1-methyl­urea], C9H11BrN2O2, is a phenyl­urea herbicide. The dihedral angle between the plane of the urea group and that of the bromo­phenyl ring is 39.13 (10)°. In the crystal, N—H⋯O and C—H⋯O hydrogen bonds and weak C—H⋯π inter­actions link adjacent mol­ecules, forming chains along the a-axis direction. In addition, short inter­molecular Br⋯Br contacts [3.648 (4) Å] are present, resulting in a two-dimensional network extend...

  19. Crystal structure of cyproconazole

    OpenAIRE

    Kang, Gihaeng; Kim, Jineun; Kwon, Eunjin; Kim, Tae Ho

    2015-01-01

    The title compound [systematic name: 2-(4-chloro­phen­yl)-3-cyclo­propyl-1-(1H-1,2,4-triazol-1-yl)butan-2-ol], C15H18ClN3O, is a conazole fungicide. The asymmetric unit comprises two enanti­omeric pairs (mol­ecules A and B) in which the dihedral angles between the chloro­phenyl and triazole rings are 46.54 (9) (mol­ecule A) and 67.03 (8)° (mol­ecule B). In the crystal, C—H⋯O, O—H⋯N and C—H⋯Cl hydrogen bonds and weak C—H⋯π inter­actions [3.473 (2) Å] link adjacent mol­ecules, forming columns a...

  20. Crystal structure of pencycuron

    OpenAIRE

    Kang, Gihaeng; Kim, Jineun; Kwon, Eunjin; Kim, Tae Ho

    2015-01-01

    In the title compound [systematic name: 1-(4-chloro­benz­yl)-1-cyclo­pentyl-3-phenyl­urea], C19H21ClN2O, which is a urea fungicide, the cyclo­pentyl ring adopts an envelope conformation, with one of the methyl­ene C atoms adjacent to the C atom bonding to the N atom as the flap. The dihedral angles between the mean planes of the central cyclo­pentyl ring (all atoms) and the chloro­benzyl and phenyl rings are 77.96 (6) and 57.77 (7)°, respectively. In the crystal, N—H⋯O hydrogen bonds link adj...

  1. Crystal structure of metobromuron

    Directory of Open Access Journals (Sweden)

    Gihaeng Kang

    2015-08-01

    Full Text Available The title compound [systematic name: 3-(4-bromophenyl-1-methoxy-1-methylurea], C9H11BrN2O2, is a phenylurea herbicide. The dihedral angle between the plane of the urea group and that of the bromophenyl ring is 39.13 (10°. In the crystal, N—H...O and C—H...O hydrogen bonds and weak C—H...π interactions link adjacent molecules, forming chains along the a-axis direction. In addition, short intermolecular Br...Br contacts [3.648 (4 Å] are present, resulting in a two-dimensional network extending parallel to (101.

  2. Crystal structure of cyproconazole

    Directory of Open Access Journals (Sweden)

    Gihaeng Kang

    2015-12-01

    Full Text Available The title compound [systematic name: 2-(4-chlorophenyl-3-cyclopropyl-1-(1H-1,2,4-triazol-1-ylbutan-2-ol], C15H18ClN3O, is a conazole fungicide. The asymmetric unit comprises two enantiomeric pairs (molecules A and B in which the dihedral angles between the chlorophenyl and triazole rings are 46.54 (9 (molecule A and 67.03 (8° (molecule B. In the crystal, C—H...O, O—H...N and C—H...Cl hydrogen bonds and weak C—H...π interactions [3.473 (2 Å] link adjacent molecules, forming columns along the a axis.

  3. Crystal structure of flumioxazin

    OpenAIRE

    Park, Hyunjin; Kim, Jineun; Kwon, Eunjin; Kim, Tae Ho

    2015-01-01

    The title compound {systematic name: 2-[7-fluoro-3,4-di­hydro-3-oxo-4-(prop-2-yn-1-yl)-2H-1,4-benzoxazin-6-yl]-4,5,6,7-tetra­hydro-1H-iso­indole-1,3(2H)-dione}, C19H15FN2O4, is a dicarboximide herbicide. The dihedral angle between the male­imide and benzene ring planes is 66.13 (5)°. In the crystal, C—H⋯O and C—H⋯F hydrogen bonds and weak C—H⋯π inter­actions [3.5601 (19) Å] link adjacent mol­ecules, forming two-dimensional networks extending parallel to the (110) plane....

  4. Crystal structure of azimsulfuron

    OpenAIRE

    Jeon, Youngeun; Kim, Jineun; Kwon, Eunjin; Kim, Tae Ho

    2015-01-01

    The title compound {systematic name: 1-(4,6-di­meth­oxy­pyrimidin-2-yl)-3-[1-methyl-4-(2-methyl-2H-tetra­zol-5-yl)pyrazol-5-ylsulfon­yl]urea}, C13H16N10O5S, is a sulfonyl­urea herbicide. In this compound, the dihedral angles between the planes of the central pyrazole and the terminal di­meth­oxy­pyrimidine and tetra­zole rings are 79.10 (8) and 17.21 (16)°, respectively. In the crystal, N—H⋯O hydrogen bonds link adjacent mol­ecules, forming R 2 2(8) inversion dimers. In addition, weak C—H⋯O a...

  5. Crystal structure of azimsulfuron

    Directory of Open Access Journals (Sweden)

    Youngeun Jeon

    2015-07-01

    Full Text Available The title compound {systematic name: 1-(4,6-dimethoxypyrimidin-2-yl-3-[1-methyl-4-(2-methyl-2H-tetrazol-5-ylpyrazol-5-ylsulfonyl]urea}, C13H16N10O5S, is a sulfonylurea herbicide. In this compound, the dihedral angles between the planes of the central pyrazole and the terminal dimethoxypyrimidine and tetrazole rings are 79.10 (8 and 17.21 (16°, respectively. In the crystal, N—H...O hydrogen bonds link adjacent molecules, forming R22(8 inversion dimers. In addition, weak C—H...O and C—H...N hydrogen bonds and weak π–π interactions [ring centroid separation = 3.8255 (12 Å] are present, resulting in a three-dimensional architecture.

  6. Crystal structure of dimethomorph

    OpenAIRE

    Kang, Gihaeng; Kim, Jineun; Kwon, Eunjin; Kim, Tae Ho

    2015-01-01

    In the title compound, C21H22ClNO4 [systematic name: (E)-3-(4-chloro­phen­yl)-3-(3,4-di­meth­oxy­phen­yl)-1-(morpholin-4-yl)prop-2-en-1-one], which is the morpholine fungicide dimethomorph, the dihedral angles between the mean planes of the central chloro­phenyl and the terminal benzene and morpholine (r.m.s. deviation = 0.2233 Å) rings are 71.74 (6) and 63.65 (7)°, respectively. In the crystal, molecules are linked via C—H⋯O hydrogen bonds and weak Cl⋯π interactions [3.8539 (11) Å], forming ...

  7. Synthesis, Crystal Structure and Characterization of a One-dimensional Supramolecular Rare Earth Complex of N-(6-(4-Methylpyridinyl))ketoacetamide

    Institute of Scientific and Technical Information of China (English)

    XU Li; TANG Kuan-Zhen; MA Yu-Fei; TANG Yu; TAN Min-Yu

    2007-01-01

    A one-dimensional (1D) supramolecular rare earth complex [Nd(NO3)2L2-(C3H6O)][NdL(NO3)4]} (L=N-(6-(4-methylpyridinyl))ketoacetamide) has been prepared and characterized by elemental analysis, IR and electronic spectroscopy, and single-crystal X-ray diffraction. The crystal crystallizes in the triclinic system, space group P-1 with a=0.9146(6), b=1.2581(8), c=2.2316(14) nm, α=99.352(10),β=97.209(9), γ=103.935(9)°, V=2.422(3) nm3, Dc=1.776 g/cm3, C33H42N12Nd2O25, Mr=1295.27, Z=2, F(000)=1288, μ=2.217 mm-1, R=0.0508and wR=0.1046 for 5173 observed reflections (I > 2σ(I)). In the structure of the title complex,one-dimensional supramolecular double-chains are formed by intermolecular hydrogen bonding interactions.

  8. Synthesis, crystal structure and characterization of a new mixed ligand cationic-anionic nickel(II) complex containing 1,4-diazepane

    Science.gov (United States)

    Sain, Saugata; Saha, Rajat; Pilet, Guillaume; Bandyopadhyay, Debasis

    2010-12-01

    A new mixed ligand cationic-anionic nickel(II) complex, [NiL 2][Ni(NCS) 4(H 2O) 2] ( 1), where L = 1,4-diazepane has been synthesized by reacting nickel perchlorate with 1,4-diazepane and ammonium thiocyanate in the 1:1:2 M ratio. The complex has been characterized by elemental analysis, IR spectroscopy, TGA and single crystal X-ray diffraction studies. Structural studies reveal the presence of two independent mononuclear complex ions in 1 viz., a square planar [NiL 2] 2+ and an octahedral [Ni(NCS) 4(H 2O) 2] 2- which are held together by H-bonding to form a 3D supramolecular structure in the solid state.

  9. Crystal structure determination of Efavirenz

    Energy Technology Data Exchange (ETDEWEB)

    Popeneciu, Horea, E-mail: horea.popeneciu@itim-cj.ro; Dumitru, Ristoiu [College of Environmental Science on Engineering Babes Bolyai University, 30 Fantanele, 400294 Cluj Napoca (Romania); Tripon, Carmen, E-mail: horea.popeneciu@itim-cj.ro; Borodi, Gheorghe, E-mail: horea.popeneciu@itim-cj.ro; Pop, Mihaela Maria, E-mail: mihaelapop@teracrystal.com

    2015-12-23

    Needle-shaped single crystals of the title compound, C{sub 14}H{sub 9}ClF{sub 3}NO{sub 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.

  10. 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)

    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)

  11. Synthesis, crystal structure and vibrational spectra characterization of MILa(PO3)4 (MI = Na, Ag)

    OpenAIRE

    El Masloumi, Mohamed; Imaz, Inhar; Chaminade, Jean-Pierre; Videau, Jean-Jacques; Couzi, Michel; Mesnaoui, Mohamed; Maazaz, Mohamed

    2005-01-01

    The single crystals of lanthanum metaphosphate MLa(PO3)4 (M=Na, Ag) have been synthesized and studied by a combination of X-ray crystal diffraction and vibrational spectroscopy. The sodium and silver compounds crystallize in the same monoclinic P21/n space group ( factor group) with the following respective unit cell dimensions: a=7.255(2), b=13.186(3), , β=90.40(2)°, , Z=4 and a=7.300(5), b=13.211(9), , β=90.47(4)°, , Z=4. This three-dimensional framework is built of twisted zig-zag chains r...

  12. 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.

  13. Crystal structure of cyclosulfamuron

    Directory of Open Access Journals (Sweden)

    Gihaeng Kang

    2015-08-01

    Full Text Available The title compound (systematic name: 1-{[2-(cyclopropylcarbonylanilino]sulfonyl}-3-(4,6-dimethoxypyrimidin-2-ylurea, C17H19N5O6S, is a pyrimidinylsulfonylurea herbicide. The dihedral angles between the mean planes of the central benzene ring and the cyclopropyl and pyrimidinyl rings are 75.32 (9 and 88.79 (4°, respectively. The C atoms of the methoxy groups lie almost in the plane of the pyrimidine ring [deviations = 0.043 (2 and 0.028 (2 Å] and intramolecular N—H...N, N—H...O and C—H...O hydrogen bonds all close S(6 rings. In the crystal, N—H...O and C—H...O hydrogen bonds and weak π–π interactions [centroid–centroid distances = 3.6175 (9 and 3.7068 (9 Å] link adjacent molecules, forming a three-dimensional network.

  14. Crystal structure of pyrazoxyfen

    Directory of Open Access Journals (Sweden)

    Eunjin Kwon

    2015-12-01

    Full Text Available The title compound, C20H16Cl2N2O3 (systematic name: 2-{[4-(2,4-dichlorobenzoyl-1,3-dimethylpyrazol-5-yl}oxy}-1-phenylethan-1-one, is the benzoylpyrazole herbicide pyrazoxyfen. The asymmetric unit comprises two independent molecules, A and B, in which the pyrazole ring makes dihedral angles of 80.29 (10 and 61.70 (10° and 87.60 (10 and 63.92 (8°, respectively, with the dichlorophenyl and phenyl rings. In the crystal, C—H...O and C—H...N hydrogen bonds, and C—H...π and π–π [3.646 (2 Å] interactions link adjacent molecules, forming a two-dimensional network parellel to (011. In addition, the networks are linked by weak intermolecular C—Cl...π [3.356 (2, 3.950 (2, 3.250 (2 and 3.575 (2 Å] interactions, resulting in a three-dimensional architecture.

  15. Characterization of structural alteration in diamond turned silicon crystal by means of micro raman spectroscopy and transmission electron microscopy

    Directory of Open Access Journals (Sweden)

    Renato Goulart Jasinevicius

    2005-09-01

    Full Text Available In this work, (100 oriented monocrystalline silicon samples were single point diamond turned under conditions that led to a ductile and brittle regime. Raman spectroscopy results showed that the ductile regime diamond turning of silicon surfaces induced amorphization and, on the contrary, in the brittle mode machining condition this amorphous layer does not exist. Ductile machined surface was found to be a mixture of crystalline and amorphous phases probed by (macro-Raman spectroscopy. Transmission Electron Microscopy (TEM analyses were then carried out in order to characterize the structural alteration in the machined surface and chips. The electron diffraction pattern of the machined surface detected a crystalline phase along with the amorphous silicon confirming the former results. The mechanism of material removal is widely discussed based upon the results presented here.

  16. 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.

  17. 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.

  18. 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.

  19. Copper inorganic-organic hybrid coordination compound as a novel L-cysteine electrochemical sensor: Synthesis, characterization, spectroscopy and crystal structure

    Indian Academy of Sciences (India)

    Zohreh Derikvand; Azadeh Azadbakht

    2015-11-01

    Dinuclear coordination compound of Cu(II), namely, [Cu2(pydc)2(pz)(H2O)2]·2H2O, where pydc = pyridine-2,6-dicarboxylic acid (dipicolinic acid) and pz = pyrazine has been synthesized and characterized by elemental analysis, spectra (IR, UV-Vis), thermal (TG/DTG) analysis, magnetic measurements and single crystal X-ray diffraction. In the dimeric structure, the planar tridentate pyridine-2,6-dicarboxylic acid dianion coordinates to a Cu(II) ion in a meridional fashion and defines the basal plane of the complex. The fourth equatorial coordination site is then occupied by a pyrazine molecule that functions as a linear bidentate ligand bridging two Cu(II) complexes to form a dimer. The axial positions of each Cu(II) complex are occupied by one water molecule to form a distorted square pyramidal geometry. The complicated hydrogen bonding network accompanied with C–O· · · and C–H· · · stacking interactions assemble the crystal structure of 1 into a fascinating supramolecular architecture. Electrochemical behavior of [Cu2(pydc)2(pz)(H2O)2] (Cu-PDAP) on the surface of carbon nanotube (CNTs) glassy carbon electrode (GCE) is described. Oxidation of cysteine on the surface of modified electrode was investigated with cyclic voltammetry and electrochemical impedance spectroscopy (EIS). The results show that the Cu-PDAP/CNTs film displays excellent electrochemical catalytic activities towards L-cysteine oxidation.

  20. Structural characterization of Burkholderia pseudomallei adenylate kinase (Adk): Profound asymmetry in the crystal structure of the 'open' state

    Energy Technology Data Exchange (ETDEWEB)

    Buchko, G.W.; Robinson, H.; Abendroth, J.; Staker, B. L.; Myler, P. J.

    2010-04-16

    In all organisms adenylate kinases (Adks) play a vital role in cellular energy metabolism and nucleic acid synthesis. Due to differences in catalytic properties between the Adks found in prokaryotes and in the cytoplasm of eukaryotes, there is interest in targeting this enzyme for new drug therapies against infectious bacterial agents. Here we report the 2.1 {angstrom} resolution crystal structure for the 220-residue Adk from Burkholderia pseudomallei (BpAdk), the etiological agent responsible for the infectious disease melioidosis. The general structure of apo BpAdk is similar to other Adk structures, composed of a CORE subdomain with peripheral ATP-binding (ATP{sub bd}) and LID subdomains. The two molecules in the asymmetric unit have significantly different conformations, with a backbone RMSD of 1.46 {angstrom}. These two BpAdk conformations may represent 'open' Adk sub-states along the preferential pathway to the 'closed' substrate-bound state.

  1. Characterization of sodium chloride crystals grown in microgravity

    Science.gov (United States)

    Fontana, Pietro; Schefer, Jürg; Pettit, Donald

    2011-06-01

    NaCl crystals grown by the evaporation of an aqueous salt solution in microgravity on the International Space Station (ISS) were characterized and compared to salt crystals grown on earth. NaCl crystallized as thin wafers in a supersaturated film of 200-700 μm thickness and 50 mm diameter, or as hopper cubes in 10 mm diameter supersaturated spheres. Neutron diffraction shows no change in crystal structure and in cell parameters compared to earth-grown crystals. However, the morphology can be different, frequently showing circular, disk-like shapes of single crystals with perpendicular to the disks, an unusual morphology for salt crystals. In contrast to the growth on earth the lateral faces of the microgravity tabular hopper crystals are symmetrical because they are free floating during the crystallization process. Hopper cubes were produced without the need to suspend the growing crystals by an ongoing stirring. "Fleur de Sel" is shown as an example of two-dimensional growth of salt on earth and compared to the space grown crystals. It is shown that in microgravity conditions brine fluid inclusions form within the salt crystals.

  2. Nickel(II) complexes containing ONS donor ligands: Synthesis, characterization, crystal structure and catalytic application towards C-C cross-coupling reactions

    Indian Academy of Sciences (India)

    Panneerselvam Anitha; Rajendran Manikandan; Paranthaman Vijayan; Govindan Prakash; Periasamy Viswanathamurthi; Ray Jay Butcher

    2015-04-01

    Nickel(II) complexes containing thiosemicarbazone ligands [Ni(L)2] (1-3) (L = 9,10-phenanthrenequinonethiosemicarbazone (HL1), 9,10-phenanthrenequinone-N-methylthio semicarbazone (HL2) and 9, 10-phenanthrenequinone-N-phenylthiosemicarbazone (HL3)) have been synthesized and characterized by elemental analysis and spectroscopic (IR, UV-Vis, 1H, 13C-NMR and ESI mass) methods. The molecular structures of complexes 1 and 2 were identified by means of single-crystal X-ray diffraction analysis. The analysis revealed that the complexes possess a distorted octahedral geometry with the ligand coordinating in a uni-negative tridentate ONS fashion. The catalytic activity of complexes towards some C–C coupling reactions (viz., Kumada-Corriu, Suzuki-Miyaura and Sonogashira) has been examined. The complexes behave as efficient catalysts in the Kumada-Corriu and Sonogashira coupling reactions rather than Suzuki-Miyaura coupling.

  3. Dimeric and polymeric mercury(II) complexes of 1-methyl-1,2,3,4-tetrazole-5-thiol: Synthesis, crystal structure, spectroscopic characterization, and thermal analyses

    Science.gov (United States)

    Taheriha, Mohammad; Ghadermazi, Mohammad; Amani, Vahid

    2016-03-01

    Two-dimensional coordination polymer of [Hg(μ3-mmtz)2]n (1) and centrosymmetric dinuclear complexes of {[H2en][Hg2(mmtz)4(μ-Br)2]} (2) and {[H2en][Hg2(mmtz)4(μ-I)2]} (3) (where Hmmtz is 1-methyl-1,2,3,4-tetrazole-5-thiol and en is ethylene diamine) were synthesized from the reaction of Hmmtz and en with HgCl2, HgBr2 and HgI2, respectively, in CH3OH. Complex 1 was also synthesized from the reaction of Hmmtz and en with HgX2 (X = OAc and SCN) in CH3OH. These three complexes were thoroughly characterized by elemental analysis (CHN), thermal gravimetric analysis (TGA), differential thermal analyses (DTA), infrared, UV-vis, 1H NMR, and luminescence spectroscopy, and their structures were determined by single-crystal X-ray diffraction.

  4. Characterization of three LYSO crystal batches

    International Nuclear Information System (INIS)

    We report on three LYSO crystal batches characterized at the Caltech crystal laboratory for future HEP experiments: 25 20 cm long crystals for the SuperB experiment; 12 13 cm long crystals for the Mu2e experiment and 623 14×14×1.5 mm3 plates with five holes for a LYSO/W Shashlik matrix for a beam test at Fermilab. Optical and scintillation properties measured are longitudinal transmittance, light output and FWHM energy resolution. Correlations between these properties are also investigated

  5. Characterization of Three LYSO Crystal Batches

    International Nuclear Information System (INIS)

    We report on three LYSO crystal batches characterized at the Caltech crystal laboratory for future HEP experiments: Twenty-five 20 cm long crystals for the SuperB experiment; twelve 13 cm long crystals for the Mu2e experiment and 623 14×14×1.5 mm plates with five holes for a LYSO/W Shashlik matrix for a beam test at Fermilab. Optical and scintillation properties measured are longitudinal Transmittance, light output and FWHM energy resolution. Correlations between these properties are also investigated

  6. Synthesis and characterization of tetraethylammonium tetrachlorocobaltate crystals

    Indian Academy of Sciences (India)

    M A Kandhaswamy; V Srinivasan

    2002-02-01

    Single crystals of tetraethylammonium tetrachlorocobaltate were grown by solution method and characterized through single crystal X-ray diffraction, thermogravimetric analysis (TGA), differential scanning calorimetric studies (DSC) and infrared spectroscopic technique (IR). The crystals were bright, transparent and blue coloured. The unit cell parameters were found to be = = 9.0363 Å and = 14.9879 Å and = = = 90°, showing tetragonal lattice from the XRD data. Thermogravimetric analysis showed a loss of weight at 683 K from which the decomposition reaction was formulated. Thermal anomalies were found for this crystal at temperatures 200 K, 220 K in the cooling cycle and at temperatures 200 K, 240 K in the heating cycle, respectively which showed that this crystal was associated with first order phase transition. All the vibrational frequencies corresponding to (TEA)+ ions and CoCl$^{2-}_4$ ions were assigned from the IR spectral data of this crystal.

  7. Supramolecular complexes of Co(II), Ni(II) and Zn(II) p-hydroxybenzoates with caffeine: Synthesis, spectral characterization and crystal structure

    Science.gov (United States)

    Taşdemir, Erdal; Özbek, Füreya Elif; Sertçelik, Mustafa; Hökelek, Tuncer; Çelik, Raziye Çatak; Necefoğlu, Hacali

    2016-09-01

    Three novel complexes Co(II), Ni(II) and Zn(II) containing p-hydroxybenzoates and caffeine ligands were synthesized and characterized by elemental analysis, FT-IR and UV-vis Spectroscopy, molar conductivity and single crystal X-ray diffraction methods. The thermal properties of the synthesized complexes were investigated by TGA/DTA. The general formula of the complexes is [M(HOC6H4COO)2(H2O)4]·2(C8H10N4O2)·8H2O (where: M: Co, Ni and Zn). The IR studies showed that carboxylate groups of p-hydroxybenzoate ligands have monodentate coordination mode. The M2+ ions are octahedrally coordinated by two p-hydroxybenzoate ligands, four water molecules leading to an overall MO6 coordination environment. The medium-strength hydrogen bondings involving the uncoordinated caffeine ligands and water molecules, coordinated and uncoordinated water molecules and p-hydroxybenzoate ligands lead to three-dimensional supramolecular networks in the crystal structures.

  8. 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

  9. Synthesis, crystal structure and vibrational spectra characterization of MILa(PO3)4 (MI=Na, Ag)

    International Nuclear Information System (INIS)

    The single crystals of lanthanum metaphosphate MLa(PO3)4 (M=Na, Ag) have been synthesized and studied by a combination of X-ray crystal diffraction and vibrational spectroscopy. The sodium and silver compounds crystallize in the same monoclinic P21/n space group (C25h factor group) with the following respective unit cell dimensions: a=7.255(2), b=13.186(3), c=10.076(2)A, β=90.40(2)o, V=963.0(4)A3, Z=4 and a=7.300(5), b=13.211(9), c=10.079(7)A, β=90.47(4)o, V=972.09(12)A3, Z=4. This three-dimensional framework is built of twisted zig-zag chains running along a direction and made up of PO4 tetrahedra sharing two corners, connected to the LaO8 and NaO7 or AgO7 polyhedra by common oxygen atoms to the chains. The infrared and Raman vibrational spectra have been investigated. A group factor analysis leads to the determination of internal modes of (PO3)- anion in the phosphate chain

  10. Synthesis, characterization and crystal structure of four new asymmetric triazene ligands: An example of linear HII complex with H... secondary bonding interactions

    Indian Academy of Sciences (India)

    Mohammad Reza Melardi; Fatemeh Baber Shamsi Mogoii; Ayoob Babaii Sajirani; Jafar Attar Gharamaleki; Behrouz Notash; Mohammad Kazem Rofouei

    2015-12-01

    In this work, the asymmetric ligands [1-(phenyl)-3-(2-nitro-4-methylphenyl)]triazene (1), [1-(4-methylphenyl)-3-(2-nitro-4-methylphenyl)]triazene (2), [1-(4-ethylphenyl)-3-(2-nitro-4-methylphenyl)]triazene (3) and [1-(4-ethoxyphenyl)-3-(2-nitro-4-methylphenyl)]triazene (4), were synthesized. The reaction of the ligand (3) with HgCl2 in methanol resulted in the formation of the [HgL2] complex, (5). All compounds were characterized by means of CHN analysis, FT-IR, 1H NMR, 13C NMR spectroscopy. In addition, the crystal structures of the ligands (2) to (4) were investigated by single crystal X-ray analysis. In the solid state, all ligands exhibited trans conformation about the –N=N– double bond. The HgII complex (5) crystallized in monoclinic system with 2/ space group. The triazene ligand was found to be deprotonated prior to coordination and acts as monodentate ligand. The HgII which lies on inversion center (site symmetry $\\bar{1}$), is surrounded by two N atoms from L ligands forming a linear geometry. The other two Hg–N bonds are relatively longer and can only be regarded as weak secondary bonds. Also, Hg-3-arene -interactions are present in this compound. Hydrogen bonds, · · · and C–H· · · stacking interactions help in the stabilization of the resulted frameworks. These C–H· · · edge-to-face interactions are present with H· · · distance of 3.00 Å.

  11. Piperazine as counter ion for insulin-enhancing anions [VO2(dipic-OH)]-: Synthesis, characterization and X-ray crystal structure

    Science.gov (United States)

    Ghasemi, Fatemeh; Ghasemi, Khaled; Rezvani, Ali Reza; Graiff, Claudia

    2016-01-01

    The new complex [H2Pipz][VO2(dipic-OH)]2·2H2O (1), where H2dipic-OH = 4-hydroxypyridine-2,6-dicarboxylic acid and Pipz = piperazine, was synthesized and characterized by elemental analysis, FTIR, 1H NMR, 13C NMR and UV-Vis spectroscopy and single crystal X-ray diffraction. The crystal system is triclinic with space group Pī. In this compound, piperazine is diprotonated and acts as counter ion.

  12. Crystal structure and biochemical characterization of Chlamydomonas FDX2 reveal two residues that, when mutated, partially confer FDX2 the redox potential and catalytic properties of FDX1.

    Science.gov (United States)

    Boehm, Marko; Alahuhta, Markus; Mulder, David W; Peden, Erin A; Long, Hai; Brunecky, Roman; Lunin, Vladimir V; King, Paul W; Ghirardi, Maria L; Dubini, Alexandra

    2016-04-01

    The green alga Chlamydomonas reinhardtii contains six plastidic [2Fe2S]-cluster ferredoxins (FDXs), with FDX1 as the predominant isoform under photoautotrophic growth. FDX2 is highly similar to FDX1 and has been shown to interact with specific enzymes (such as nitrite reductase), as well as to share interactors with FDX1, such as the hydrogenases (HYDA), ferredoxin:NAD(P) reductase I (FNR1), and pyruvate:ferredoxin oxidoreductase (PFR1), albeit performing at low catalytic rates. Here we report the FDX2 crystal structure solved at 1.18 Å resolution. Based on differences between the Chlorella fusca FDX1 and C. reinhardtii FDX2 structures, we generated and purified point-mutated versions of the FDX2 protein and assayed them in vitro for their ability to catalyze hydrogen and NADPH photo-production. The data show that structural differences at two amino acid positions contribute to functional differences between FDX1 and FDX2, suggesting that FDX2 might have evolved from FDX1 toward a different physiological role in the cell. Moreover, we demonstrate that the mutations affect both the midpoint potentials of the FDX and kinetics of the FNR reaction, possibly due to altered binding between FDX and FNR. An effect on H2 photo-production rates was also observed, although the kinetics of the reaction were not further characterized. PMID:26526668

  13. Characterization of D-glucaric acid using NMR, x-ray crystal structure, and MM3 molecular modeling analyses

    Science.gov (United States)

    D-glucaric acid was characterized in solution by comparing NMR spectra from the isotopically unlabeled molecule with those from D-glucaric acid labeled with deuterium or carbon-13 atoms. The NMR studies provided unequivocal assignments for all carbon atoms and non-hydroxyl protons of the molecule. ...

  14. Calcium oxalate crystals in eucalypt ectomycorrhizae: morphochemical characterization.

    Science.gov (United States)

    Pylro, Victor Satler; de Freitas, André Luiz Moreira; Otoni, Wagner Campos; da Silva, Ivo Ribeiro; Borges, Arnaldo Chaer; Costa, Maurício Dutra

    2013-01-01

    Ectomycorrhizal fungi are ubiquitous in forest ecosystems, benefitting plants principally by increasing the uptake of water and nutrients such as calcium from the soil. Previous work has demonstrated accumulation of crystallites in eucalypt ectomycorrhizas, but detailed morphological and chemical characterization of these crystals has not been performed. In this work, cross sections of acetic acid-treated and cleared ectomycorrhizal fragments were visualized by polarized light microscopy to evaluate the location of crystals within cortical root cells. Ectomycorrhizal sections were also observed by scanning electron microscopy (SEM) coupled with energy dispersive x-ray (EDS) microprobe analysis. The predominant forms of crystals were crystal sand (granules) and concretions. Calcium, carbon and oxygen were detected by EDS as constituent elements and similar elemental profiles were observed between both crystal morphologies. All analyzed crystalline structures were characterized as calcium oxalate crystals. This is the first report of the stoichiometry and morphology of crystals occurring in eucalypt ectomycorrhizas in tropical soils. The data corroborates the role of ectomycorrhizae in the uptake and accumulation of calcium in the form of calcium oxalate crystals in hybrid eucalypt plants. PMID:23844062

  15. Calcium oxalate crystals in eucalypt ectomycorrhizae: morphochemical characterization.

    Directory of Open Access Journals (Sweden)

    Victor Satler Pylro

    Full Text Available Ectomycorrhizal fungi are ubiquitous in forest ecosystems, benefitting plants principally by increasing the uptake of water and nutrients such as calcium from the soil. Previous work has demonstrated accumulation of crystallites in eucalypt ectomycorrhizas, but detailed morphological and chemical characterization of these crystals has not been performed. In this work, cross sections of acetic acid-treated and cleared ectomycorrhizal fragments were visualized by polarized light microscopy to evaluate the location of crystals within cortical root cells. Ectomycorrhizal sections were also observed by scanning electron microscopy (SEM coupled with energy dispersive x-ray (EDS microprobe analysis. The predominant forms of crystals were crystal sand (granules and concretions. Calcium, carbon and oxygen were detected by EDS as constituent elements and similar elemental profiles were observed between both crystal morphologies. All analyzed crystalline structures were characterized as calcium oxalate crystals. This is the first report of the stoichiometry and morphology of crystals occurring in eucalypt ectomycorrhizas in tropical soils. The data corroborates the role of ectomycorrhizae in the uptake and accumulation of calcium in the form of calcium oxalate crystals in hybrid eucalypt plants.

  16. Synthesis, characterization and crystal structure of cobalt(III) complexes containing 2-acetylpyridine thiosemicarbazones: DNA/protein interaction, radical scavenging and cytotoxic activities.

    Science.gov (United States)

    Manikandan, Rajendran; Viswanathamurthi, Periasamy; Velmurugan, Krishnaswamy; Nandhakumar, Raju; Hashimoto, Takeshi; Endo, Akira

    2014-01-01

    The synthesis, structure and biological studies of cobalt(III) complexes supported by NNS-tridentate ligands are reported. Reactions of 2-acetylpyridine N-substituted thiosemicarbazone (HL(1-3)) with [CoCl2(PPh3)2] resulted [Co(L(1-3))2]Cl (1-3) which were characterized by elemental analysis and various spectral studies. The molecular structure of the complex 1 has been determined by single crystal X-ray diffraction studies. In vitro DNA binding studies of complexes 1-3 carried out by fluorescence studies and the results revealed the binding of complexes to DNA via intercalation. The binding constant (Kb) values of complexes 1-3 from fluorescence experiments showed that the complex 3 has greater binding propensity for DNA. The DNA cleavage activity of the complexes 1 and 3 were ascertained by gel electrophoresis assay which revealed that the complexes are good DNA cleavage agents. Further, the interactions of the complexes with bovine serum albumin (BSA) were also investigated using fluorescence spectroscopic method, which showed that the complexes 1-3 could bind strongly with BSA. The antioxidant property of the complexes was evaluated to test their free-radical scavenging ability. Furthermore, in vitro cytotoxicity of the complexes against MCF-7 and A431 cell lines was assayed which showed higher activity and efficiently vanished the cancer cells even at low concentrations. PMID:24342132

  17. Surfactant-assisted hydrothermal crystallization of nanostructured lithium metasilicate (Li2SiO3) hollow spheres: (I) Synthesis, structural and microstructural characterization

    International Nuclear Information System (INIS)

    Lithium metasilicate (Li2SiO3) was successfully synthesized using a hydrothermal process in the presence of different surfactants with cationic, non-ionic and anionic characters. The samples obtained were compared to a sample prepared by the conventional solid-state reaction method. The structural and microstructural characterizations of different Li2SiO3 powders were performed using various techniques. Diffraction analyses revealed the successful crystallization of pure Li2SiO3 single phase by hydrothermal technique, even without further heat-treatments and independent of the surfactant used. Electron microscopy analyses revealed that Li2SiO3 powders were composed of uniform micrometric particles with a hollow sphere morphology and nanostructured walls. Finally, different thermal analyses showed that Li2SiO3 samples preserved their structure and microstructure after further thermal treatments. Specific aspects regarding the formation mechanism of the spherical aggregates under hydrothermal conditions are discussed, and there is a special emphasis on the effect of the synthesis pathway on the morphological characteristics. -- Graphical abstract: Li2SiO3 was synthesized using a hydrothermal process in the presence of different surfactants. Li2SiO3 powders were composed of uniform micrometric particles with a hollow sphere morphology and nanostructured walls. Display Omitted Highlights: → Pure Li2SiO3 was synthesized by the hydrothermal method. → Surfactant addition produced microstructural and morphological variations. → TEM reveled the generation of nanostructured hollow spheres.

  18. A dysprosium-based metal-organic framework: Synthesis, characterization, crystal structure and interaction with calf thymus-DNA and bovine serum albumin

    Indian Academy of Sciences (India)

    Biplab Mondal; Buddhadeb Sen; Ennio Zangrando; Pabitra Chattopadhyay

    2014-07-01

    A dysprosium-based metallo-organic framework (MOF) containing calcium ions formulated as {Dy(pyda)3Ca1.5(H2O)6} · 5.5H2O (1) (H2pyda = pyridine-2,6-dicarboxylic acid) was solvothermally synthesized in ethanolic medium and characterized by physico-chemical and spectroscopic tools. A detailed structural analysis of the solid state structure of 1 by single crystal X-ray diffraction study showed a tricapped trigonal prism geometry for lanthanide in the [Dy(pyda)3]3− fragment. The mode of interaction of 1 with calf thymus- DNA and with protein bovine serum albumin (BSA) was investigated by using absorption and emission spectroscopic tools. The apparent association constant of complex 1 with CT-DNA was deduced from an absorption spectral study (b = 4.08 × 104 M-1). Spectral and viscosity measurements indicated a groove-binding mode of 1 with CT-DNA, and from spectroscopic study the formation of a metal complex-BSA adduct was assumed to be the result of the interaction of 1 with BSA.

  19. Crystal structure of gold hydride

    International Nuclear Information System (INIS)

    Highlights: • Volume expansion of metal hydrides is due to the increase in the s-band filling. • AuH structure is similar to that of Hg having one more s electron compared to Au. • Structure stability of both Hg and AuH is governed by the Hume-Rothery rule. - Abstract: A number of transition metal hydrides with close-packed metal sublattices of fcc or hcp structures with hydrogen in octahedral interstitial positions were obtained by the high-pressure-hydrogen technique described by Ponyatovskii et al. (1982). In this paper we consider volume increase of metals by hydrogenation and possible crystal structure of gold hydride in relation with the structure of mercury, the nearest neighbor of Au in the Periodic table. Suggested structure of AuH has a basic tetragonal body-centered cell that is very similar to the mercury structure Hg-t I 2. The reasons of stability for this structure are discussed within the model of Fermi sphere–Brillouin zone interactions

  20. Crystal structure of gold hydride

    Energy Technology Data Exchange (ETDEWEB)

    Degtyareva, Valentina F., E-mail: degtyar@issp.ac.ru

    2015-10-05

    Highlights: • Volume expansion of metal hydrides is due to the increase in the s-band filling. • AuH structure is similar to that of Hg having one more s electron compared to Au. • Structure stability of both Hg and AuH is governed by the Hume-Rothery rule. - Abstract: A number of transition metal hydrides with close-packed metal sublattices of fcc or hcp structures with hydrogen in octahedral interstitial positions were obtained by the high-pressure-hydrogen technique described by Ponyatovskii et al. (1982). In this paper we consider volume increase of metals by hydrogenation and possible crystal structure of gold hydride in relation with the structure of mercury, the nearest neighbor of Au in the Periodic table. Suggested structure of AuH has a basic tetragonal body-centered cell that is very similar to the mercury structure Hg-t I 2. The reasons of stability for this structure are discussed within the model of Fermi sphere–Brillouin zone interactions.

  1. Crystal growth and characterization of L-valine cadmium acetate a semiorganic NLO crystals

    Science.gov (United States)

    Chandrasekaran, J.; Ilayabarathi, P.; Maadeswaran, P.

    2012-08-01

    A new semiorganic nonlinear optical material, L-valine cadmium acetate, was grown successfully from aqueous solution by slow evaporation method. The grown crystals characterized by using Powder X-ray diffraction analysis confirms the structure of the grown title compound. The functional groups have been identified using FTIR spectral data. Transmittance compound was analyzed by using UV-vis spectrum. The thermal behavior of the grown crystal was determined with the aid of thermogravimetric analysis (TGA), differential thermal analysis (DTA) and differential scanning calorimetry (DSC). The dielectric constant was studied as a function of frequency for various temperatures. The grown crystal has positive photoconductivity nature. The fluorescence spectrum of the crystal was recorded and its optical band gap is about 3.4479 eV. Second order nonlinear optical property of the grown crystal has been confirmed by modified Kurtz-Perry powder second harmonic generation (SHG) test.

  2. Laser MBE-grown yttrium iron garnet films on GaN: characterization of the crystal structure and magnetic properties

    Science.gov (United States)

    Kaveev, A. K.; Bursian, V. E.; Gastev, S. V.; Krichevtsov, B. B.; Suturin, S. M.; Volkov, M. P.; Sokolov, N. S.

    2016-07-01

    Yttrium iron garnet (YIG) films were grown on GaN substrates using the laser molecular beam epitaxy method. X-ray diffraction data showed polycrystalline YIG layers without additional structural modifications. The magnetic properties of the YIG films were studied at room temperature with the aid of a vibration sample magnetometer, the magneto-optical Kerr effect and ferromagnetic resonance methods. ‘Easy-plane’-type magnetic anisotropy was found in the films. The gyromagnetic ratio and 4 πMS value were calculated.

  3. Synthesis, characterization, crystal structures, and antibacterial activity of some new 1-(3,4,5-trimethoxybenzoyl)-3-aryl thioureasreas

    OpenAIRE

    Saeed, Aamer; Khera, Rasheed Ahmad; Abbas, Naeem; Latif, Muhammad

    2010-01-01

    Synthesis of some novel 1-(3,4,5-trimethoxy)benzoyl-3- arylthiourea derivatives (1a-o) was accomplished in 2 steps. The synthetic route involves the reaction of 1-(3,4,5-trimethoxy)benzoyl chloride with potassium thiocyanate in 1:1 molar ratio in acetone to afford the corresponding isothiocyante followed by treatment with suitably substituted anilines. The structures of the products were established by elemental analyses, IR, 1H- and 13C-NMR, and mass spectroscopy and for 1b and 1m f...

  4. Synthesis, characterization, crystal structure, DNA- and HSA-binding studies of a dinuclear Schiff base Zn(II) complex derived from 2-hydroxynaphtaldehyde and 2-picolylamine

    Science.gov (United States)

    Kazemi, Zahra; Rudbari, Hadi Amiri; Mirkhani, Valiollah; Sahihi, Mehdi; Moghadam, Majid; Tangestaninejad, Sharam; Mohammadpoor-Baltork, Iraj

    2015-09-01

    A tridentate Schiff base ligand NNO donor (HL: 1-((E)-((pyridin-2-yl)methylimino)methyl)naphthalen-2-ol was synthesized from condensation of 2-hydroxynaphtaldehyde and 2-picolylamine. Zinc complex, Zn2L2(NO3)2, was prepared from reaction of Zn(NO3)2 and HL at ambient temperature. The ligand and complex were characterized by FT-IR, 1H NMR, 13C NMR and elemental analysis (CHN). Furthermore, the structure of dinuclear Zn(II) complex was determined by single crystal X-ray analysis. The complex, Zn2L2(NO3)2, is centrosymmetric dimer in which deprotonated phenolates bridge the two Zn(II) atoms and link the two halves of the dimer. In the structure, Zinc(II) ions have a highly distorted six-coordinate structure bonded to two oxygen atoms from a bidentate nitrate group, the pyridine nitrogen, an amine nitrogen and phenolate oxygens. The interaction of dinuclear Zn(II) complex with fish sperm DNA (FS-DNA) and HSA was investigated under physiological conditions using fluorescence quenching, UV-Vis spectroscopy, molecular dynamics simulation and molecular docking methods. The estimated binding constants for the DNA-complex and HSA-complex were (3.60 ± 0.18) × 104 M-1 and (1.35 ± 0.24) × 104 M-1, respectively. The distance between dinuclear Zn(II) complex and HSA was obtained based on the Förster's theory of non-radiative energy transfer. Molecular docking studies revealed the binding of dinuclear Zn(II) complex to the major groove of FS-DNA and IIA site of protein by formation of hydrogen bond, π-cation and hydrophobic interactions.

  5. Crystal Structure of Macrocalyxin J

    Institute of Scientific and Technical Information of China (English)

    HE Shan; WU Bin; SHI Hao; SUN Cui-Rong

    2007-01-01

    The title compound, (1α,6β, 1 1β, 14α)-1,7:6,20-diepoxy-6,1 1-dihydroxy- 6,7-secoent- kaur-1 6-ene-7,15-dione-14-acetate (macrocalyxin J), is a diterpenoid which was isolated from the leaves of Rabdosia macrocalyx and characterized by single-crystal X-ray diffraction. It crystallizes in orthorhombic, spac e group P212121 with a = 9.3608(8), b = 14.9787(12), c = 15.5750(13)(A), Z = 4, V = 2183.8(3) (A)3, C22H30O9, Mr = 438.46, Dc = 1.334 g/m3, μ(MoKα) = 0.103 mm-1,F(000) = 936, the final R = 0.0532 and wR = 0.1262 for 2252 observed reflections (I > 2σ(I)). In the molecule, three six-membered rings adopt chair, boat and slightly distorted boat conformations,respectively, while both five-membered rings have approximate envelope conformations.

  6. Keggin (K5, H3O)[SiV3W9O40H]·xH2O: Characterization and crystal structure

    Science.gov (United States)

    Bonfim, Rodrigo de Paiva Floro; de Moura, Luiza Cristina; Eon, Jean-Guillaume; Mentré, Olivier; Vezin, Hervé; Caldarelli, Stefano

    2014-05-01

    Single crystals of the potassium salt (K5, H3O)[SiV3W9O40H]·xH2O of the vanadium tri-substituted α-Keggin dodecatungstosilicate were prepared and analyzed by vibrational, EPR and 51V NMR spectroscopy. Varying the synthesis conditions allows crystallization of partially reduced anions. The crystal structure was determined for both oxidized (V5+) and partially reduced (V4+/5+) potassium salts. Single crystal X-ray diffraction data and solid state 51V-NMR spectra confirm the occurrence of a single vanadium site in a cubic structure due to rotational disorder of the Keggin ion. Partially reduced compounds crystallize within the same structure as fully oxidized ones. EPR experiments confirm strong interaction of V4+ with two V5+ ions, in accordance with insertion of a V3 subunit into the lacunary Keggin ion as designed in the synthesis method. The 3D-edifice is composed of K+/H2O counter-sublattice with evidence of tunable water occupancy.

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

    International Nuclear Information System (INIS)

    2-Amino-7-methyl-5-oxo-4-phenyl-4,5-dihydropyrano[3,2-c] pyran-3-carbonitrile, C16H12N2O3 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. P21/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

  8. 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.

  9. Influence of microgravity on protein crystal structures

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    Structural determination and comparison of microgravity and ground grown protein crystals have been carried out in order to investigate the effect of microgravity on the structure of protein crystals. Following the structural studies on the hen egg-white lysozyme cystals grown in space and on the ground, the same kind of comparative studies was performed with acidic phospholipase A2 crystals grown in different gravities. Based on the results obtained so far, a conclusion could be made that microgravity might not be strong enough to change the conformation of polypeptide chain of proteins, but it may improve the bound waters' structure, and this might be an important factor for microgravity to improve the protein crystal quality. In addition, the difference in the improvement between the two kinds of protein crystals may imply that the degree of improvement of a protein crystal in microgravity may be related to the solvent content in the protein crystal.

  10. Synthesis, characterization and crystal structures of new Zinc(II) and Nickel(II) complexes containing morpholine moiety and their antibacterial studies

    Czech Academy of Sciences Publication Activity Database

    Goudarziafshar, H.; Rezaeivala, M.; Khosravi, F.; Abbasityula, Y.; Yousefi, S.; Özbek, N.; Eigner, Václav; Dušek, Michal

    2015-01-01

    Roč. 12, č. 1 (2015), 113-119. ISSN 1735-207X Grant ostatní: AV ČR(CZ) Praemium Academiae Institutional support: RVO:68378271 Keywords : crystal structure * morpholine moiety * antibacterial effects * zinc(ii) complex * nickel(ii) complex Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.087, year: 2014

  11. 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: 1.587, year: 2014

  12. 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

    the competitive interaction and high potency. To delineate the binding mechanism, we have solved the crystal structure of the GluN1 ligand-binding domain in complex with TK40 and show that TK40 binds to the orthosteric binding site of the GluN1 subunit with a binding mode that was also predicted by virtual...

  13. Synthesis, spectral characterization, and single crystal structure studies of (2-nitro-ethene-1,1-diyl)-bis-((4-isopropyl-benzyl)sulfane)

    International Nuclear Information System (INIS)

    The title compound (2-nitro-ethene-1,1-diyl)-bis-(4-isopropylbenzyl)sulfane) (5), was synthesised using a two step process. The structure of the product (5) was established by UV, FT-IR, 1H NMR, 13C NMR, C,H,N analysis, LC-MS and single crystal X-ray diffraction analysis. The single crystal of the title compound (5) was crystallized in Monoclinic with the space group of P21/c. The crystal exhibit the following unit cell parameters a = 12.8165(18), b = 6.1878(6), c = 27.082(4) Å, β = 90.705(17)°, V = 2147.6(5) A3, Z = 4, Dx = 1.242 Mg/m3 and the molecular formula of C22H27N1O2S2 was found. The final R value was 0.0776. The crystal structure is stabilized by an interesting intramolecular push and pull five membered electrocyclic interaction between the O1–N1–C2–C1–S1- and via the intermolecular H-bonding interaction between C2–H2···O2

  14. Synthesis, spectral characterization, and single crystal structure studies of (2-nitro-ethene-1,1-diyl)-bis-((4-isopropyl-benzyl)sulfane)

    Science.gov (United States)

    Sakthikumar, L.; Mahalakshmy, R.; Bhargavi, G.; Srinivasan, N.

    2015-12-01

    The title compound (2-nitro-ethene-1,1-diyl)-bis-(4-isopropylbenzyl)sulfane) (5), was synthesised using a two step process. The structure of the product (5) was established by UV, FT-IR, 1H NMR, 13C NMR, C,H,N analysis, LC-MS and single crystal X-ray diffraction analysis. The single crystal of the title compound (5) was crystallized in Monoclinic with the space group of P21/ c. The crystal exhibit the following unit cell parameters a = 12.8165(18), b = 6.1878(6), c = 27.082(4) Å, β = 90.705(17)°, V = 2147.6(5) A3, Z = 4, D x = 1.242 Mg/m3 and the molecular formula of C22H27N1O2S2 was found. The final R value was 0.0776. The crystal structure is stabilized by an interesting intramolecular push and pull five membered electrocyclic interaction between the O1-N1-C2-C1-S1- and via the intermolecular H-bonding interaction between C2-H2···O2.

  15. Synthesis, spectral characterization, and single crystal structure studies of (2-nitro-ethene-1,1-diyl)-bis-((4-isopropyl-benzyl)sulfane)

    Energy Technology Data Exchange (ETDEWEB)

    Sakthikumar, L., E-mail: lsakthisbk@gmail.com [Saiva Bhanu Kshatriya College, Department of Chemistry (India); Mahalakshmy, R. [Thiagarajar College, PG & Department of Chemistry (India); Bhargavi, G.; Srinivasan, N. [University of Hyderabad, School of Chemistry (India)

    2015-12-15

    The title compound (2-nitro-ethene-1,1-diyl)-bis-(4-isopropylbenzyl)sulfane) (5), was synthesised using a two step process. The structure of the product (5) was established by UV, FT-IR, {sup 1}H NMR, {sup 13}C NMR, C,H,N analysis, LC-MS and single crystal X-ray diffraction analysis. The single crystal of the title compound (5) was crystallized in Monoclinic with the space group of P21/c. The crystal exhibit the following unit cell parameters a = 12.8165(18), b = 6.1878(6), c = 27.082(4) Å, β = 90.705(17)°, V = 2147.6(5) A{sup 3}, Z = 4, D{sub x} = 1.242 Mg/m{sup 3} and the molecular formula of C{sub 22}H{sub 27}N{sub 1}O{sub 2}S{sub 2} was found. The final R value was 0.0776. The crystal structure is stabilized by an interesting intramolecular push and pull five membered electrocyclic interaction between the O1–N1–C2–C1–S1- and via the intermolecular H-bonding interaction between C2–H2···O2.

  16. Synthesis,Characterization and Crystal Structures of the μ-Oxygen-Bis[Tri(p-Fluorobenzyl)tin]%μ-氧-双[三(对氟苄基)锡]的合成、表征及晶体结构

    Institute of Scientific and Technical Information of China (English)

    尹汉东; 洪敏; 王传华

    2005-01-01

    The μ-oxygen-bis[tri(p-fluorobenzyl)tin] was synthesized. The structure were characterized by elementary analysis, IR and 1H NMR and the crystal structure were determined by X-ray single crystal diffraction. The crystal of the title compound belongs to rhombohedral with space group R, α=1.3464(4), b=1.3464(4), c=1.7729(7)nm, α=90°,β=90°, γ=120°, Z=3, V=2.7832(15)nm3, Dc=1.625g·cm-3,μ(Mo Kα)=1.408mm-1, S=1.088, F(000)=1350, R1=0.0275, ωR2=0.0659. In compound,the tin atom has a distorted tetrahedral coordination configuration. CCDC: 257079.

  17. Synthesis, Characterization, Crystal Structure, and Biological Studies of a Cadmium(II) Complex with a Tridentate Ligand 4′-Chloro-2,2′:6′,2′′-Terpyridine

    Science.gov (United States)

    Saghatforoush, L. A.; Valencia, L.; Chalabian, F.; Ghammamy, Sh.

    2011-01-01

    A new Cd(II) complex with the ligand 4′-chloro-2,2′6′,2′′-terpyridine (Cltpy), [Cd(Cltpy)(I)2], has been synthesized and characterized by CHN elemental analysis, 1H-NMR, 13C-NMR, and IR spectroscopy and structurally analyzed by X-ray single-crystal diffraction. The single-crystal X-ray analyses show that the coordination number in complex is five with three terpyridine (Cltpy) N-donor atoms and two iodine atoms. The antibacterial activities of Cltpy and its Cd(II) complex are tested against different bacteria. PMID:21738495

  18. Synthesis, Characterization, Crystal Structure, and Biological Studies of a Cadmium(II Complex with a Tridentate Ligand 4′-Chloro-2,2′:6′,2′′-Terpyridine

    Directory of Open Access Journals (Sweden)

    L. A. Saghatforoush

    2011-01-01

    Full Text Available A new Cd(II complex with the ligand 4′-chloro-2,2′6′,2′′-terpyridine (Cltpy, [Cd(Cltpy(I2], has been synthesized and characterized by CHN elemental analysis, 1H-NMR, 13C-NMR, and IR spectroscopy and structurally analyzed by X-ray single-crystal diffraction. The single-crystal X-ray analyses show that the coordination number in complex is five with three terpyridine (Cltpy N-donor atoms and two iodine atoms. The antibacterial activities of Cltpy and its Cd(II complex are tested against different bacteria.

  19. Synthesis, spectral (IR, UV-Vis and variable temperature NMR) characterization and crystal structure of (N-benzyl-N-furfuryldithicarbamato-S,S‧)(thiocyanato-N)(triphenylphosphine)nickel(II)

    Science.gov (United States)

    Valarmathi, P.; Thirumaran, S.; Sarmal, Lovely; Kant, Rajni

    2014-08-01

    Planar (N-benzyl-N-furfuryldithiocarbamato-S,S‧)(thiocyanato-N)(triphenylphospine)nickel(II), [Ni(bfdtc)(NCS)(PPh3)], (1) was prepared from bis(N-benzyl-N-furfuryldithiocarbamato-S,S‧)nickel(II), [Ni(bfdtc)2], (2) and characterized by elemental analysis, cyclic voltammetry, electronic, IR and variable temperature 1H and 13C NMR spectra. For complex 1, the thioureide vCsbnd N value is shifted to higher wavenumber compared to 2 and N13CS2 carbon signal observed for 1 is additionally shielded compared to the parent complex 2, suggesting increased strength of the thioureide bond due to the presence of the π-accepting phosphine. In the room temperature 13C NMR spectrum of 1, two pseudo doublets are observed in the aliphatic region. Variable temperature 13C NMR spectral studies suggest that the fast thiocyanate exchange appears to be responsible for the appearance of pseudo doublets. Single crystal X-ray structural analysis of 1 and 2 confirm the presence of four coordinated nickel in a distorted square planar arrangement with the NiS2PN and NiS4 chromophores, respectively. The Nisbnd S bonds are symmetric in 2 (2.1914(14) and 2.2073(13) Å). But significant asymmetry in Nisbnd S bond distances was observed in 1 (2.2202(8) Å and 2.1841 Å). This observation clearly supports the less effective trans effect of SCN- over PPh3. Cyclic voltammetric studies revealed easier reduction of nickel(II) to nickel(I) in complex 1 compared to 2.

  20. Synthesis, spectral (IR, UV-Vis and variable temperature NMR) characterization and crystal structure of (N-benzyl-N-furfuryldithicarbamato-S,S')(thiocyanato-N)(triphenylphosphine)nickel(II).

    Science.gov (United States)

    Valarmathi, P; Thirumaran, S; Sarmal, Lovely; Kant, Rajni

    2014-08-14

    Planar (N-benzyl-N-furfuryldithiocarbamato-S,S')(thiocyanato-N)(triphenylphospine)nickel(II), [Ni(bfdtc)(NCS)(PPh3)], (1) was prepared from bis(N-benzyl-N-furfuryldithiocarbamato-S,S')nickel(II), [Ni(bfdtc)2], (2) and characterized by elemental analysis, cyclic voltammetry, electronic, IR and variable temperature (1)H and (13)C NMR spectra. For complex 1, the thioureide vCN value is shifted to higher wavenumber compared to 2 and N(13)CS2 carbon signal observed for 1 is additionally shielded compared to the parent complex 2, suggesting increased strength of the thioureide bond due to the presence of the π-accepting phosphine. In the room temperature (13)C NMR spectrum of 1, two pseudo doublets are observed in the aliphatic region. Variable temperature (13)C NMR spectral studies suggest that the fast thiocyanate exchange appears to be responsible for the appearance of pseudo doublets. Single crystal X-ray structural analysis of 1 and 2 confirm the presence of four coordinated nickel in a distorted square planar arrangement with the NiS2PN and NiS4 chromophores, respectively. The NiS bonds are symmetric in 2 (2.1914(14) and 2.2073(13)Å). But significant asymmetry in NiS bond distances was observed in 1 (2.2202(8)Å and 2.1841Å). This observation clearly supports the less effective trans effect of SCN(-) over PPh3. Cyclic voltammetric studies revealed easier reduction of nickel(II) to nickel(I) in complex 1 compared to 2. PMID:24747850

  1. Crystal Structure of 8-Demethoxyrunanine

    Institute of Scientific and Technical Information of China (English)

    WANG Xiao-Ling

    2008-01-01

    A new hasubanane-type alkaloid, 8-demethoxyrunanine, was isolated from Sino- menium acutum and characterized by melting point, HREIMS, 1H NMR, and X-ray diffraction analysis. X-ray diffraction reveals that the title compound crystallizes in the orthorhombic system, space group P212121 with a = 7.308(1), b = 21.742(5), c = 22.893(4) ?, V = 3637.5(11) ?3, Z = 8, Dx = 1.254 g/cm3, F(000) = 1472, μ(MoKα) = 0.087 mm-1, the final R = 0.0438 and wR = 0.0575 for 4497 independent reflections with Rint = 0.0192 and 2091 observed reflections with I > 2σ(I). Four rings (ring A: one benzene ring, ring B: one hexagon carbon ring in a half-chair conformation, ring C: one hexagon carbon ring with α,β-unsaturated ketone segment (-CR2=CR1-C=O) in a screw-boat conformation, and ring D: one nonplanar tetrahydropyrrole) form a hasubanane-type alkaloid.

  2. Synthesis,Characterization and X-ray Crystal Structure of N,N'-Bis(4-nitrophenylcarba-mothioyl)-isophthalamide·DMF

    Institute of Scientific and Technical Information of China (English)

    WANG Hai-Qin; CHEN Le; PENG Hao; HE Hong-Wu

    2011-01-01

    A new crystal of N,N'-bis(4-nitrophenylcarbamothioyl)isophthalamide DMF solva-te has been prepared at room temperature and characterized by elemental analysis and IR,MS,1H NMR spectra and X-ray single-crystal determination.The complex crystallizes in monoclinic,space group P21/c with a = 11.2093(12),b = 22.081(2),c = 13.9640(15) ,β= 112.128(2)°,V = 3201.8(6) 3,C28H30N8O8S2,Mr = 670.72,Dc = 1.391 Mg/m3,Z = 4,μ= 0.228 mm-1,F(000) = 1400,the final R = 0.0483 and wR = 0.1411(I 2σ(I)).The molecular packing in the crystal is the result of N-H…O hydrogen bonding.

  3. Photonic crystal laser-driven accelerator structures

    CERN Document Server

    Cowan, Benjamin

    2005-01-01

    We discuss simulated photonic crystal structure designs, including two- and three-dimensional planar structures and fibers. The discussion of 2D structures demonstrates guiding of a speed-of-light accelerating mode by a defect in a photonic crystal lattice and reveals design considerations and trade-offs. With a three-dimensional lattice, we introduce a candidate geometry and discuss beam dynamics, coupling, and manufacturing techniques for that structure. In addition we discuss W-band scale tests of photonic crystal structures. The computational methods are also discussed.

  4. 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.

  5. Crystal Structure of Isoquinoline Derivatives

    Institute of Scientific and Technical Information of China (English)

    LUO Mei; ZHANG Jia-Hai; ZHOU Shi-Ming; SUN Jie; YIN Hao; HU Ke-Liang

    2011-01-01

    The chiral compound 5H-imidazol[2,3-b]isoquinoline-l-ethanol-5-one-1,2, 3, 10b-tetrahydro- β(S)-phenyl-3(S)-phenyl was synthesized from the direct condensation of 2- cyanophenyacetonitrile with optically active (S)-(+)-2-phenylglycinol in chlorobenzene under dry, anaerobic conditions. ZnCl2 was used as a Lewis acid catalyst in this reaction, and the structure of this compound was determined by X-ray diffraction, NMR, MS and IR. Crystal data of the title compound: C25H22N2O2, Mr = 382.45, P 21 21 21, a = 5.341(5), b = 16.735(5), c = 22.129(5) A, γ = 90°, V = 1978(2)A^3, Z = 4, Dc = 1.284 g/cm^3, the final R = 0.0321 for 2269 observed reflections with I 〉 2 σ(I) and Rw = 0.0771 for all data.

  6. Crystal Structure of Chabazite K

    International Nuclear Information System (INIS)

    The crystal structure of the chabazite K with the formula (K1.33Na1.02Ca0.84)[Al4Si8O24] · 12.17H2O from late hydrothermalites in the Khibiny alkaline massif (Kola Peninsula) is established by X-ray diffraction analysis (CAD4 four-circle diffractometer, λMoKα radiation, graphite monochromator, T = 193 K, 2θmax = 70 deg., R1 = 0.047 for 4745 reflections) on the basis of experimental data (6265 reflections) obtained from a twin (twinning parameter 0.535(1)): a = 13.831(3) A, c = 15.023(5) A, sp. gr. R3-barm, Z = 3, ρcalcd = 2.016 g/cm3 . It is shown that cations occupy five independent positions in large cavities of the tetrahedral Al,Si,O anionic framework in potassium-rich chabazite. A comparative crystallochemical analysis of chabazites of different composition and origin is performed

  7. Crystal structure of benzimidazolium salicylate

    Directory of Open Access Journals (Sweden)

    M. Amudha

    2015-10-01

    Full Text Available In the anion of the title molecular salt, C7H7N2+·C7H5O3− (systematic name: 1H-benzimidazol-3-ium 2-hydroxybenzoate, there is an intramolecular O—H...O hydrogen bond that generates an S(6 ring motif. The CO2 group makes a dihedral angle of 5.33 (15° with its attached ring. In the crystal, the dihedral angle between the benzimidazolium ring and the anion benzene ring is 75.88 (5°. Two cations bridge two anions via two pairs of N—H...O hydrogen bonds, enclosing an R44(16 ring motif, forming a four-membered centrosymmetric arrangement. These units are linked via C—H...O hydrogen bonds, forming chains propagating along the b-axis direction. The chains are linked by C—H...π and π–π interactions [inter-centroid distances = 3.4156 (7 and 3.8196 (8 Å], forming a three-dimensional structure.

  8. Structural Characterization of Lateral-grown 6H-SiC am-plane Seed Crystals by Hot Wall CVD Epitaxy

    Science.gov (United States)

    Goue, Ouloide Yannick; Raghothamachar, Balaji; Dudley, Michael; Trunek, Andrew J.; Neudeck, Philip G.; Woodworth, Andrew A.; Spry, David J.

    2014-01-01

    The performance of commercially available silicon carbide (SiC) power devices is limited due to inherently high density of screw dislocations (SD), which are necessary for maintaining polytype during boule growth and commercially viable growth rates. The NASA Glenn Research Center (GRC) has recently proposed a new bulk growth process based on axial fiber growth (parallel to the c-axis) followed by lateral expansion (perpendicular to the c-axis) for producing multi-faceted m-plane SiC boules that can potentially produce wafers with as few as one SD per wafer. In order to implement this novel growth technique, the lateral homoepitaxial growth expansion of a SiC fiber without introducing a significant number of additional defects is critical. Lateral expansion is being investigated by hot wall chemical vapor deposition (HWCVD) growth of 6H-SiC am-plane seed crystals (0.8mm x 0.5mm x 15mm) designed to replicate axially grown SiC single crystal fibers. The post-growth crystals exhibit hexagonal morphology with approximately 1500 m (1.5 mm) of total lateral expansion. Preliminary analysis by synchrotron white beam x-ray topography (SWBXT) confirms that the growth was homoepitaxial, matching the polytype of the respective underlying region of the seed crystal. Axial and transverse sections from the as grown crystal samples were characterized in detail by a combination of SWBXT, transmission electron microscopy (TEM) and Raman spectroscopy to map defect types and distribution. X-ray diffraction analysis indicates the seed crystal contained stacking disorders and this appears to have been reproduced in the lateral growth sections. Analysis of the relative intensity for folded transverse acoustic (FTA) and optical (FTO) modes on the Raman spectra indicate the existence of stacking faults. Further, the density of stacking faults is higher in the seed than in the grown crystal. Bundles of dislocations are observed propagating from the seed in m-axis lateral directions

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

    International Nuclear Information System (INIS)

    The stannides CuLi2Sn (CSD-427095) and Cu2LiSn (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 Cu2Sn lattices form channels which host Cu and Li atoms at partly mixed occupied positions exhibiting extensive vacancies. For CuLi2Sn, the space group F-43m. was verified (structure type CuHg2Ti; a=6.295(2) Å; wR2(F²)=0.0355 for 78 unique reflections). The 4(c) and 4(d) positions are occupied by Cu atoms and Cu+Li atoms, respectively. For Cu2LiSn, the space group P63/mmc was confirmed (structure type InPt2Gd; a=4.3022(15) Å, c=7.618(3) Å; wR2(F²)=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. - Highlights: • First single crystal investigation of CuLi2Sn and Cu2LiSn clarifies contradictions from literature. • Lithium atoms are ordered in channels, which is interesting for application as anode materials for lithium ion batteries. • Structural relationships to binary Cu–Sn-phases are shown. • Close structural relationship between both ternary phases exists

  11. Neutron diffraction analysis of crystal magnetic structures

    International Nuclear Information System (INIS)

    An investigation of the state-of-the art of the neutron diffraction analysis of magnetic structures from the point of view of the theory of crystal symmetry is given. Various and numerous structures determined from the neutron diffraction analysis investigations can be classified and described with the theory of space group representations of crystals. The analysis of quite a number of various magnetic structures shows that they arise according to Landau hypothesis. The foundations of a symmetry analysis of magnetic structures and the methods for their determination are given. A physical explanation is given for the existence of magnetic structures. The experimental investigations of the crystal lattice distortions accompanying a magnetic ordering are reviewed. In this review is given a symmetry approach to the description of the magnetic structures of crystals; and a possibility to analyze them by a scattering of nonpolarized and polarized neutrons

  12. Modelling molecular flexibility for crystal structure prediction

    OpenAIRE

    Uzoh, O. G.

    2015-01-01

    In the crystal packing of molecules wherein a single bond links aromatic groups, a change in the torsion angle can optimise close packing of the molecule. The improved intermolecular interactions, Uinter, outweigh the conformational energy penalty, ΔEintra, to give a more stable lattice energy, Elatt = Uinter + ΔEintra. This thesis uses this lattice energy model hierarchically in a new Crystal Structure Prediction (CSP) algorithm, CrystalPredictor version 1.6, which varies the low-barrier tor...

  13. Synthesis, single crystal structure, spectroscopic characterization and molecular properties of (2E)-3-(2,6-dichlorophenyl)-1-(3,4-dimethoxyphenyl)prop-2-en-1-one

    Science.gov (United States)

    Chidan Kumar, C. S.; Quah, Ching Kheng; Balachandran, V.; Fun, Hoong-Kun; Asiri, A. M.; Chandraju, Siddegowda; Karabacak, Mehmet

    2016-07-01

    A novel (2E)-3-(2,6-dichlorophenyl)-1-(3,4-dimethoxyphenyl)prop-2-en-1-one (DCPDMP) compound has been synthesized and its single crystal has been grown by slow evaporation technique. The structure of the compound has been characterized by FT-IR, FT-Raman and single-crystal X-ray diffraction techniques. The optimized molecular structure, vibrational wavenumbers, corresponding vibrational assignments of the compound have been investigated by means of the density functional theory. The molecule crystallizes in triclinic system, space group P-1 with a = 7.6179 (7), b = 8.5023 (7), c = 12.1967 (10) Å, V = 764.39 (11) Å3 and two molecules in the unit cell. The crystal structure is primarily stabilized through intramolecular C-H … Cl and C-H … O hydrogen bonds and intermolecular C-H … O and weak C-H … π interactions. These inter- and intramolecular interactions are analyzed. Moreover, the molecular electrostatic potential surface of the molecule has been constructed. Global and local reactivity descriptors and dipole moment (μ), static polarizability (α), first order hyperpolarizability (β) and optical gap (ΔE) have been also calculated to study the nonlinear optical (NLO) property of the title compound.

  14. 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.

  15. Synthesis, characterization, crystal structure and solution studies of a novel proton transfer (charge transfer) complex of 2,2‧-dipyridylamine with 2,6-pyridine dicarboxylic acid

    Science.gov (United States)

    Ghasemi, Khaled; Rezvani, Ali Reza; Shokrollahi, Ardeshir; Zarghampour, Fereshteh; Moghimi, Abolghasem; García-Granda, Santiago; Mendoza-Meroño, Rafael

    2015-06-01

    Reaction between 2,2‧-dipyridylamine (DPA) and 2,6-pyridine dicarboxylic acid (dipicolinic acid, dipicH2), in water results in the formation of a proton transfer or charge transfer (CT) complex, (DPAH)+(dipicH)-·H2O, 1. The characterization was performed using 1H NMR and FTIR spectroscopy, elemental analysis and X-ray crystallography. The crystal system is triclinic with space group P1. The structural investigations exhibit that the hydrogen bonds and π-π stacking interactions stabilize the crystal structure of proton transfer complex. The protonation constants of 2,6-pyridine dicarboxylic acid, 2,2‧-dipyridylamine and the equilibrium constants for dipic-DPA (1:1) proton transfer system were calculated by potentiometric pH titration method using Hyperquad2008 program. The stoichiometries of the proton transfer species in solution was in agreement with the solid state result.

  16. Crystal structure of human GDF11.

    Science.gov (United States)

    Padyana, Anil K; Vaidialingam, Bhamini; Hayes, David B; Gupta, Priyanka; Franti, Michael; Farrow, Neil A

    2016-03-01

    Members of the TGF-β family of proteins are believed to play critical roles in cellular signaling processes such as those involved in muscle differentiation. The extent to which individual family members have been characterized and linked to biological function varies greatly. The role of myostatin, also known as growth differentiation factor 8 (GDF8), as an inhibitor of muscle differentiation is well understood through genetic linkages. In contrast, the role of growth differentiation factor 11 (GDF11) is much less well understood. In humans, the mature forms of GDF11 and myostatin are over 94% identical. In order to understand the role that the small differences in sequence may play in the differential signaling of these molecules, the crystal structure of GDF11 was determined to a resolution of 1.50 Å. A comparison of the GDF11 structure with those of other family members reveals that the canonical TGF-β domain fold is conserved. A detailed structural comparison of GDF11 and myostatin shows that several of the differences between these proteins are likely to be localized at interfaces that are critical for the interaction with downstream receptors and inhibitors. PMID:26919518

  17. Synthesis, characterization and crystal structures of two polymorphs of the iodo-bridged ruthenium salt, μ-iodido-bis{η5-cyclopentadienyl-dicarbonyl-ruthenium(II)} tetrafluoroborate

    Science.gov (United States)

    Nyawade, Eunice A.; Friedrich, Holger B.; M'thiruaine, Cyprian M.; Omondi, Bernard

    2013-09-01

    The reaction of RpI (Rp = (η5-C5H5)Ru(CO)2) and AgBF4 in two different solvents, tetrahydrofuran and dichloromethane afforded two polymorphs of the iodo-bridged cationic complex [Rp2I]BF4. Polymorph I precipitates out of solution as yellow broad-shaped blocks while polymorph II crystallises out as thin-shaped blocks. While I crystallizes in the monoclinic P2/c space group with a = 12.0982(5) Å, b = 9.7923(4) Å, c = 15.5321(6) Å, β = 102.9880(10)°, polymorph (II) crystallizes in the monoclinic P21/c with a = 7.00560(10) Å, b = 14.1446(3) Å, c = 18.2226(3) Å, β = 96.2390(10)°. The IR spectra of the compound showed the presence of terminal carbonyl groups but the absence of bridging carbonyl groups. Thermal studies of the two polymorphs reveal very close melting points, 432.2 and 435.2 K for I and II respectively. The enthalpies associated with their melting points are +15.1 kJ mol-1 and +21.9 kJ mol-1 for polymorphs I and II, respectively. ESI-mass spectroscopy showed the presence of a number of statistically possible combinations of the cationic species. The two polymorphs have also been characterized using DSC, IR and NMR.

  18. Synthesis, Characterization, and Crystal Structure Determination of a New Indium (III) Complex: [In(5,5’-DiMeBiPy)Cl3(DMSO)].2(DMSO)

    OpenAIRE

    Sadif A. Shirvan; Fereydoon Khazali; Sara Haydari Dezfuli

    2014-01-01

    [In(5,5’-DiMeBiPy)Cl3(DMSO)].2(DMSO) complex (5,5’-DiMeBiPy is 5,5’-Dimethyl-2,2’-bipyridine) was prepared from reaction of InCl3.4H2O with 5,5’-DiMeBiPy in 1.1 molar ratio in DMSO. This compound has been characterized by IR, 1H NMR, UV-Vis spectroscopy as well as X-ray crystallography. This compound crystallizes in the space group Pī of the triclinic system. The unit cell dimensions is: a = 8.6695(8) Å, b = 12.8456(14) Å, c = 13.0877(12) Å, a = 78.258(8)º, β = 85.270(8)º, g = 74.932(8)º. Acc...

  19. Growth and characterization of gel grown pure and mixed iron–manganese levo-tartrate crystals

    Indian Academy of Sciences (India)

    S J Joshi; B B Parekh; K D Vohra; M J Joshi

    2006-06-01

    Several applications of iron tartrate and manganese tartrate compounds are reported in the literature. In the present investigation, we have grown pure and mixed iron (II)–manganese levo-tartrate crystals by single diffusion gel growth technique. Crystals with spherulitic morphology were harvested. The colouration of the crystals changed from black to pinkish brown upon increasing the content of manganese in the crystals. The crystals were characterized by FTIR spectroscopy, powder XRD, TGA, VSM and dielectric study. Crystal structures of different mixed crystals were studied. From TGA it was observed that on heating the hydrated crystals became anhydrous and then converted into oxides. Paramagnetic nature of the crystals was revealed from VSM study. The variation of the dielectric constant with frequency was studied. The results are discussed.

  20. Crystal structure of cyclohexylammonium thiocyanate

    OpenAIRE

    Abdulaziz A. Bagabas; Sultan B. Alhoshan; Hazem A. Ghabbour; C S Chidan Kumar; Hoong-Kun Fun

    2015-01-01

    In the title salt, C6H11NH3+·SCN−, the cyclohexylammonium ring adopts a slightly distorted chair conformation. The ammonium group occupies an equatorial position to minimize 1,3 and 1,5 diaxial interactions. In the crystal, the components are linked by N—H...N and N—H...S hydrogen-bonding interactions, resulting in a three-dimensional network.

  1. Crystal structure of cyclohexylammonium thiocyanate

    Directory of Open Access Journals (Sweden)

    Abdulaziz A. Bagabas

    2015-01-01

    Full Text Available In the title salt, C6H11NH3+·SCN−, the cyclohexylammonium ring adopts a slightly distorted chair conformation. The ammonium group occupies an equatorial position to minimize 1,3 and 1,5 diaxial interactions. In the crystal, the components are linked by N—H...N and N—H...S hydrogen-bonding interactions, resulting in a three-dimensional network.

  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. The hydride fluoride crystal structure database, HFD

    Energy Technology Data Exchange (ETDEWEB)

    Gingl, F.; Gelato, L.; Yvon, K. [Geneva Univ. (Switzerland). Lab. Crystallographie aux Rayons X

    1997-05-20

    HFD is a new data base containing crystal structure information on more than one thousand metal hydrides and fluorides. It includes space group, cell parameters, standardized atom positions, site occupancies and references. The compilation is critical as only refined crystal structures are considered and the data are checked for internal consistency. It is comprehensive as structural information is extracted from all major scientific journals, and it is continuously updated. HFD can be searched according to various criteria such as symmetry, chemical elements, composition etc. The primary motivation for creating HFD was to predict new metal hydrides and to study their structural analogies with metal fluorides. However, HFD can also be used for other applications such as the simulation of diffraction patterns and the drawing of crystal structures. (orig.) 13 refs.

  4. Pholcodine monohydrate: Crystal structure and polymorphism

    Science.gov (United States)

    Petruševski, Gjorgji; Zbačnik, Marija; Kajdžanoska, Marina; Ugarkovic, Sonja; Trimčeski, Vase; Kaitner, Branko; Jovanovski, Gligor; Makreski, Petre

    2013-07-01

    The first crystal structure elucidation of pholcodine monohydrate, an important antitussive active pharmaceutical ingredient is reported herein. The studied compound crystallizes in the orthorhombic system in the space group P212121. Each H2O molecule is shared by two pholcodine molecules via three strong hydrogen bonds. The detailed crystallization screening from several different organic solvents afforded single crystals with various quality, all exhibiting prism-to-needlelike micro morphology. The investigation of the obtained single crystals by means of several physico-chemical, solid-state instrumental techniques (FT-IR, DSC, TG/DTG and XRPD) proved that pholcodine monohydrate exists in a single crystalline modification, identical to the commercial form of the compound.

  5. Nucleation and structural growth of cluster crystals

    CERN Document Server

    Leitold, Christian

    2016-01-01

    We study the nucleation of crystalline cluster phases in the generalized exponential model with exponent n=4. Due to the finite value of this pair potential for zero separation, at high densities the system forms cluster crystals with multiply occupied lattice sites. Here, we investigate the microscopic mechanisms that lead to the formation of cluster crystals from a supercooled liquid in the low-temperature region of the phase diagram. Using molecular dynamics and umbrella sampling, we calculate the free energy as a function of the size of the largest crystalline nucleus in the system, and compare our results with predictions from classical nucleation theory. Employing bond-order parameters based on a Voronoi tessellation to distinguish different crystal structures, we analyze the average composition of crystalline nuclei. We find that even for conditions where a multiply-occupied fcc crystal is the thermodynamically stable phase, the nucleation into bcc cluster crystals is strongly preferred. Furthermore, w...

  6. Fabrication and characterization of three-dimensional infrared photonic crystals

    Science.gov (United States)

    Zavieh, Lisa

    It has been predicted theoretically that photonic crystals can be used to control the propagation of light through dielectric media for wavelengths extending beyond the microwave to include the infrared and the visible. Fabrication of 3-D photonic crystals with a bandgap in the near infrared or visible would have application in the design of a new class of photonic devices that include optical mirrors, waveguides, and cavity resonators. Demonstrations of 3-D photonic crystals have been limited primarily to the microwave and infrared wavelength regimes because of the constraints imposed by the nanometer scale dimensions required for operation in the visible. This thesis presents a novel method of fabricating a simple cubic photonic crystal which potentially can be tailored to operate at any wavelength. Fabrication was broken down into several processing steps, each of which was investigated independently. Design of Experiment (DOE) was used in a parametric study to optimize dry etching conditions by which GaAs/AlxGa1--x As multilayer structures were etched with anisotropic profile and rapid etch rate. Also, the etching properties of diffusion controlled wet lateral etching of buried AlxGa1--xAs layers in hydrofluoric acid solutions (HF) were investigated. Using the results obtained from the etching studies, both dry and wet etching techniques were employed to fabricate the simple-cubic photonic structure. Following fabrication, the photonic crystal was characterized at normal angles and oblique incidence using Fourier transform infrared spectroscopy (FTIR). The experimental results show strong correlation to theoretically predicted values. The simplicity of the process and positive results indicate that it may be possible to scale down the structure to obtain an photonic band lattice with a bandgap of 1.55 mum.

  7. Synthesis, crystal structure, and characterization of two-dimensional coordination polymers of three heavy rare-earth elements: [RE(5-Nip)(5-HNip)(H2O)2](H2O)2 (RE = Y, Ho, Er)

    International Nuclear Information System (INIS)

    Three new coordination polymers, [RE(5-Nip)(5-HNip)(H2O)2] · 2H2O (RE = Y (I), Ho (II), and Er (III)) were synthesized by hydrothermal reactions of lanthanide nitrates with 5-nitroisophthalic acid (H2Nip), and characterized by IR spectra, elemental analysis, and single-crystal X-ray diffraction. X-ray diffraction studies suggest that all the two-dimensional 5-nitroisophthalic complexes crystallize in the P1-bar space group and are isomorphic. The two-dimensional layer-like structures are constructed by the lanthanide ions bridged by 5-Nip2- ligands, and the layers further packed into 3D complexes through hydrogen bonds and two kinds of π-π stacking interactions. These complexes exhibit high stabilities up to 465 (1), 518 (2), and 528 deg C (3), respectively

  8. Copper(II) ion catalytic oxidation of o-phenylenediamine and characterization, X-ray crystal structure and solution studies of the final product [DAPH][H3O][Cu(dipic)2]·3H2O

    Science.gov (United States)

    Ghasemi, Khaled; Rezvani, Ali Reza; Shokrollahi, Ardeshir; Abdul Razak, Ibrahim; Refahi, Masoud; Moghimi, Abolghasem; Rosli, Mohd Mustaqim

    2015-09-01

    The complex [DAPH][H3O][Cu(dipic)2]·3H2O, (1) (dipicH2 = 2,6-pyridinedicarboxylic acid and DAP = 2,3-diaminophenazine) was prepared from the reaction of Cu(NO3)2·2H2O with mixture of o-phenylenediamine (OPD) and 2,6-pyridinedicarboxylic acid in water. The complex was characterized by FTIR, elemental analysis, UV-Vis and the single-crystal X-ray diffraction. The crystal system is monoclinic with the space group P21/c. This complex is stabilized in the solid state by an extensive network of hydrogen bonds between crystallized water, anionic and cationic fragments, which form a three-dimensional network. Furthermore, hydrogen bonds, π⋯π and Csbnd O⋯π stacking interactions seem to be effective in stabilizing the crystal structures. The protonation constants of dipic (L) and DAP (Q), the equilibrium constants for the dipic-DAP proton transfer system and the stoichiometry and stability constants of binary complexes including each of ligands (dipic, DAP) in presence Cu2+ ion, ternary complexes including, both of ligands (dipic-DAP) in presence of metal ion were calculated in aqueous solutions by potentiometric pH titration method using the Hyperquad2008 program. The stoichiometry of the most complexes species in solution was found to be very similar to the solid-state of cited metal ion complex.

  9. Crystal structure of 2-pentyloxybenzamide

    OpenAIRE

    Bernhard Bugenhagen; Yosef Al Jasem; Thies Thiemann

    2014-01-01

    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...

  10. Structural characterization of two benzene-1,2-di­amine complexes of zinc chloride: a mol­ecular compound and a co-crystal salt

    Science.gov (United States)

    Zick, Patricia L.; Geiger, David K.

    2016-01-01

    The structures of two zinc complexes containing bidentate benzene-1,2-di­amine ligands are reported. (Benzene-1,2-di­amine-κ2 N,N′)di­chloro­idozinc, [ZnCl2(C6H8N2)], (I), displays a distorted tetra­hedral coordination sphere for the metal cation. The di­amine ligand and the Zn atom reside on a crystallographic mirror plane. In the 1:1 co-crystal salt trans-di­aqua­bis­(4,5-di­methyl­benzene-1,2-di­amine-κ2 N,N′)zinc chloride–4,5-di­methyl­benzene-1,2-di­amine (1/1), [Zn(C8H12N2)2(H2O)2]Cl2·2C8H12N2, (II), the zinc(II) complex cation exhibits a tetra­gonally distorted octa­hedral coordination sphere. The Zn atom sits on a crystallographically imposed inversion center and the di­amine ligands are tilted 30.63 (6)° with respect to the ZnN4 plane. Both complexes exhibit extensive hydrogen bonding. In (I), a stacked-sheet extended structure parallel to (101) is observed. In (II), the co-crystallized di­amine is hydrogen-bonded to the complex cation via O—H⋯N and N—H⋯N linkages. These units are in turn linked into planes along (200) by O—H⋯Cl and N—H⋯Cl hydrogen bonds. PMID:27555958

  11. Structural characterization of two benzene-1,2-di-amine complexes of zinc chloride: a mol-ecular compound and a co-crystal salt.

    Science.gov (United States)

    Zick, Patricia L; Geiger, David K

    2016-07-01

    The structures of two zinc complexes containing bidentate benzene-1,2-di-amine ligands are reported. (Benzene-1,2-di-amine-κ(2) N,N')di-chloro-idozinc, [ZnCl2(C6H8N2)], (I), displays a distorted tetra-hedral coordination sphere for the metal cation. The di-amine ligand and the Zn atom reside on a crystallographic mirror plane. In the 1:1 co-crystal salt trans-di-aqua-bis-(4,5-di-methyl-benzene-1,2-di-amine-κ(2) N,N')zinc chloride-4,5-di-methyl-benzene-1,2-di-amine (1/1), [Zn(C8H12N2)2(H2O)2]Cl2·2C8H12N2, (II), the zinc(II) complex cation exhibits a tetra-gonally distorted octa-hedral coordination sphere. The Zn atom sits on a crystallographically imposed inversion center and the di-amine ligands are tilted 30.63 (6)° with respect to the ZnN4 plane. Both complexes exhibit extensive hydrogen bonding. In (I), a stacked-sheet extended structure parallel to (101) is observed. In (II), the co-crystallized di-amine is hydrogen-bonded to the complex cation via O-H⋯N and N-H⋯N linkages. These units are in turn linked into planes along (200) by O-H⋯Cl and N-H⋯Cl hydrogen bonds. PMID:27555958

  12. Crystal structure of L-alanine phosphate

    International Nuclear Information System (INIS)

    The crystal structure of L-alanine phosphate (C3O2NH7 · H3PO4) is determined by the single-crystal diffraction technique; a 11.918(1) A, b = 9.117(1) A, c = 7.285(1) A, γ = 104.7(1) deg., space group P21, and Z = 4. The amino group of the alanine is protonated by the hydrogen atom of the phosphoric acid. Pairs of H2PO-4 hydrogen-bonded ions are packed into layers alternating with layers of alanine molecules in the crystal. No hydrogen bonds are formed immediately between the alanine molecules

  13. Crystal and molecular structure of paclitaxel (taxol).

    OpenAIRE

    Mastropaolo, D; Camerman, A; Luo, Y.; Brayer, G. D.; Camerman, N

    1995-01-01

    Paclitaxel (formerly called taxol), an important anticancer drug, inhibits cell replication by binding to and stabilizing microtubule polymers. As drug-receptor interactions are governed by the three-dimensional stereochemistries of both participants, we have determined the crystal structure of paclitaxel to identify its conformational preferences that may be related to biological activity. The monoclinic crystals contain two independent paclitaxel molecules in the asymmetric unit plus severa...

  14. Isolation, Co-Crystallization and Structure-Based Characterization of Anabaenopeptins as Highly Potent Inhibitors of Activated Thrombin Activatable Fibrinolysis Inhibitor (TAFIa).

    Science.gov (United States)

    Schreuder, Herman; Liesum, Alexander; Lönze, Petra; Stump, Heike; Hoffmann, Holger; Schiell, Matthias; Kurz, Michael; Toti, Luigi; Bauer, Armin; Kallus, Christopher; Klemke-Jahn, Christine; Czech, Jörg; Kramer, Dan; Enke, Heike; Niedermeyer, Timo H J; Morrison, Vincent; Kumar, Vasant; Brönstrup, Mark

    2016-01-01

    Mature thrombin activatable fibrinolysis inhibitor (TAFIa) is a carboxypeptidase that stabilizes fibrin clots by removing C-terminal arginines and lysines from partially degraded fibrin. Inhibition of TAFIa stimulates the degradation of fibrin clots and may help to prevent thrombosis. Applying a lead finding approach based on literature-mining, we discovered that anabaenopeptins, cyclic peptides produced by cyanobacteria, were potent inhibitors of TAFIa with IC50 values as low as 1.5 nM. We describe the isolation and structure elucidation of 20 anabaenopeptins, including 13 novel congeners, as well as their pronounced structure-activity relationships (SAR) with respect to inhibition of TAFIa. Crystal structures of the anabaenopeptins B, C and F bound to the surrogate protease carboxypeptidase B revealed the binding modes of these large (~850 Da) compounds in detail and explained the observed SAR, i.e. the strong dependence of the potency on a basic (Arg, Lys) exocyclic residue that addressed the S1' binding pocket, and a broad tolerance towards substitutions in the pentacyclic ring that acted as a plug of the active site. PMID:27604544

  15. Growth and characterization of struvite-K crystals

    Energy Technology Data Exchange (ETDEWEB)

    Chauhan, C.K.; Vyas, P.M.; Joshi, M.J. [Crystal Growth Laboratory, Department of Physics, Saurashtra University, Rajkot - 360 005, Gujarat (India)

    2011-02-15

    Struvite-K is the natural potassium equivalent to Struvite. Struvite-K crystals were grown by single diffusion gel growth technique in silica hydro gel medium. Struvite-K crystals with different morphologies having transparent to translucent diaphaneity were grown with different growth parameters. The phenomenon of Liesegang rings was also observed with some particular growth parameters. The crystals were characterized by powder XRD, FT-IR, TGA and dielectric study. The powder XRD results of Struvite-K confirmed the orthorhombic crystal structure. The FT-IR spectrum proved the presence of water of hydration, metal - oxygen bond and P - O bond. The TGA, DSC and DTA were carried out simultaneously. It was found that crystals started dehydrating and decomposing from 75 C and finally at 600 C temperature it became 64.14% of the original weight and remained almost constant up to the end of analysis. From the thermo-gravimetry, the numbers of the water molecules associated with the crystal were calculated and found to be 5. The kinetic and thermodynamic parameters of dehydration / decomposition process were calculated. The variation of dielectric constant with frequency of applied field was studied in the range from 400 Hz to 100 kHz, which exhibited the decreasing nature of the dielectric constant as frequency increased. The dielectric study showed that a.c. conductivity increased and consequently the a.c. resistivity decreased with the increase in frequency. (copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  16. 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.

  17. Characterization of the cofactor-binding site in the SPOUT-fold methyltransferases by computational docking of S-adenosylmethionine to three crystal structures

    Directory of Open Access Journals (Sweden)

    Debski Janusz

    2003-03-01

    Full Text Available Abstract Background There are several evolutionarily unrelated and structurally dissimilar superfamilies of S-adenosylmethionine (AdoMet-dependent methyltransferases (MTases. A new superfamily (SPOUT has been recently characterized on a sequence level and three structures of its members (1gz0, 1ipa, and 1k3r have been solved. However, none of these structures include the cofactor or the substrate. Due to the strong evolutionary divergence and the paucity of experimental information, no confident predictions of protein-ligand and protein-substrate interactions could be made, which hampered the study of sequence-structure-function relationships in the SPOUT superfamily. Results We used the computational docking program AutoDock to identify the AdoMet-binding site on the surface of three MTase structures. We analyzed the sequence divergence in two distinct lineages of the SPOUT superfamily in the context of surface features and preferred cofactor binding mode to propose specific function for the conserved residues. Conclusion Our docking analysis has confidently predicted the common AdoMet-binding site in three remotely related proteins structures. In the vicinity of the cofactor-binding site, subfamily-conserved grooves were identified on the protein surface, suggesting location of the target-binding/catalytic site. Functionally important residues were inferred and a general reaction mechanism, involving conformational change of a glycine-rich loop, was proposed.

  18. Novel decavanadate cluster complex (HImz)12(V10O28)2·3H2O: Synthesis, characterization, crystal structure, optical and thermal properties

    Science.gov (United States)

    Omri, Issam; Mhiri, Tahar; Graia, Mohsen

    2015-10-01

    A novel decavanadate with organic cations, (HImz)12(V10O28)2·3H2O (Imz: Imidazole), has been synthesized in aqueous solution and characterized by IR, Raman and UV-Vis spectroscopies and single crystal X-Ray diffraction. The asymmetric unit of (HImz)12(V10O28)2·3H2O is composed of two decavanadates [V10O28]6- anions, twelve imidazolium (C3H5N2)+ cations and water molecules. The cohesion is provided by two types of bonds: hydrogen bonds O-H---N, O-H---O and N-H---O involving water molecules and organic molecules, and Vander Waals bonds for the connection between the organic molecules. The IR and Raman spectra proved the presence of organic cations, decavanadate (V10O28)6- groups and water molecules. The UV-Vis diffuse reflectance spectrum shows that this compound exhibits semiconducting behavior with an optical band gap of 2.54 eV. TGA curves indicate that the weight loss of this compound can be divided into four stages.

  19. Syntheses, Characterizations, Crystal Structures and Antibacterial Activities of Two Zinc(Ⅱ) Complexes with a Schiff Base Derived from o-Vanillin and p-Toluidine

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    Two new zinc(Ⅱ) complexes, [Zn2L2aCl4]·2[ZnL(CH3OH)Cl2] 1 and [ZnL2(NO3)2] 2,were synthesized by reacting ZnX2·nH2O (X = Cl-, NO3-) and a Schiff base ligand 2-[(4-me-thylphenylimino)methyl]-6-methoxyphenol (C15H15NO2, L) which was obtained by the condensation of o-vanillin (2-hydroxy-3-methoxybenzaldehyde) with p-toluidine. Both 1 and 2 were characterized by single-crystal X-ray diffraction technique, elemental analysis, molar conductance, FT-IR, UV-Vis,1H-NMR spectra and thermogravimetric analysis. The Schiff base ligand and its zinc(Ⅱ) complexes have been tested in vitro to evaluate their antibacterial activity against bacteria, viz., Escherichia Coli,Staphylococcus aureus and Bacillus Subtilis. The results show that these complexes have higher activity than the corresponding free Schiff base ligand against the same bacteria.

  20. Characterization of the (0001) cleavage surface of antimony single crystals using scanning probe microscopy: Atomic structure, vacancies, cleavage steps, and twinned interlayers

    Science.gov (United States)

    Stegemann, Bert; Ritter, Claudia; Kaiser, Bernhard; Rademann, Klaus

    2004-04-01

    Atomically resolved scanning tunneling microscopy images of the unreconstructed hexagonal structure of surface atoms on Sb(0001) are presented. Lateral and vertical lattice parameters have been determined. The interatomic spacing of 4.31 Å (±0.05 Å) on the Sb(0001) surface corresponds to the known bulk data. Cleavage has been found to occur always between adjacent double layers, yielding at least diatomic cleavage steps of 3.75 Å (±0.10 Å) height. Different kinds of defect structures on the cleavage plane have been imaged with atomic resolution. Point defects, caused by a single or by three missing surface atoms, have been uncovered. Stable imaging of cleavage steps, which were found to be straight along the atomic rows, has been achieved. Twinned interlayers formed upon cleavage of Sb even at room temperature have been revealed by atomic force microscopy. The mean twinning angle of 2.42° (±0.20°) is quantitatively in accord with the value of 2.45° predicted by the model of twinning in Sb crystals. The observed features are discussed with respect to other layered materials and with regard to their relevance for the use of Sb(0001) as a support of nanostructures.

  1. Lessons from crystal structures of kainate receptors

    DEFF Research Database (Denmark)

    Møllerud, Stine; Frydenvang, Karla Andrea; Pickering, Darryl S;

    2016-01-01

    structure and how they bind agonists, antagonists and ions. The first structure of the ligand-binding domain of the GluK1 subunit was reported in 2005, seven years after publication of the crystal structure of a soluble construct of the ligand-binding domain of the AMPA-type subunit GluA2. Today, a full......-length structure has been determined of GluK2 by cryo electron microscopy to 7.6 Å resolution as well as 84 high-resolution crystal structures of N-terminal domains and ligand-binding domains, including agonist and antagonist bound structures, modulatory ions and mutations. However, there are still many unanswered...

  2. Crystal structure of clathrates of Hofmann dma-type

    International Nuclear Information System (INIS)

    Seven new clathrates Cd(DMA)2Ni(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

  3. The crystal structure and crystal chemistry of fernandinite and corvusite

    Science.gov (United States)

    Evans, H.T., Jr.; Post, J.E.; Ross, D.R.; Nelen, J.A.

    1994-01-01

    Using type material of fernandinite from Minasragra, Peru, and corvusite from the Jack Claim, La Sal Mountains, Utah, the properties and crystal chemistry of these minerals have been determined by Rietveld analysis of the powder X-ray-diffraction patterns. The crystal structure of both species is isotypic with the V2O5 -type layer first found for ??-Ag0.68V2O5; it consists of chains of VO6 octahedra linked by opposite corners (parallel to b) condensed by edge-sharing to form the layer. The vanadium has average valence 4.8, and the resulting layer-charge is balanced by varying amounts of Ca, Na, and K in the interlayer region accompanied by labile water. This study has confirmed the validity of fernandinite as a unique mineral species. It is closely related to corvusite, from which it is distinguished on the basis of the dominant interlayer cation: Ca for fernandinite, Na for curvusite. -Authors

  4. Syntheses and Crystal Structures of Some Aryloxy and Alkoxy Substituted Phthalonitriles

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    Phthalonitriles substituted with aryloxy and alkoxy groups have been synthesized and characterized by elemental analyses, IR, mass spectra and 1H NMR spectroscopy. And four of such crystal structures have also been determined. In the crystal structures, the major intermolecular interactions between the neighboring molecules are the hydrogen bonds as C≡N…H and C-O…H that lead to similar networks in the crystal structures.

  5. Crystal Structure of the Dynein Motor Domain

    OpenAIRE

    Carter, Andrew P.; Cho, Carol; Jin, Lan; Vale, Ronald D.

    2011-01-01

    Dyneins are microtubule-based motor proteins that power ciliary beating, transport intracellular cargos, and help to construct the mitotic spindle. Evolved from ring-shaped hexameric AAA-family adenosine triphosphatases (ATPases), dynein’s large size and complexity have posed challenges for understanding its structure and mechanism. Here, we present a 6 angstrom crystal structure of a functional dimer of two ~300-kilodalton motor domains of yeast cytoplasmic dynein. The structure reveals an u...

  6. Surface structure of potassium sulphate crystals

    International Nuclear Information System (INIS)

    Full text: It is known, that the surface structure of crystals differs from crystal structure far from a surface. It is connected to that on a surface there is a necessity of indemnification of charges of surface ions. In this connection occurs either a relaxation, or reorganization of surface structure. As many electronic processes, including a luminescence and processes of energy transfer, can be subject to influence of the surface phenomena, the knowledge of structure of a surface can be crucial. Objects of research in the present work are the crystal K2SO4, and also the activated crystal K2SO4-Tl. Potassium sulfate has ionic type of connection between metal ions and oxi-anionic group. Inside oxi-anionic groups four atoms of oxygen and one atom of sulfur are connected by covalent connection. The atom of sulfur is located in the center of tetrahedral pyramids on which tops atoms of oxygen settle down. It agrees to the data of X-ray structural analysis an ion SO4- has correct a tetrahedral structure. The formula of such connection can be written down as AIAIIX4, where AI and AII - potassium ions in positions I and II, and X - SO4- -anion. Monocrystals of researched sulfates were raised from water solutions by a method of slow evaporation. Crystals - the columns extended along one direction have been chosen. Measurements on a scanning electronic microscope were carried out on the natural raw side. For this purpose on this side the corresponding covering was rendered. The surface of crystals has been covered with set of 'tracks' in width about 10 microns. Tracks represented long bent raised roads above a surface of constant width and constant height. In directions of tracks there is no system. They are frequently crossed; some tracks come to an end, being gradually narrowed on distance 10-15 microns. All tracks have in the middle a failure of constant width about 1 micron. Such system of tracks is present as on a surface of a pure crystal, and a crystal an impurity

  7. Crystal structure determination of Jatrorrhizine chloride

    Institute of Scientific and Technical Information of China (English)

    LEI XianRong; YANG JianHua; LIN Xiang; DAI Qin; CHENG Qiang; GUO LingHong; LI Hui

    2009-01-01

    Optimum resolution data of powder X-ray diffraction (PXRD) for Jatrorrhizine (Jat) were collected by an X' Pert Pro MPD diffractometer with an X'celerator detector under the stepwise scanning condition as 8.255 ms and 0.00836°per step,2θrange of 50°-80° and total scanning period of 8-10 min. Indexing of the crystal system and a search of the space group from the powder X-ray diffraction data were conducted by the computational crystallography method. The pilot crystal models of Jat were globally optimized with Monte Carlo method and then refined with the Rietveld method. In parallel with PXRD test,single crystals of Jat were cultured in an aqueous solution by a slow-decreasing temperature method,then its crystal structure was determined by single crystal X-ray diffraction (SCXRD). Both crystal structures from PXRD and SCXRD are identical. The results show that the crystal structure of Jat belongs to a monoclinic system and the space group P21/c. The parameters of cell dimensions from PXRD are a=7.69(A),b= 12.55(A),c=20.89(A),β=106.53°,Z=4,and V=1933.4(A)3,meanwhile the parameters from SCXRD are a=7.72(A),b=12.61(A),c=20.99(A),β=106.38°,Z=4,and V=1961.3(A)3.

  8. Band Structure Based Analysis of Certain Photonic Crystal Structures

    OpenAIRE

    Wolff, Christian

    2011-01-01

    Photonic crystals are periodic dielectric structures that may exhibit a complete photonic band gap. First, I discuss geometric properties of the band structure such as band edges. In a second part, I present work on photonic Wannier functions and their use for solving the wave equation. The third part is devoted to applications of the presented methods: A polarization resolved transmission experiment of opel films and an analogy experiment for spontaneous emission inside a photonic crystal.

  9. Crystal structure from one-electron theory

    DEFF Research Database (Denmark)

    Skriver, H. L.

    1985-01-01

    theory, the predicted crystal structures are in accord with experiment in all cases except 79Au. In addition, they have investigated the effect of pressure upon the alkali metals (3Li, 11Na, 37Rb, 55Cs) and selected lanthanide metals (57La, 58Ce, 71Lu) and actinide metals (90Th, 91Pa). In these cases 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 by the...... theory gives accurate predictions of the stability of the closed-packed structures but is found to be less accurate for open structures such as α-U...

  10. Information and crystal structure estimation

    International Nuclear Information System (INIS)

    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.)

  11. Modular crystals as modulated structures

    DEFF Research Database (Denmark)

    Elcoro, L.; Perez-Mato, J.M.; Friese, K.; Petricek, V.; Balic Zunic, Tonci; Olsen, L.A.

    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...

  12. Controls of Crystal Morphology, Size and Structure in Spontaneous Precipitation of Calcium Carbonate

    OpenAIRE

    YANG Ya-Nan, ZHU Xiao-Li, KONG Xiang-Zheng

    2013-01-01

    Nano- to micron-meter CaCO3 particles with different shape and crystal structures were prepared by adjusting the experimental conditions, including use of crystal growth inhibitors, concentrations of CaCl2 and Na2CO3, and dispersing methods. CaCO3 particles were characterized using electronic microscope, dynamic light scattering and X-ray diffraction. The results indicated that the nature and concentration of the crystal growth inhibitors had important effects on the morphology and crystal st...

  13. Crystal Structure of the C-terminal Region of Streptococcus mutans Antigen I/II and Characterization of Salivary Agglutinin Adherence Domains

    Energy Technology Data Exchange (ETDEWEB)

    Larson, Matthew R.; Rajashankar, Kanagalaghatta R.; Crowley, Paula J.; Kelly, Charles; Mitchell, Tim J.; Brady, L. Jeannine; Deivanayagam, Champion (King); (Cornell); (UAB); (Glasgow); (Florida)

    2012-05-29

    The Streptococcus mutans antigen I/II (AgI/II) is a cell surface-localized protein that adheres to salivary components and extracellular matrix molecules. Here we report the 2.5 {angstrom} resolution crystal structure of the complete C-terminal region of AgI/II. The C-terminal region is comprised of three major domains: C{sub 1}, C{sub 2}, and C{sub 3}. Each domain adopts a DE-variant IgG fold, with two {beta}-sheets whose A and F strands are linked through an intramolecular isopeptide bond. The adherence of the C-terminal AgI/II fragments to the putative tooth surface receptor salivary agglutinin (SAG), as monitored by surface plasmon resonance, indicated that the minimal region of binding was contained within the first and second DE-variant-IgG domains (C{sub 1} and C{sub 2}) of the C terminus. The minimal C-terminal region that could inhibit S. mutans adherence to SAG was also confirmed to be within the C{sub 1} and C{sub 2} domains. Competition experiments demonstrated that the C- and N-terminal regions of AgI/II adhere to distinct sites on SAG. A cleft formed at the intersection between these C{sub 1} and C{sub 2} domains bound glucose molecules from the cryo-protectant solution, revealing a putative binding site for its highly glycosylated receptor SAG. Finally, electron microscopy images confirmed the elongated structure of AgI/II and enabled building a composite tertiary model that encompasses its two distinct binding regions.

  14. 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.

  15. 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

    International Nuclear Information System (INIS)

    The title compound, C13H14O2N3Cl, 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. P21/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 R22 (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 λmax = 298 nm was determined by UV-Vis spectrophotometer

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

    Science.gov (United States)

    Sharma, R.; Nayak, P. S.; Narayana, B.; Kant, R.

    2015-12-01

    The title compound, C13H14O2N3Cl, 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. P21/ 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 2 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 λmax = 298 nm was determined by UV-Vis spectrophotometer.

  17. 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.

  18. Crystal Structure of Human Enterovirus 71

    OpenAIRE

    Plevka, Pavel; Perera, Rushika; Cardosa, Jane; Kuhn, Richard J.; Rossmann, Michael G.

    2012-01-01

    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.

  19. 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.

  20. Optical characterization of lyotropic chromonic liquid crystals

    Science.gov (United States)

    Liu, Hui

    Lyotropic chromonic liquid crystals (LCLCs) represent a special class of lyotropic mesophases markedly different from conventional amphiphilic mesogens. Materials forming LCLCs are composed of plank-like molecules with a polyaromatic central core and hydrophilic ionic groups at the periphery. The individual molecules tend to assemble into rodlike aggregates that form the N phase once the concentration exceeds about 0.1M. The LCLC materials show a tremendous potential for applications in optics as self-assembling polarizing and compensating films and in the area of real-time biological sensing. The emerging applications require an understanding of basic properties of LCLC. This work addresses these needs by providing the optical characterization of LCLC. We studied in detail the optical anisotropic properties of three different nematic LCLCs: disodium cromoglycate (DSCG), Blue 27, and Violet 20. We determined the birefringence of these three materials as the function of the temperature T and wavelength lambda and the corresponding dependencies of the absorption coefficients for Blue 27 and Violet 20. The birefringence is negative and significantly lower in the absolute value as compared to the birefringence of typical thermotropic N materials. We determined the scalar order parameter of the nematic phase of Blue 27 and its temperature dependence. The scalar order parameter is close to the one predicted by the classic Onsager theory for solutions of rigid rods. However, this similarity is not complete, as the measured scalar order parameter depends on temperature. The I-N pretransitional fluctuations in an aqueous solution of DSCG were studied by light scattering. We obtained the correlation length of the orientational order-parameter fluctuations of isotropic DSCG solution. The pretransitional behavior of light scattering does not completely follow the classic Landau-de Gennes model. This feature is explained by the variable length of DSCG aggregates as a function

  1. Photonic Crystal Laser-Driven Accelerator Structures

    Energy Technology Data Exchange (ETDEWEB)

    Cowan, Benjamin M.

    2007-08-22

    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.

  2. Synthesis, spectral, single crystal X-ray structural, CShM and BVS characterization of iron(III) cyclohexyl dithiocarbamates and their solvothermal decomposition to nano iron(II) sulphide

    Science.gov (United States)

    Ramalingam, K.; Srinivasan, S.

    2015-11-01

    [Fe(chmdtc)3] (1), [Fe(chedtc)3] (2), [Fe(achdtc)3] (3) and [Fe(chpdtc)3] (4) (where chmdtc = cyclohexylmethylcarbodithioate, chedtc = cyclohexylethylcarbodithioate, achdtc = allylcyclohexylcarbodithioate and chpdtc = cyclohexylpiperazinecarbodithioate) have been prepared and characterisized by elemental analysis, electronic, IR spectral, magnetic susceptibility, thermogravimetric analysis. The single crystal X-ray crystal structures of [Fe(chedtc)3] (2)and [Fe(chpdtc)3] (4) have been determined. Characteristic thioureide IR bands occur at 1483, 1477, 1454 and 1479 cm-1 for (1), (2), (3) and (4) respectively. Electronic spectral bands at 514,512,510 and 510 nm for (1), (2), (3) and (4) respectively are due to dxy → dx2 - y2 transition. One electron quasi reversible reductions due to Fe(III)/Fe(II) redox process are observed in CV. Magnetic susceptibility measurements exhibit a temperature dependent variation. Final residue obtained in thermal processes is FeS, which indicates the reduction of Fe(III) → Fe(II). Single crystal X-ray structures of [Fe(chedtc)3] (2)and [Fe(chpdtc)3] (4) show that the central atom is in a distorted octahedral environment. The CShM values have been calculated from the structural data as 2.5807 and 3.2329 for (2) and (4) respectively in a scale of zero to hundred. The observed values show that compound (4) is relatively more distorted than (2) in its octahedral coordination due to the steric demands of the cyclohexyl ring attached to piperazine. Both of them prefer octahedral coordination environment over trigonal prism. Bond Valence Sum (BVS) calculations confirmed the oxidation state of iron as +3. A non conventional solvothermal formation of FeS nano particles is reported with iron dithiocarbamates as single source precursors. Morphology and composition of the nano product have been characterized by PXRD and EDX analysis.

  3. Preparation and characterization of cadmium(II) halide complexes with N-substituted glycines, and the crystal structures of dichloro(N-methylglycine)cadmium(II) and diaquadichloro(N,N-dimethylglycine)cadmium(II)

    Energy Technology Data Exchange (ETDEWEB)

    Yamada, Junichi; Hashimoto, Haruki; Inomata, Yoshie; Takeuchi, Toshio [Jochi Univ., Tokyo (Japan). Faculty of Science and Technology

    1994-12-01

    Eight cadmium(II) halide complexes with N-methylglycine (sarcosine, Hsar), N,N-dimethylglycine (Hdmgly), and N,N,N-trimethylglycine (betaine, Hbet) have been prepared and characterized by using their infrared absorption spectra and thermal analyses. In addition, the crystal and molecular structures of [CdCl{sub 2}(Hsar)] (1) and [CdCl{sub 2}(Hdmgly)(H{sub 2}O){sub 2}] (2) were determined by a single-crystal X-ray diffraction method. The crystal data for these two complexes are as follows: Complex (1): monoclinic, space group P2{sub 1}/n, a=7.960(2), b=13.844(1), c=6.917(1) A, {beta}=92.42(2)deg, Z=4. Complex (2): monoclinic, space group P2{sub 1}/a, a=7.696(2), b=21.854(4), c=6.253(2) A, {beta}=103.69(2)deg, Z=4. These structures were solved by the heavy-atom method and refined by full-matrix least-square methods to final R values of 0.043 for 2533 reflections about 1 and 0.068 for 3615 reflections about 2, respectively. For 1 the structure consists of a one-dimensional polymer bridged by two chlorine atoms. The cadmium atom is hexa-coordinated, being ligated with two oxygen atoms of a carboxyl group and four chlorine atoms. For 2 the cadmium atom is in a distorted octahedral geometry, ligated by a carboxylato oxygen atom, two water molecules, and three chlorine atoms, in which one is terminal and the other two are bridging cadmium atoms to make a polymer. (author).

  4. Diffractaic acid: Crystalline structure and physicochemical characterization

    Science.gov (United States)

    de Castro Fonseca, Jéssica; de Oliveira, Yara Santiago; Bezerra, Beatriz P.; Ellena, Javier; Honda, Neli Kika; Silva, Camilla V. N. S.; da Silva Santos, Noemia Pereira; Santos-Magalhães, Nereide Stela; Ayala, Alejandro Pedro

    2016-08-01

    Diffractaic acid (DA) is a secondary metabolite of lichens that belongs to the chemical class of depsides, and some relevant pharmacological properties are associated with this natural product, such as antioxidant, antiulcerogenic and gastroprotective effects. Considering the relevant biological activities and taking into account that the activities are intrinsically related to the structure, the main goal of this study was to elucidate the structure of diffractaic acid by single crystal X-ray diffraction as well to characterize its physicochemical properties by powder X-ray diffraction, thermal analysis and vibrational spectroscopy. It was observed that DA belongs to the monoclinic crystal system, crystallizing in the space group P21/c with the following cell parameters: a = 18.535(7) Å, b = 4.0439(18) Å, c = 23.964(6) Å, β = 91.55(3)°. The crystal packing is characterized by difractaic acid dimers, which are reflected in the vibrational spectrum. These observations were supported by quantum mechanical calculations.

  5. PREPARATION AND CHARACTERIZATION OF FREEZE DRIED CRYSTALS OF IBUPROFEN

    OpenAIRE

    Dixit Mudit; Kulkarni Parthasarathi Keshavarao; Panner Selvam; Syed Mohsin Ali

    2011-01-01

    Ibuprofen, an anti-inflammatory drug, exhibits poor water solubility and flow properties.. Crystallization medium used for freeze dried crystals of Ibuprofen consisted of Isopropyl alcohol and water (50:50%) respectively. Freeze dried crystals were characterized by differential scanning calorimetry, Infrared spectroscopy, X-ray diffractometry and scanning electron microscopy. Micromeritic and mechanical property and dissolution behavior studies were carried out. Process variables such as amou...

  6. Growth and characterization of propyl-para-hydroxybenzoate single crystals

    Indian Academy of Sciences (India)

    N Karunagaran; P Ramasamy; R Perumal Ramasamy

    2014-10-01

    Single crystals of propyl--hydroxybenzoate have been grown by slow evaporation solution technique. The structure of the compound was confirmed by FT–IR, FT–Raman spectroscopy and single crystal X-ray diffraction studies. The crystalline perfection of the grown single crystals has been analysed by high resolution X-ray diffraction measurements. Optical properties of the grown single crystals were studied by UV–Vis NIR spectrum. The luminescence behaviour of the single crystal has been analysed by photoluminescence analysis and found maximum luminescence in the lower wavelength region. A simple interferometric technique was used for measuring birefringence of the crystal. The laser damage threshold of the crystal is 1.3 GW/cm2. The mechanical strength of the grown crystal is measured using Vickers microhardness tester. The dielectric properties have been investigated.

  7. 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.

  8. Absorption enhancement in graphene photonic crystal structures.

    Science.gov (United States)

    Khaleque, Abdul; Hattori, Haroldo T

    2016-04-10

    Graphene, a single layer of carbon atoms arranged in a honeycomb lattice, is attracting significant interest because of its potential applications in electronic and optoelectronic devices. Although graphene exhibits almost uniform absorption within a large wavelength range, its interaction with light is weak. In this paper, the enhancement of the optical absorption in graphene photonic crystal structures is studied: the structure is modified by introducing scatterers and mirrors. It is shown that the absorption of the graphene photonic crystal structure can be enhanced about four times (nearly 40%) with respect to initial reference absorption of 9.8%. The study can be a useful tool for investigating graphene physics in different optical settings. PMID:27139857

  9. Crystal structure of low-symmetry rondorfite

    International Nuclear Information System (INIS)

    The crystal structure of an aluminum-rich variety of the mineral rondorfite with the composition Ca16[Mg2(Si7Al)(O31OH)]Cl4 from the skarns of the Verkhne-Chegemskoe plateau (the Kabardino-Balkarian Republic, the Northern Caucasus Region, Russia) was solved in the triclinic space group with the unit-cell parameters a = 15.100(2) Å, b = 15.110(2) Å, c = 15.092(2) Å, α = 90.06(1)°, β = 90.01(1)°, γ = 89.93(1)°, Z = 4, sp. gr. P1. The structural model consisting of 248 independent atoms was determined by the phase-correction method and refined to R = 3.8% with anisotropic displacement parameters based on all 7156 independent reflections with 7156 F > 3σ(F). The crystal structure is based on pentamers consisting of four Si tetrahedra linked by the central Mg tetrahedron. The structure can formally be refined in the cubic space group (a = 15.105 Å, sp. gr. Fd 3 bar , seven independent positions) with anisotropic displacement parameters to R = 2.74% based on 579 reflections with F > 3σ(F) without accounting for more than 1000 observed reflections, which are inconsistent with the cubic symmetry of the crystal structure.

  10. Synthesis and Crystal Structure of Tetranuclear Zinc Benzoate

    Institute of Scientific and Technical Information of China (English)

    YIN Ming-cai; WANG Chi-wei; AI Chang-chun; YUAN Liang-jie; SUN Ju-tang

    2004-01-01

    A tetranuclear zinc benzoate Zn4O(C6H5CO2)6 was synthesized and characterized by X-ray single crystal determination. It crystallizes in cubic, space group Ia-3d. Its crystal cell is very large, a=4.100 63(18) nm, V=68.953(5) nm3 and Z = 48. The structure is composed of discrete Zn4O(C6H5CO2)6 molecules. In each molecule, four zinc atoms are held together by a central oxygen atom, which results in the formation of a regular tetrahedron. All benzoate ligands coordinate to zinc atoms in a bidentate bridging mode. Each zinc atom is in a slightly distorted tetrahedral geometry, coordinated by three benzoate oxygen atoms and the central oxygen atom. The intermolecular interactions result in the formation of a three-dimensional supramolecular framework, with non-intersecting parallel channels.

  11. The purification, crystallization and preliminary structural characterization of FAD-dependent monooxygenase PhzS, a phenazine-modifying enzyme from Pseudomonas aeruginosa

    International Nuclear Information System (INIS)

    PhzS, an FAD-dependent monooxygenase that catalyzes a reaction involved in the biosynthesis of the virulence factor pyocyanin in P. aeruginosa, was cloned, overexpressed and crystallized. Data collection from native and seleno-l-methionine-labelled crystals is reported. The blue chloroform-soluble bacterial metabolite pyocyanin (1-hydroxy-5-methyl-phenazine) contributes to the survival and virulence of Pseudomonas aeruginosa, an important Gram-negative opportunistic pathogen of humans and animals. Little is known about the two enzymes, designated PhzM and PhzS, that function in the synthesis of pyocyanin from phenazine-1-carboxylic acid. In this study, the FAD-dependent monooxygenase PhzS was purified and crystallized from lithium sulfate/ammonium sulfate/sodium citrate pH 5.5. Native crystals belong to space group C2, with unit-cell parameters a = 144.2, b = 96.2, c = 71.7 Å, α = γ = 90, β = 110.5°. They contain two monomers of PhzS in the asymmetric unit and diffract to a resolution of 2.4 Å. Seleno-l-methionine-labelled PhzS also crystallizes in space group C2, but the unit-cell parameters change to a = 70.6, b = 76.2, c = 80.2 Å, α = γ = 90, β = 110.5° and the diffraction limit is 2.7 Å

  12. Structure sensitive properties of KTP-type crystals

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    Adding various dopants during the growth of the parent KTiOPO4 (KTP) crystal has given rise to an extensive series of KTP-type crystals. The doped KTP or KTP-type crystals often have very subtle structural variations from pure KTP crystals. As a result of these structural changes the KTP-type crystals often exhibit different physical properties, which may be referred to as structure sensitive properties. It is possible to fine-tune the nonlinear optical properties of KTP crystals through doping. This results in a broad range of applications for KTP-type crystals.

  13. Growth and characterization of diammonium copper disulphate hexahydrate single crystal

    Energy Technology Data Exchange (ETDEWEB)

    Siva Sankari, R. [Department of Physics, Agni College of Technology, Thalambur, Chennai 603103 (India); Perumal, Rajesh Narayana, E-mail: r.shankarisai@gmail.com [Department of Physics, SSN College of Engineering, Kalavakkam, Chennai 603110 (India)

    2014-03-01

    Graphical abstract: Diammonium copper disulphate hexahydrate (DACS) is one of the most promising inorganic dielectric crystals with exceptional mechanical properties. Good quality crystals of DACS were grown by using solution method in a period of 30 days. The grown crystals were subjected to single crystal X-ray diffraction analysis in order to establish their crystalline nature. Thermo gravimetric, differential thermal analysis, FTIR, and UV–vis–NIR analysis were performed for the crystal. Several solid state physical parameters have been determined for the grown crystals. The dielectric constant and the dielectric loss and AC conductivity of the grown crystal were studied as a function of frequency and temperature has been calculated and plotted. - Highlights: • Diammonium copper disulphate is grown for the first time and CCDC number obtained. • Thermal analysis is done to see the stability range of the crystals. • Band gap and UV cut off wavelength of the crystal are determined to be 2.4 eV and 472.86 nm, respectively. • Dielectric constant, dielectric loss and AC conductivity are plotted as a function of applied field. - Abstract: Diammonium copper disulphate hexahydrate is one of the most promising inorganic crystals with exceptional dielectric properties. A good quality crystal was harvested in a 30-day period using solution growth method. The grown crystal was subjected to various characterization techniques like single crystal X-ray diffraction analysis, thermo gravimetric, differential thermal analysis, FTIR, and UV–vis–NIR analysis. Unit cell dimensions of the grown crystal have been identified from XRD studies. Functional groups of the title compounds have been identified from FTIR studies. Thermal stability of the samples was checked by TG/DTA studies. Band gap of the crystal was calculated. The dielectric constant and dielectric loss were studied as a function of frequency of the applied field. AC conductivity was plotted as a function

  14. Chelation, spectroscopic characterization, biological activity and crystal structure of 2,3-butanedione isonicotinylhydrazone: Determination of Zr4+ after flotation separation

    Science.gov (United States)

    Al-Fulaij, O. A.; Jeragh, B.; El-Sayed, A. E. M.; El-Defrawy, M. M.; El-Asmy, A. A.

    2015-02-01

    New metal complexes of Co(II), Ni(II) Cu(II), Zn(II), Cd(II), Pd(II) and Hg(II) with 2,3-butanedione isonicotinylhydrazone [BINH] have been prepared and investigated. Single crystal for BINH is grown and solved as orthorhombic with P 21 21 2 space group. The formula of the ligand was assigned based on the elemental analysis, mass spectra and conductivity measurements. The complexes assigned the formulae [M(BINH-H)Cl]ṡnH2O (Mdbnd Co(II), Ni(II), Cu(II), Zn(II); n = 0 or 1); [Hg(BINH-H)(H2O)2Cl]; [Cd(BINH)Cl2]ṡ2H2O and [Pd(BINH)Cl2]ṡH2O. All complexes are nonelectrolytes. BINH acts as a tridentate ligand in [M(BINH-H)Cl]ṡnH2O and [Hg(BINH-H)(H2O)2Cl] coordinating through Cdbnd Oketonic, Csbnd Oamedic and Cdbnd Nhy and as a neutral bidentate through Cdbnd Oketonic and Cdbnd Nhy in [Cd(BINH)Cl2]ṡ2H2O and [Pd(BINH)Cl2]ṡH2O; the pyridine nitrogen has no rule in coordination. The data are supported by NMR (1H and 13C) spectra. The magnetic moments and electronic spectra provide a tetrahedral structure for the Co(II), Ni(II), Cu(II), Zn(II) and Cd(II) complexes; square-planar for the Pd(II) complex and octahedral for the Hg(II) complex. The TGA of the complexes depicted the outer and inner water molecules as well as the final residue. The cobalt and cadmium complexes ended with the metal while the Cu(II), Zn(II) and Pd(II) complexes ended with complex species. [Hg(BINH-H)(H2O)2Cl] has no residue. The ligand is inactive against all tested organisms except for Bacillus thuringiensis. The Hg(II) complex is found more active than the other complexes. The flotation technique is found applicable for the separation of micro amount (10 ppm) of Zr4+ using 10 ppm of BINH and 1 × 10-5 mol L-1 of oleic acid at pH 6 with efficiency of 98% with no interferences.

  15. 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.

  16. Crystal Structure of New Heusler Compounds

    OpenAIRE

    Graf, Tanja; Casper, Frederick; Winterlik, Jürgen; Balke, Benjamin; FECHER, GERHARD H.; Felser, Claudia

    2009-01-01

    Heusler compounds are promising materials in many fields of contemporary research. The spectrum of their possible applications ranges from magnetic and magneto-mechanical materials over semiconductors and thermoelectrics to superconductors. An important feature of the Heusler compounds is the possibility of controlling the valence electron concentration by partial substitution of elements. On the other hand, the properties also depend on the degree of ordering of the the crystal structure. In...

  17. Synthesis, characterization, crystal structure, catalytic activity in oxidative bromination, and thermal study of a new oxidovanadium Schiff base complex containing O, N-bidentate Schiff base ligand

    Czech Academy of Sciences Publication Activity Database

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

    2014-01-01

    Roč. 67, č. 22 (2014), s. 3664-3677. ISSN 0095-8972 Institutional support: RVO:68378271 Keywords : oxidovanadium(IV) * Schiff base * single crystal * oxidative bromination Subject RIV: CA - Inorganic Chemistry Impact factor: 2.012, year: 2014

  18. Characterization of interfaces in mosaic CVD diamond crystal

    Science.gov (United States)

    Muchnikov, Anatoly B.; Radishev, Dmitry B.; Vikharev, Anatoly L.; Gorbachev, Alexei M.; Mitenkin, Anatoly V.; Drozdov, Mikhail N.; Drozdov, Yuri N.; Yunin, Pavel A.

    2016-05-01

    Detailed description of a way to accrete diamond single crystals in one plate using the CVD method is presented. It was found that each region of the mosaic CVD diamond crystal grown over a certain seed substrate "inherits" the crystallographic orientation of its substrate. No correlation was found between the value of misorientation of the accreted crystals and entrance of hydrogen to the boundary. It is shown that successful accretion of single crystal diamond plates in a single mosaic crystal occurs even in the case of great misorientation of crystals. The mechanical stresses appear during the fabrication of the mosaic CVD diamond crystal. Stresses accumulate during accretion of the regions, which grow over substrates with different orientations, in a common structure.

  19. PREPARATION AND CHARACTERIZATION OF FREEZE DRIED CRYSTALS OF IBUPROFEN

    Directory of Open Access Journals (Sweden)

    Dixit Mudit

    2011-12-01

    Full Text Available Ibuprofen, an anti-inflammatory drug, exhibits poor water solubility and flow properties.. Crystallization medium used for freeze dried crystals of Ibuprofen consisted of Isopropyl alcohol and water (50:50% respectively. Freeze dried crystals were characterized by differential scanning calorimetry, Infrared spectroscopy, X-ray diffractometry and scanning electron microscopy. Micromeritic and mechanical property and dissolution behavior studies were carried out. Process variables such as amount of bridging liquid, stirring time and duration of stirring were optimized. Dissolution profile of the freeze dried crystals was compared with pure sample and recrystallized sample. Freeze dried crystals exhibited decreased crystallinity and improved micromeritic properties. The dissolution of the freeze dried crystals was improved compared with pure sample.

  20. Synthesis and characterization of superconducting single-crystal Sn nanowires

    Science.gov (United States)

    Tian, Mingliang; Wang, Jinguo; Snyder, Joseph; Kurtz, James; Liu, Ying; Schiffer, Peter; Mallouk, Thomas E.; Chan, M. H. W.

    2003-08-01

    Single-crystal superconducting tin nanowires with diameters of 40-160 nm have been prepared by electrochemical deposition in porous polycarbonate membranes. Structural characterization through transmission electron microscopy and x-ray diffraction showed that the nanowires are highly oriented along the [100] direction. Although the superconducting transition temperature is close to the bulk value of 3.7 K, the effect of reduced dimensionality is clearly evident in the electrical transport properties of the thinnest wires (40 nm diameter). Magnetization measurements show that the critical field of the nanowires increases significantly with decreasing diameter to ˜0.3 T for the thinnest wires, nearly an order of magnitude larger than the bulk value.

  1. Synthesis, crystal structures and spectral characterization of imidazo[1,2-a]pyrimidin-2-yl-acetic acid and related analog with imidazo[2,1-b]thiazole ring

    Science.gov (United States)

    Dylong, Agnieszka; Goldeman, Waldemar; Sowa, Michał; Ślepokura, Katarzyna; Drożdżewski, Piotr; Matczak-Jon, Ewa

    2016-08-01

    Imidazo[1,2-a]pyrimidin-2-yl-acetic acid (HIPM-2-ac) and its analog with imidazo[2,1-b]thiazole ring (HITZ-6-ac) were synthesized and structurally characterized by single-crystal X-ray diffraction corroborated with calculations of Hirshfeld surfaces, which provided detailed insight into intermolecular interactions constituting both crystals. The IR and Raman spectra of HIPM-2-ac and HITZ-6-ac were recorded and interpreted in details with the aid of Density Functional Theory (DFT) calculations and Potential Energy Distribution (PED) analysis of computed normal vibrations. Special attention was paid on hydroxyl and methylene groups involved in hydrogen bonds, which vibrations were monitored by H/D substitution. Recrystallization of parent compounds from deuterium oxide (D2O) solutions resulted in deuteration of their carboxylic OH groups and almost complete deuteration of HIPM-2-ac methylene group. The latter phenomenon is clearly reflected in the vibrational spectra and confirmed by 1H NMR experiments in solution.

  2. 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. PMID:25546494

  3. 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.

  4. Characterization of bent crystals for Laue lenses

    CERN Document Server

    Liccardo, V; Frontera, F; Valsan, V

    2012-01-01

    In the context of the LAUE project devoted to build a long focal-length focusing optics for soft $\\gamma$-ray astronomy (80 - 600 keV), we present the results of reflectivity measurements of bent crystals in different configurations, obtained by bending perfect or mosaic flat crystals. We also compare these results with those obtained using flat crystals. The measurements were performed using the K$\\alpha$ line of the Tungsten anode of the X-ray tube used in the LARIX facility of the University of Ferrara. These results are finalized to select the best materials and to optimize the thickness of the crystal tiles that will be used for building a Laue lens petal which is a part of an entire Laue lens, with 20 m focal length and 100-300 keV passband. The final goal of the LAUE project is overcome, by at least 2 orders of magnitude, the sensitivity limits of the current generation of $\\gamma$-ray telescopes, and to improve the current $\\gamma$-ray imaging capability.

  5. Crystal Structure Prediction from First Principles: The Crystal Structures of Glycine

    OpenAIRE

    Lund, Albert M.; Pagola, Gabriel I.; Orendt, Anita M.; Ferraro, Marta B.; Facelli, Julio C.

    2015-01-01

    Here we present the results of our unbiased searches of glycine polymorphs obtained using the Genetic Algorithms search implemented in Modified Genetic Algorithm for Crystals coupled with the local optimization and energy evaluation provided by Quantum Espresso. We demonstrate that it is possible to predict the crystal structures of a biomedical molecule using solely first principles calculations. We were able to find all the ambient pressure stable glycine polymorphs, which are found in the ...

  6. Growth of PrFeAsO1-y single crystals and its characterization

    International Nuclear Information System (INIS)

    Single crystals of oxygen deficient oxypnictide superconductor PrFeAsO1-y have been grown by using belt-type anvil high-pressure synthesis apparatus. Superconducting transition temperature (Tc) of the obtained single crystal is 45 K, and typical size is about 800 x 1000 x 30 μm3. In-plane electrical resistivity shows s-shaped behavior, and can well be fitted by T1.2 temperature dependence near 150 K. In addition, we obtained non-superconducting parent single crystal by annealing the as-grown single crystal under ambient pressure. Resistivity of parent single crystal is characterized by the kink near 150 K corresponding to the structural transition, and the structure near 12 K, which is thought to be originating from the magnetic order of Pr ion.

  7. Characterization of Injection Molded Structures

    DEFF Research Database (Denmark)

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

    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...... understand structure-properties relationship of the injection molded polymer samples. These results are very important in optimizing injection molding parameters....

  8. Characterization of some wide viewing angle liquid crystal devices

    Science.gov (United States)

    Liu, Weimin

    2001-08-01

    It is well known that a standard twisted nematic (TN) display, which is most commonly used in flat panel displays, has inherently narrow and non-uniform viewing angle characteristics. Normally black TN (NBTN) displays suffer from problems with chromaticity and contrast for normal and poor grayscale at wide viewing angles. Ideal compensation of the dark state for a NBTN requires a negative birefringence film with a uniformly twisted optical axis distribution. However, such films have not been fabricated to date. In our work we approximate the twisted structure of compensation film for NBTN displays by stacking several layers of polymer film having in- plane negative retardation. Using only 4 layers of film we obtain much wider viewing cone and higher contrast compare to uncompensated NBTN. The chromaticity is also greatly improved over the uncompensated cell. Modeling of liquid crystal displays is an efficient and economical way to LCD characterization and optimization without assembling a large number of test cells. It has become a useful tool for the development of new display modes. In the past, optical simulation of LCDs has mainly relied on one-dimensional models. As the liquid crystal technology advances, multidimensional modeling is required for better understanding of optical behavior at smaller feature sizes. In our work, a generalized geometrical optics approach (GOA) has been applied to liquid crystal devices with multiple dimensions. It is faster than other approaches (e.g. FDTD) and proved to be a useful design tool for optimization of liquid crystal devices in more than one-dimension. We performed detailed characterization of the electrically-induced optical compensation (EOC) mode for information display applications. This mode shows very wide viewing angle and excellent grayscale performance when a negative birefringent compensation film is added. Using GOA, we investigated the detailed transmission profile and the viewing angle properties of EOC

  9. Crystal Structure and Magnetic Studies of a New Nitronyl Nitroxide Compound

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    Compound 1 was first synthesized and characterized. Its crystal structure and magnetic property were determined and investigated. Discussion about the molecule packing in crystal and the macroscopic magnetism was also presented, in combination with computing study of the spatial distribution over the molecule.

  10. Characterization of polymer-liquid crystal blends

    OpenAIRE

    DOINA MACOCINSCHI; CRISTOFOR I. SIMIONESCU; DANIELA FILIP

    2001-01-01

    Blends of semi-crystalline polymers (polyethylene adipate and two poly(ester-urethane) s) with liquid crystal cholesteryl palmitate with different compositions were prepared by solution casting. One of the poly(ester-urethane)s was based on 2,4-tolylene diisocyanate (TDI) and the other one on 4,4-diphenylmethane diisocyanate (MDI). The miscibility and phase transition were investigated over the whole range of concentration by differential scanning calorimetry and polarizing optical microscopy.

  11. Growth and characterization of cadmium magnesium tetra thiocyanate crystals

    Energy Technology Data Exchange (ETDEWEB)

    Gunasekaran, S. [Post Graduate and Research Department of Physics, Pachaiyappa' s College, Chennai - 600 030 (India); Ponnusamy, S. [Department of Physics, S. R. M. Institute of Science and Technology, Kattankulathur - 603 203 (India)

    2006-02-01

    Cadmium Magnesium Tetra Thiocyanate, CdMg(SCN){sub 4}, [CMTC] belongs to bimetallic thiocyanate complexes. CMTC crystals has been grown by solution growth technique at room temperature. The morphologies of the grown crystals are identified by single crystal analysis. Also the Powder X-ray Diffractogram of the crystal has been recorded and the various planes of reflection are identified. The title compound crystallizes under triclinic structure with lattice parameters a=10.0976 Aa, b=7.5015 Aa, c=5.7720 Aa and {beta}=90.2135 . The presence of magnesium and cadmium in the grown crystals were confirmed through Atomic Absorption Spectroscopy. The grown crystals are analysed qualitatively by Fourier Transform Infrared (FTIR) and Fourier Transform Raman spectral measurements. The transmittance spectrum of the crystal in the UV-Visible region has been recorded and analysed. The dielectric measurements for the crystals were carried out in the microwave region. The thermal stabilities of the crystals were studied by using different thermal analyses like Thermo Gravimetric Analysis (TGA), Differential Thermal Analysis (DTA) and Differential Scanning Calorimetry (DSC). (copyright 2006 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  12. Revealed Cores: Characterizations and Structure

    OpenAIRE

    Stefano Vannucci

    2010-01-01

    Characterizations of the choice functions that select the cores or the externally stable cores induced by an underlying revealed dominance digraph are provided. Relying on such characterizations, the basic order-theoretic structure of the corresponding sets of revealed cores is also analyzed

  13. Crystal Structure Prediction could have helped the Experimentalists with Polymorphism in Benzamide!

    OpenAIRE

    2008-01-01

    Abstract Benzamide was the first molecular material for which polymorphism was reported as long as 176 years ago. Unfortunately, due to very similar cell metrics leading to massive peak overlap, the metastable form reported by Liebig escaped structural characterization by XRD until recently. With the help of crystal structure prediction this old riddle of ?Liebig's? polymorph of benzamide could have been solved many years earlier. Performing state of the art crystal structure predi...

  14. Non-isothermal melt crystallization of poly(tetramethylene succinate) under high pressure: Characterization and kinetics

    Energy Technology Data Exchange (ETDEWEB)

    Rohindra, David [Graduate School of Engineering, Department of Organic and Polymeric Materials, Tokyo Institute of Technology, 2-12-1-S8-33, O-okayama, Meguro-ku, Tokyo 152-8552 (Japan); School of Biological and Chemical Sciences, Faculty of Science, Technology and Environment, The University of the South Pacific, Suva (Fiji); Kuboyama, Keiichi [Graduate School of Engineering, Department of Organic and Polymeric Materials, Tokyo Institute of Technology, 2-12-1-S8-33, O-okayama, Meguro-ku, Tokyo 152-8552 (Japan); Ougizawa, Toshiaki, E-mail: tougizawa@op.titech.ac.jp [Graduate School of Engineering, Department of Organic and Polymeric Materials, Tokyo Institute of Technology, 2-12-1-S8-33, O-okayama, Meguro-ku, Tokyo 152-8552 (Japan)

    2012-10-10

    Highlights: Black-Right-Pointing-Pointer Non-isothermal crystallization of PTMS under high pressure is reported. Black-Right-Pointing-Pointer Nucleation pattern analyzed using Ozawa model. Black-Right-Pointing-Pointer Crystallization and nucleation behavior changed above 300 MPa. - Abstract: The non-isothermal melt crystallization behavior (characterization and kinetics) of poly(tetramethylene succinate) (PTMS) under high pressure was investigated using high pressure differential thermal analysis (HP-DTA). Wide angle X-ray diffraction (WAXD), small angle X-ray scattering (SAXS), differential scanning calorimetry (DSC), polarized optical microscopy (POM), and density measurement were used to study the crystal structure, the melting temperature and the morphology of the samples crystallized under various pressures. No new crystal structure or formation of extended chain crystals were found in the pressure crystallized samples. Optical micrographs revealed nucleation density decreased and spherulite morphology changed (presence of banding pattern) above 300 MPa. DTA crystallization curves showed a single exothermic peak at all pressures which shifted to higher temperatures with increasing pressure and became broad above 300 MPa. The kinetics was studied using the Ozawa model. A change in the nucleation pattern was predicted from the Ozawa exponent, instantaneous at low pressures and sporadic above 300 MPa. From kinetic and morphological results it was found that a critical pressure region existed around 300 MPa.

  15. Purification, crystallization and preliminary structural characterization of the periplasmic domain P1 of the Escherichia coli membrane-protein insertase YidC

    International Nuclear Information System (INIS)

    The overproduction, purification, crystallization and preliminary crystallographic studies of the native and selenomethionine-labelled P1 domain are reported here as a first step towards the elucidation of the molecular mechanism of YidC as a membrane-protein insertase. In Escherichia coli, the biogenesis of inner membrane proteins (IMPs) requires targeting and insertion factors such as the signal recognition particle (SRP) and the Sec translocon. Recent studies have identified YidC as a novel and essential component involved in membrane insertion of IMPs both in conjunction with the Sec translocon and as a separate entity. E. coli YidC is a member of the YidC (in bacteria)/Oxa1 (in mitochondria)/Alb3 (in chloroplasts) protein family and contains six transmembrane segments and a very large periplasmic domain P1. The overproduction, purification, crystallization and preliminary crystallographic studies of the native and selenomethionine-labelled P1 domain are reported here as a first step towards the elucidation of the molecular mechanism of YidC as a membrane-protein insertase

  16. 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.

  17. Nonlinear optics determination of the symmetry group of a crystal using structured light

    CERN Document Server

    Jauregui, Rocio

    2015-01-01

    We put forward a technique to unveil to which symmetry group a nonlinear crystal belongs, making use of nonlinear optics with structured light. We consider as example the process of spontaneous parametric down-conversion. The crystal, which is illuminated with a special type of Bessel beam, is characterized by a nonlinear susceptibility tensor whose structure is dictated by the symmetry group of the crystal. The observation of the spatial angular dependence of the lower-frequency generated light provides direct information about the symmetry group of the crystal.

  18. Synthesis, growth and characterization of cadmium manganese thiocyanate (CMTC) crystal

    Science.gov (United States)

    Paramasivam, P.; Raja, C. Ramachandra

    2011-09-01

    Single crystals of cadmium manganese thiocyanate, CdMn(SCN)4 (CMTC) have been successfully synthesized and grown by slow evaporation solution growth technique using water as solvent at room temperature. The crystal was characterized by different techniques for finding its suitability for device fabrications. From the single crystal XRD the crystal system was identified as tetragonal. The functional groups were identified from FTIR analysis. The optical studies have been carried out and found that the tendency of transmission observed from the specimen with respect to the wavelength of light is practically more suitable for the present trends in communication engineering. From the thermal analysis the decomposing temperature of the grown crystal is more significant when compared with the studies performed earlier.

  19. Isolation and Crystal Structure of Horminone

    Institute of Scientific and Technical Information of China (English)

    陈晓; 廖仁安; 翁林红; 谢庆兰; 邓锋杰

    2000-01-01

    The horminone (C20H28O4, Mr= 332.85) was first isolated from the leaves of Rabdosia Serra (Maxim) Hara and its crystal structure was determined by X-ray diffraction method. Horminone is orthorhombic with space group P21P21P21, a=7.7186(7), b=9.5506(9), c=24.227(2) A, V=1785.9(3) A3, Z=4, Dc=1.236g/cm3, λ=0. 71073 A , μ(MoKα)=0. 085mm-1, F(000)=720. The structure was refined to R=0. 0369, wR=0.0978 for 2446 reflections with I>2σ(Ⅰ). X-ray diffraction analysis reveals that there are three six-membered rings in the title molecule. Ring A is in the chair conformation, ring C has the structure of quinone and there are two intermolecular hydrogen bonds between two molecules.

  20. Crystal structure of plant photosystem I

    Science.gov (United States)

    Ben-Shem, Adam; Frolow, Felix; Nelson, Nathan

    2003-12-01

    Oxygenic photosynthesis is the principal producer of both oxygen and organic matter on Earth. The conversion of sunlight into chemical energy is driven by two multisubunit membrane protein complexes named photosystem I and II. We determined the crystal structure of the complete photosystem I (PSI) from a higher plant (Pisum sativum var. alaska) to 4.4Å resolution. Its intricate structure shows 12 core subunits, 4 different light-harvesting membrane proteins (LHCI) assembled in a half-moon shape on one side of the core, 45 transmembrane helices, 167 chlorophylls, 3 Fe-S clusters and 2 phylloquinones. About 20 chlorophylls are positioned in strategic locations in the cleft between LHCI and the core. This structure provides a framework for exploration not only of energy and electron transfer but also of the evolutionary forces that shaped the photosynthetic apparatus of terrestrial plants after the divergence of chloroplasts from marine cyanobacteria one billion years ago.

  1. Crystal structure prediction from first principles: The crystal structures of glycine

    Science.gov (United States)

    Lund, Albert M.; Pagola, Gabriel I.; Orendt, Anita M.; Ferraro, Marta B.; Facelli, Julio C.

    2015-04-01

    Here we present the results of our unbiased searches of glycine polymorphs obtained using the genetic algorithms search implemented in MGAC, modified genetic algorithm for crystals, coupled with the local optimization and energy evaluation provided by Quantum Espresso. We demonstrate that it is possible to predict the crystal structures of a biomedical molecule using solely first principles calculations. We were able to find all the ambient pressure stable glycine polymorphs, which are found in the same energetic ordering as observed experimentally and the agreement between the experimental and predicted structures is of such accuracy that the two are visually almost indistinguishable.

  2. Crystal structure of thiamin tetrahydrofurfuryl disulfide

    International Nuclear Information System (INIS)

    The crystal structure of thiamin tetrahydrofurfuryl disulfide, one of the ring-opened derivatives of thiamin, has been determined by the X-ray diffraction methods. The crystal is monoclinic with cell dimensions of a=8.704(1), b=11.207 (2), c=21.260(3) A and β=92.44(2)o, space group P21/c and Z=4. The structure was solved by direct methods and refined to R= 0.076 for 1252 observed reflections measured on a diffractometer. The molecule assumes a folded conformation in which the pyrimidine and the tetrahydrofurfuryl rings are on the same side of the ethylenic plane. The pyrimidinyl, N-formyl and etylenic planes are mutually perpendicular to each other and the N(3)-C(4) bond retains a single bond character. The structure is stabilized by an intramolecular N(4'α)-H --- O(2α) hydrogen bond. The molecules are connected via N(4'α)-H --- (N3') and O(5γ)-H --- (N1') hydrogen bonds, forming a two-dimensional hydrogen-bonding network. The tetrahydrofurfuryl ring is dynamically disordered. The overall conformation as well as the packing model is very similar to that of thiamin propyl disulfide. (Author)

  3. Crystal structure of (ferrocenylmethyldimethylammonium hydrogen oxalate

    Directory of Open Access Journals (Sweden)

    Mamadou Ndiaye

    2015-08-01

    Full Text Available The crystal structure of the title salt, [Fe(C5H5(C8H13N](HC2O4, consists of discrete (ferrocenylmethyldimethylammonium cations and hydrogen oxalate anions. The anions are connected through a strong O—H...O hydrogen bond, forming linear chains running parallel to [100]. The cations are linked to the anions through bifurcated N—H...(O,O′ hydrogen bonds. Weak C—H...π interactions between neighbouring ferrocenyl moieties are also observed.

  4. Monocrystalline structure formation of doped perfect silicon crystals

    International Nuclear Information System (INIS)

    In this paper we consider perfect doped silicon single crystals growth. Special features of anodic etching of n- and p-type single crystals has been revealed. An impact of seed orientation on dislocation and defect structure evolution in crystal on different growth stages has been found. Influence of heat treatment on phase-structural condition of single crystals and nonequilibrium carrier lifetime has been determined

  5. Topological and metrical property characterization of radical subunits for ternary hard sphere crystals

    Science.gov (United States)

    Wang, Lin; An, Xizhong; Wang, Defeng; Qian, Quan

    2016-01-01

    Quantitative characterization on the topological and metrical properties of radical subunits (polyhedra) for two new ternary hard sphere crystals was studied. These two ideal crystalline structures are numerically constructed by filling small and medium spheres into interstices (corresponding to regular tetrahedral and octahedral pores) of perfect face centered cubic (FCC) and hexagonal close packed (HCP) crystals formed by the packing of large spheres. Topological properties such as face number, edge number, vertex number of each radical polyhedron (RP), edge number of each RP face and metrical properties such as volume, surface area, total perimeter and pore volume of each RP, area and perimeter of each RP face were analyzed and compared. The results show that even though the overall packing densities for FCC and HCP ternary crystals are the same, different characteristics of radical polyhedra for corresponding spheres in these two crystals can be identified. That is, in the former structure RPs are more symmetric than those in the latter; the orientations of corresponding RP in the latter are twice as many as that in the former. Moreover, RP topological and metrical properties in the HCP ternary crystal are much more complicated than those in the FCC ternary crystal. These differences imply the structure and property differences of these two ternary crystals. Analyses of RPs provide intensive understanding of pores in the structure.

  6. Topological and metrical property characterization of radical subunits for ternary hard sphere crystals

    Directory of Open Access Journals (Sweden)

    Lin Wang

    2016-01-01

    Full Text Available Quantitative characterization on the topological and metrical properties of radical subunits (polyhedra for two new ternary hard sphere crystals was studied. These two ideal crystalline structures are numerically constructed by filling small and medium spheres into interstices (corresponding to regular tetrahedral and octahedral pores of perfect face centered cubic (FCC and hexagonal close packed (HCP crystals formed by the packing of large spheres. Topological properties such as face number, edge number, vertex number of each radical polyhedron (RP, edge number of each RP face and metrical properties such as volume, surface area, total perimeter and pore volume of each RP, area and perimeter of each RP face were analyzed and compared. The results show that even though the overall packing densities for FCC and HCP ternary crystals are the same, different characteristics of radical polyhedra for corresponding spheres in these two crystals can be identified. That is, in the former structure RPs are more symmetric than those in the latter; the orientations of corresponding RP in the latter are twice as many as that in the former. Moreover, RP topological and metrical properties in the HCP ternary crystal are much more complicated than those in the FCC ternary crystal. These differences imply the structure and property differences of these two ternary crystals. Analyses of RPs provide intensive understanding of pores in the structure.

  7. Active Photonic Crystal Switches: Modeling, Design and Experimental Characterization

    DEFF Research Database (Denmark)

    Heuck, Mikkel; Yu, Yi; Kristensen, Philip Trøst; Kuznetsova, Nadezda; Yvind, Kresten; Mørk, Jesper

    2013-01-01

    In this paper, we present recent progress in modeling, design, fabrication and experimental characterization of InP photonic crystal all-optical switches. Novel designs with increased flexibility and performance are presented, and their operation using high speed data signals is analyzed numerica......In this paper, we present recent progress in modeling, design, fabrication and experimental characterization of InP photonic crystal all-optical switches. Novel designs with increased flexibility and performance are presented, and their operation using high speed data signals is analyzed...

  8. Synthesis, characterization, crystal structure determination and computational study of a new Cu(II) complex of bis [2-{(E)-[2-chloroethyl)imino]methyl}phenolato)] copper(II) Schiff base complex

    Science.gov (United States)

    Grivani, Gholamhossein; Vakili, Mohammad; Khalaji, Aliakbar Dehno; Bruno, Giuseppe; Rudbari, Hadi Amiri; Taghavi, Maedeh

    2016-07-01

    The copper (II) Schiff base complex of [CuL2] (1), HL = 2-{(E)-[2-chloroethyl) imino]methyl}phenol, has been synthesized and characterized by elemental (CHN) analysis, UV-Vis and FT-IR spectroscopy. The molecular structure of 1 was determined by single crystal X-ray diffraction technique. The conformational analysis and molecular structures of CuL2 were investigated by means of density functional theory (DFT) calculations at B3LYP/6-311G* level. An excellent agreement was observed between theoretical and experimental results. The Schiff base ligand of HL acts as a chelating ligand and coordinates via one nitrogen atom and one oxygen atom to the metal center. The copper (II) center is coordinated by two nitrogen atoms and two oxygen atoms from two Schiff base ligands in an approximately square planar trans-[MN2O2] coordination geometry. Thermogravimetric analysis of CuL2 showed that it was decomposed in five stages. In addition, the CuL2 complex thermally decomposed in air at 660 °C and the XRD pattern of the obtained solid showed the formation of CuO nanoparticles with an average size of 34 nm.

  9. Crystal structure of mammalian acid sphingomyelinase.

    Science.gov (United States)

    Gorelik, Alexei; Illes, Katalin; Heinz, Leonhard X; Superti-Furga, Giulio; Nagar, Bhushan

    2016-01-01

    Acid sphingomyelinase (ASMase, ASM, SMPD1) converts sphingomyelin into ceramide, modulating membrane properties and signal transduction. Inactivating mutations in ASMase cause Niemann-Pick disease, and its inhibition is also beneficial in models of depression and cancer. To gain a better understanding of this critical therapeutic target, we determined crystal structures of mammalian ASMase in various conformations. The catalytic domain adopts a calcineurin-like fold with two zinc ions and a hydrophobic track leading to the active site. Strikingly, the membrane interacting saposin domain assumes either a closed globular conformation independent from the catalytic domain, or an open conformation, which establishes an interface with the catalytic domain essential for activity. Structural mapping of Niemann-Pick mutations reveals that most of them likely destabilize the protein's fold. This study sheds light on the molecular mechanism of ASMase function, and provides a platform for the rational development of ASMase inhibitors and therapeutic use of recombinant ASMase. PMID:27435900

  10. The Crystal Structure of Human Argonaute2

    Energy Technology Data Exchange (ETDEWEB)

    Schirle, Nicole T.; MacRae, Ian J. (Scripps)

    2012-07-18

    Argonaute proteins form the functional core of the RNA-induced silencing complexes that mediate RNA silencing in eukaryotes. The 2.3 angstrom resolution crystal structure of human Argonaute2 (Ago2) reveals a bilobed molecule with a central cleft for binding guide and target RNAs. Nucleotides 2 to 6 of a heterogeneous mixture of guide RNAs are positioned in an A-form conformation for base pairing with target messenger RNAs. Between nucleotides 6 and 7, there is a kink that may function in microRNA target recognition or release of sliced RNA products. Tandem tryptophan-binding pockets in the PIWI domain define a likely interaction surface for recruitment of glycine-tryptophan-182 (GW182) or other tryptophan-rich cofactors. These results will enable structure-based approaches for harnessing the untapped therapeutic potential of RNA silencing in humans.

  11. The crystal structure of scandium dyhydrate triglycolate

    International Nuclear Information System (INIS)

    The structure of colorless crystals of scandium glycolate dehydrate Sc(CH2OHCOO)3x2H2O, 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/cm3; 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

  12. Structure, thermodynamics, and crystallization of amorphous hafnia

    International Nuclear Information System (INIS)

    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/HfO2. The crystallization temperature is estimated to be 421 K. The calculations suggest an explanation for the low thermal stability of amorphous hafnia

  13. 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.

  14. Synthesis, crystal structure and characterization of new biologically active Cu(II) complexes with ligand derived from N-substituted sulfonamide

    Indian Academy of Sciences (India)

    ADRIANA CORINA HANGAN; ALEXANDRU TURZA; ROXANA LIANA STAN; BOGDAN SEVASTRE; EMÖKE PÁLL; SÎNZIANA CETEAN; LUMINI¸TA SIMONA OPREAN

    2016-05-01

    A new N-sulfonamide ligand (HL1= N-(5-(4-methoxyphenyl)-[1,3,4]–thiadiazole–2-yl)-toluenesulfonamide)and two Cu(II) complexes, $[Cu(L1)­_{2}(py)_{2}]$ (C1) and $[Cu(L2)_{2}(py)_{2}(H_{2}O)]$ (C2) (HL2 = N-(5-(4-methylphenyl)-[1,3,4]–thiadiazole–2-yl)-benzenesulfonamide) were synthesized. The X-ray crystal structuresof the complexes were determined. In the complex C1, the Cu(II) ion is four-coordinated, forming a $CuN_{4}$ chromophore and in the complex C2, the Cu(II) ion is five-coordinated, forming a $CuN_{4}O$ chromophore. Theligand acts as monodentate, coordinating the Cu(II) ion through a single $N_{thiadiazole}$ atom. The molecules fromthe reaction medium (pyridine and water) are also involved in the coordination of the Cu(II) ion. The complexesC1 and C2 are square-planar and a slightly distorted square pyramidal, respectively. The compounds werecharacterized by FT-IR, electronic, EPR spectroscopic and magnetic methods. The nuclease binding activitystudies of the synthesized complexes confirm their capacity to cleave the DNA molecule. The cytotoxicitystudies were carried out on melanoma cell line WM35 which confirm that both compounds inhibit the growthof these cells. They have a higher activity compared to a platinum drug, carboplatin.

  15. Synthesis, Crystal Structure and Characterization of a Novel Super Molecule [Na(C60H80O12)]+[Au(SCN)4]%金(Ⅲ)与杯[4]乙酯合钠(Ⅰ)超分子化合物:[Na(C60H80O12)]+[Au(SCN)4]-的合成、结构及性能

    Institute of Scientific and Technical Information of China (English)

    付勇; 徐琰; 宋毛平; 吴养洁

    2005-01-01

    A novel super molecule [Na(C60H80O12)]+[Au(SCN)4]- was obtained by extraction of calix[4] arene (L) for an aqueous solution containing [AuCl4]-, and NaCl into CH2Cl2. The crystal structure and properties of the title super molecule were characterized by single-crystal X-ray diffraction, IR and 1H NMR spectra. The X-ray single crystal structure analysis shows that the crystal was Tetragonal system with space group P4/n and the unit cell parameters were as follows: a=2.880 8(18) nm, b=2.880 8(18) nm, c=2.2924(5) nm, and final R indices [I>2σ(I)]:R1=0.0485, wR2=0.1061. CCDC: 243229.

  16. Synthesis and Characterization of Star-like Liquid Crystals Centered by Silicon

    Institute of Scientific and Technical Information of China (English)

    Jian Qiang LIU; Qi Zhen ZHANG; Jing Zhi ZHANG

    2004-01-01

    The synthesis and characterization of two new star-like liquid crystals are reported.They are made of a silicon core and four alkoxyazobenzene monomers in the periphery. Their phase behaviors and the structures are determined by infrared absorption spectroscopy (IR),nuclear magnetic resonance spectroscopy (NMR), elemental analysis (EA), polarizing optical microscope (POM) and differential scanning calorimetry (DSC).

  17. Prediction of binary hard-sphere crystal structures.

    Science.gov (United States)

    Filion, Laura; Dijkstra, Marjolein

    2009-04-01

    We present a method based on a combination of a genetic algorithm and Monte Carlo simulations to predict close-packed crystal structures in hard-core systems. We employ this method to predict the binary crystal structures in a mixture of large and small hard spheres with various stoichiometries and diameter ratios between 0.4 and 0.84. In addition to known binary hard-sphere crystal structures similar to NaCl and AlB2, we predict additional crystal structures with the symmetry of CrB, gammaCuTi, alphaIrV, HgBr2, AuTe2, Ag2Se, and various structures for which an atomic analog was not found. In order to determine the crystal structures at infinite pressures, we calculate the maximum packing density as a function of size ratio for the crystal structures predicted by our GA using a simulated annealing approach. PMID:19518387

  18. Crystal structure of bacterioferritin from Rhodobacter sphaeroides

    International Nuclear Information System (INIS)

    Iron is essential for the survival of organisms, but either excess or deficient levels of iron induce oxidative stress, thereby causing cell damage. As a result, iron regulation is essential for proper cell growth and proliferation in most organisms. Bacterioferritin is a ferritin-like family protein that contains a heme molecule and a ferroxidase site at the di-iron center. This protein plays a primary role in intracellular iron storage for iron homeostasis, as well as in the maintenance of iron in a soluble and non-toxic form. Although several bacterioferritin structures have been determined, no structural studies have successfully elucidated the molecular function of the heme molecule and the ferroxidase center. Here, we report the crystal structure of bacterioferritin from Rhodobacter sphaeroides. This protein exists in a roughly spherical configuration via the assembly of 24 subunits. We describe the oligomeric arrangement, ferroxidase center and heme-binding site based on this structure. The protein contains a single iron-binding configuration in the ferroxidase center, which allows for the release of iron by His130 when the protein is in the intermediate state. The heme molecule in RsBfr is stabilized by shifting of the van der Waals interaction center between the porphyrin of the heme and Trp26. We anticipate that further structural analysis will provide a more complete understanding of the molecular mechanisms of members of the ferritin-like family.

  19. 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: 0.484, year: 2014

  20. Synthesis, characterization, crystal structure, and theoretical studies on Schiff-base compound 6-[(5-Bromopyridin-2-yl)iminomethyl]phenol

    Czech Academy of Sciences Publication Activity Database

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

    2010-01-01

    Roč. 21, č. 1 (2010), s. 153-157. ISSN 1040-0400 Grant ostatní: GA AV ČR(CZ) Praemium Academiae Institutional research plan: CEZ:AV0Z10100521 Keywords : Schiff base * X-ray structure analysis * Jana2006 * DFT calculation Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.727, year: 2010

  1. Synthesis and Crystal Structure of a Degraded Dehydroabietylamine Thiophene Imine

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    A degraded dehydroabietylamine thiophene imine (C24H30NS, Mr-364.55)has been synthesized from dehydroabietic acid, and its structure was characterized by IR, 1HNMR spectroscopy and single-crystal X-ray diffraction.White crystals of the title compound crystallize in the monoclinic system, space group P21 with a = 5.9490(12), b = 16.337(3), c = 10.780(2)(A), β= 92.21(3)°, V = 1046.9(3)(A)3, Z = 2, Dc = 1.156g/cm3, λ= 0.71073(A),μ= 0.162 mm-1, F(000) = 394, the final R = 0.0443 and wR = 0.0805 for 1325 observed reflections with(I>2σ(I).The imine group was directly attached to the chiral carbon atom of tricyclo hydrophenthenrane structure with a trans configuration.The dihedral angle between two aromatic rings is 88.3°.

  2. Photonic Crystals: Advances in Design, Fabrication, and Characterization

    Science.gov (United States)

    Busch, Kurt; Lölkes, Stefan; Wehrspohn, Ralf B.; Föll, Helmut

    2004-03-01

    The majority of the contributions in this topically edited book stems from the priority program SPP 1113 "Photonische Kristalle" run by the Deutsche Forschungsgemeinschaft (DFG), resulting in a survey of the current state of photonic crystal research in Germany. The first part of the book describes methods for the theoretical analysis of their optical properties as well as the results. The main part is dedicated to the fabrication, characterization and modeling of two- and three-dimensional photonic crystals, while the final section presents a wide spectrum of applications: gas sensors, micro-lasers, and photonic crystal fibers. Illustrated in full color, this book is not only of interest to advanced students and researchers in physics, electrical engineering, and material science, but also to company R&D departments involved in photonic crystal-related technological developments.

  3. Crystal structures of five 6-mercaptopurine derivatives.

    Science.gov (United States)

    Gomes, Lígia R; Low, John Nicolson; Magalhães E Silva, Diogo; Cagide, Fernando; Borges, Fernanda

    2016-03-01

    The crystal structures of five 6-mercaptopurine derivatives, viz. 2-[(9-acetyl-9H-purin-6-yl)sulfan-yl]-1-(3-meth-oxy-phen-yl)ethan-1-one (1), C16H14N4O3S, 2-[(9-acetyl-9H-purin-6-yl)sulfan-yl]-1-(4-meth-oxy-phen-yl)ethan-1-one (2), C16H14N4O3S, 2-[(9-acetyl-9H-purin-6-yl)sulfan-yl]-1-(4-chloro-phen-yl)ethan-1-one (3), C15H11ClN4O2S, 2-[(9-acetyl-9H-purin-6-yl)sulfan-yl]-1-(4-bromo-phen-yl)ethan-1-one (4), C15H11BrN4O2S, and 1-(3-meth-oxy-phen-yl)-2-[(9H-purin-6-yl)sulfan-yl]ethan-1-one (5), C14H12N4O2S. Compounds (2), (3) and (4) are isomorphous and accordingly their mol-ecular and supra-molecular structures are similar. An analysis of the dihedral angles between the purine and exocyclic phenyl rings show that the mol-ecules of (1) and (5) are essentially planar but that in the case of the three isomorphous compounds (2), (3) and (4), these rings are twisted by a dihedral angle of approximately 38°. With the exception of (1) all mol-ecules are linked by weak C-H⋯O hydrogen bonds in their crystals. There is π-π stacking in all compounds. A Cambridge Structural Database search revealed the existence of 11 deposited compounds containing the 1-phenyl-2-sulfanyl-ethanone scaffold; of these, only eight have a cyclic ring as substituent, the majority of these being heterocycles. PMID:27006794

  4. Crystal structures of five 6-mercaptopurine derivatives

    Directory of Open Access Journals (Sweden)

    Lígia R. Gomes

    2016-03-01

    Full Text Available The crystal structures of five 6-mercaptopurine derivatives, viz. 2-[(9-acetyl-9H-purin-6-ylsulfanyl]-1-(3-methoxyphenylethan-1-one (1, C16H14N4O3S, 2-[(9-acetyl-9H-purin-6-ylsulfanyl]-1-(4-methoxyphenylethan-1-one (2, C16H14N4O3S, 2-[(9-acetyl-9H-purin-6-ylsulfanyl]-1-(4-chlorophenylethan-1-one (3, C15H11ClN4O2S, 2-[(9-acetyl-9H-purin-6-ylsulfanyl]-1-(4-bromophenylethan-1-one (4, C15H11BrN4O2S, and 1-(3-methoxyphenyl-2-[(9H-purin-6-ylsulfanyl]ethan-1-one (5, C14H12N4O2S. Compounds (2, (3 and (4 are isomorphous and accordingly their molecular and supramolecular structures are similar. An analysis of the dihedral angles between the purine and exocyclic phenyl rings show that the molecules of (1 and (5 are essentially planar but that in the case of the three isomorphous compounds (2, (3 and (4, these rings are twisted by a dihedral angle of approximately 38°. With the exception of (1 all molecules are linked by weak C—H...O hydrogen bonds in their crystals. There is π–π stacking in all compounds. A Cambridge Structural Database search revealed the existence of 11 deposited compounds containing the 1-phenyl-2-sulfanylethanone scaffold; of these, only eight have a cyclic ring as substituent, the majority of these being heterocycles.

  5. 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.

  6. 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).

  7. Synthesis, crystal structure, spectral characterization and photoluminescence property of three Cd(II) complexes with a pyrazole based Schiff-base ligand

    Science.gov (United States)

    Mandal, Susmita; Saha, Rajat; Saha, Manan; Pradhan, Rajesh; Butcher, Ray J.; Saha, Nitis Chandra

    2016-04-01

    Substituted pyrazole containing Schiff-base ligand, 5-methyl-3-formylpyrazole-N-(2‧-methylphenoxy)methyleneimine, (MPzOA), afforded three new Cd(II) complexes, [Cd(MPzOA)Cl2]2.CH3OH (I), [Cd(MPzOA)2(H2O)2](ClO4)2 (II) and [Cd(MPzOA)(H2O)(NO3)2] (III). In the reported complex species the coordination number and geometry of Cd(II) vary. In complex I and II, Cd(II) adopts six and in (III) it adopts eight coordination modes, with prismatic, octahedral and distorted dodecahedral geometry, respectively. All the complexes are characterized by IR, 1H NMR, UV-Vis spectral parameters and X-ray analyses. The complexes have 1D, 2D and 3D supramolecular frameworks formed by non-covalent interactions, like hydrogen bonding, π … π stacking, C-H … π interactions.

  8. 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

  9. Protein crystal screening and characterization for serial femtosecond nanocrystallography

    Science.gov (United States)

    Darmanin, Connie; Strachan, Jamie; Adda, Christopher G.; Ve, Thomas; Kobe, Bostjan; Abbey, Brian

    2016-01-01

    The recent development of X-ray free electron lasers (XFELs) has spurred the development of serial femtosecond nanocrystallography (SFX) which, for the first time, is enabling structure retrieval from sub-micron protein crystals. Although there are already a growing number of structures published using SFX, the technology is still very new and presents a number of unique challenges as well as opportunities for structural biologists. One of the biggest barriers to the success of SFX experiments is the preparation and selection of suitable protein crystal samples. Here we outline a protocol for preparing and screening for suitable XFEL targets. PMID:27139248

  10. Modeling Polymorphic Molecular Crystals with Electronic Structure Theory.

    Science.gov (United States)

    Beran, Gregory J O

    2016-05-11

    Interest in molecular crystals has grown thanks to their relevance to pharmaceuticals, organic semiconductor materials, foods, and many other applications. Electronic structure methods have become an increasingly important tool for modeling molecular crystals and polymorphism. This article reviews electronic structure techniques used to model molecular crystals, including periodic density functional theory, periodic second-order Møller-Plesset perturbation theory, fragment-based electronic structure methods, and diffusion Monte Carlo. It also discusses the use of these models for predicting a variety of crystal properties that are relevant to the study of polymorphism, including lattice energies, structures, crystal structure prediction, polymorphism, phase diagrams, vibrational spectroscopies, and nuclear magnetic resonance spectroscopy. Finally, tools for analyzing crystal structures and intermolecular interactions are briefly discussed. PMID:27008426

  11. Synthesis and Crystal Structure of a Novel Calix [8] arene Ester Derivative

    Institute of Scientific and Technical Information of China (English)

    DaQiangYUAN; RuJiWANG; 等

    2002-01-01

    The synthesis and crystal structure of a novel calix[8] arene ester are reported herein. The calix [8] arene ester derivative has been characterized by IR,NMR and X-ray crystal analysis. The X-ray structure analysis revealed that the 8 phenolic hydroxy groups of the calix [8] arene have been substituted by 4 diethyl dibromomalonate molecules with each two adjacent hydroxy oxygen atoms attached to a bridge diethyl malonate.

  12. Crystal Structure of Iodotyrosine Deiodinase, a Novel Flavoprotein Responsible for Iodide Salvage in Thyroid Glands*

    OpenAIRE

    Thomas, Seth R.; McTamney, Patrick M.; Adler, Jennifer M.; LaRonde-LeBlanc, Nicole; Rokita, Steven E.

    2009-01-01

    The flavoprotein iodotyrosine deiodinase (IYD) salvages iodide from mono- and diiodotyrosine formed during the biosynthesis of the thyroid hormone thyroxine. Expression of a soluble domain of this membrane-bound enzyme provided sufficient material for crystallization and characterization by x-ray diffraction. The structures of IYD and two co-crystals containing substrates, mono- and diiodotyrosine, alternatively, were solved at resolutions of 2.0, 2.45, and 2.6 Å, respectively. The structure ...

  13. Crystal structure of zirconia by Rietveld refinement

    Institute of Scientific and Technical Information of China (English)

    王大宁; 郭永权; 梁开明; 陶琨

    1999-01-01

    The crystal structures and phase transformation of zirconia ceramics have been investigated by means of X-ray powder diffraction and Rietveld powder diffraction profile fitting technique. A structural transition from monoclinic to tetragonal occurs when Y2O3 and CeO2 are doped into zirconia. The space group of the tetragonal structure is P42/nmc, Z=2. The lattice parameters are α=0.362 6(5) nm, c=0.522 6(3)nm for CeO2 doped zirconia and α=0. 360 2(8)nm, c=0. 517 9(1)nm for Y2O3 doped zirconia, respectively. In each unit cell, there are two kinds of equivalent positions, i. e. 2b and 4d, which are occupied by Zr4+, M(M=Y3+, Ce4+) cations and O2- anions, respectively. The crystallographic correlation among the cubic, tetragonal and monoclinic structures of ZrO2 is discussed.

  14. Crystal and molecular structure of aflatrem

    Directory of Open Access Journals (Sweden)

    Bruno N. Lenta

    2015-11-01

    Full Text Available The crystal structure of the title compound, C32H39NO4, confirms the absolute configuration of the seven chiral centres in the molecule. The molecule has a 1,1-dimethylprop-2-enyl substituent on the indole nucleus and this nucleus shares one edge with the five-membered ring which is, in turn, connected to a sequence of three edge-shared fused rings. The skeleton is completed by the 7,7-trimethyl-6,8-dioxabicyclo[3.2.1]oct-3-en-2-one group connected to the terminal cyclohexene ring. The two cyclohexane rings adopt chair and half-chair conformations, while in the dioxabicyclo[3.2.1]oct-3-en-2-one unit, the six-membered ring has a half-chair conformation. The indole system of the molecule exhibits a tilt of 2.02 (1° between its two rings. In the crystal, O—H...O hydrogen bonds connect molecules into chains along [010]. Weak N—H...π interactions connect these chains, forming sheets parallel to (10-1.

  15. Crystal Structures of Respiratory Pathogen Neuraminidases

    Energy Technology Data Exchange (ETDEWEB)

    Hsiao, Y.; Parker, D; Ratner, A; Prince, A; Tong, L

    2009-01-01

    Currently there is pressing need to develop novel therapeutic agents for the treatment of infections by the human respiratory pathogens Pseudomonas aeruginosa and Streptococcus pneumoniae. The neuraminidases of these pathogens are important for host colonization in animal models of infection and are attractive targets for drug discovery. To aid in the development of inhibitors against these neuraminidases, we have determined the crystal structures of the P. aeruginosa enzyme NanPs and S. pneumoniae enzyme NanA at 1.6 and 1.7 {angstrom} resolution, respectively. In situ proteolysis with trypsin was essential for the crystallization of our recombinant NanA. The active site regions of the two enzymes are strikingly different. NanA contains a deep pocket that is similar to that in canonical neuraminidases, while the NanPs active site is much more open. The comparative studies suggest that NanPs may not be a classical neuraminidase, and may have distinct natural substrates and physiological functions. This work represents an important step in the development of drugs to prevent respiratory tract colonization by these two pathogens.

  16. Synthesis, characterization, and crystal structure of 5,5″-Difluoro-1 H,1″ H-[3,3':3',3″-terindol]-2'(1' H)-one

    Science.gov (United States)

    Sharma, Sakshi; Banerjee, Bubun; Brahmachari, Goutam; Kant, Rajni; Gupta, Vivek K.

    2016-03-01

    The new indole derivative, 5,5''-Difluoro-1 H,1'' H-[3,3':3',3''-terindol]-2'(1' H)-one C24H15F2N3O, is synthesized in 87% yield, and its crystal structure is determined by X-ray structure analysis. The crystals are monoclinic, sp. gr. P21/ n, a = 15.4563(7), b = 10.8340(6), c = 16.4718(6) Å, β = 102.403(4)°, Z = 4. Bicyclic indole moieties form dihedral angle of 61.92(5)° with each other; the oxindole ring is twisted with respect to them at angles of 85.70(5)° and 75.62(5)°. The crystal structure is stabilized by N-H···O and C-H···O hydrogen bonds involving both the DMSO solvent molecules. In addition, one C-H···π interaction is observed.

  17. Introduction of structural investigation using single crystal neutron diffraction

    International Nuclear Information System (INIS)

    Introduction of neutron structure analysis using single crystal is described. Starting two-dimensional case, principle of diffraction geometry is discussed, and then it is extend to three-dimensional measurements. For that experiment, two dimensional detector and four-circle diffractometer are used, and the methodology of these diffractometer is described. Then, the basic theory of crystal and magnetic structure analysis is given. Finally some example of crystal and magnetic structure analysis are shown. (author)

  18. Structural perfection and residual electric resistance of tungsten single crystals

    International Nuclear Information System (INIS)

    A study was made into residual relative resistance (RRR) and structural perfection (SP) of tungsten single crystals, grown by electron beam zone melting using seeding crystals of several orientations, namely, , , , . The single crystals were of 99.98 and 99.9995 wt.% purity. The RRR value is found to depend on crystallographic orientation of an axis of crystal growth and to correlate with SP. Single crystals of different purity are differ in the nature of orientational dependences. It is shown that the correlation between RRR and SP of crystals is mainly due to conduction electron scattering by subgrain boundaries (internal size effect)

  19. Hydrothermal Synthesis, Crystal Structure and Characterization of a Microporous 3D Pillared-Layer 3d-4f Copper-Holmium Heterometallic Coordination Polymer

    International Nuclear Information System (INIS)

    A microporous 3D pillared-layer 3d-4f (Cu+-Ho3+) coordination polymer based on the linkages of 2D wavelike Ho-carboxylate layers and 1D Cu4Br4 inorganic chains in centipede-type structure by IN. pillars has been obtained. Furthermore, the magnetic properties of this complex have been investigated. Our results provide an intriguing example of 3D 3d-4f PCPs and further demonstrate that the pillared-layer approach can be used for constructing novel 3D 3d-4f PCPs. There has been more and more interest in recent years in the design and synthesis of porous coordination polymers (PCPs) not only for their fascinating structural diversity but also for their potential applications as functional materials in magnetism, molecular adsorption, gas storage, ion exchange, catalysis and separation. Up to now, almost all approaches to the construction of porous materials have focused on the 3D monometallic PCPs. However, the preparation of hetero-metallic PCPs especially containing lanthanide (Ln) and transition metal (TM) ions has been drawn less attention. A pillared-layer approach to the construction of 3D 3d-4f coordination polymers upon the connections of Ln-carboxylate layers and TM-inorganic motifs by organic pillars via coordination bonding has been reported. In most such 3D pillared-layer 3d-4f structures, TM-inorganic layers/chains generally obstruct the development of channels based on the pores formed by Ln-carboxylate layers

  20. Syntheses and crystal structures of two new organically templated borates

    International Nuclear Information System (INIS)

    Two new organically templated borates, [H3N(C6H10)NH3][B4O5(OH)4] (1) and [H3N(C6H10)NH3][B5O8(OH)] (2) have been synthesized in the presence of trans-1,4-diaminocyclohexane acting as a structure-directing agent under mild solvothermal conditions. The structures were determined by single crystal X-ray diffraction and further characterized by FTIR, elemental analysis and thermogravimetric analysis. Compound 1 crystallizes in the monoclinic system, space group C2/c (No. 15), a=9.1325(3)A, b=11.4869(3)A, c=12.2756(5)A, β=105.258(6)o, V=1242.37(7)A3, Z=4. The structure contains supramolecular hydrogen-bonded network formed by isolated [B4O5(OH)4]2- polyanions. 2 is monoclinic, space group P2(1)/n (No. 14), a=6.5176(2)A, b=16.8861(5)A, c=11.1522(7)A, β=91.897(6)o, V=1226.70(9)A3, Z=4. The structure consists of layers of 3,9-membered boron rings constructed from pentaborate anion groups [B5O8(OH)]2-. The adjacent borate layers are further linked with each other by hydrogen bond to form a 3D supramolecular network. It is the first example of layered borates templated by an organic amine

  1. Synthesis, Characterization, Theoretical Crystal Structure, and Antibacterial Activities of Some Transition Metal Complexes of the Thiosemicarbazone (Z-2-(pyrrolidin-2-ylidenehydrazinecarbothioamide

    Directory of Open Access Journals (Sweden)

    Ahmed A. Al-Amiery

    2011-01-01

    Full Text Available Problem Statement. In Iraq like most third world countries, attempts discovered new antibiotic drugs derived from thiosemicarbazide and its metal complexes and developed the branch of applied in organic chemistry. Approach. New (Z-2-(pyrrolidin-2-ylidenehydrazinecarbothioamide (L was synthesized in a good yield by the reaction of pyrrolidone with thiosemicarbazide. Co(II, Ni(II, and Cu(II complexes of (L were prepared and characterized by FT-IR, UV/visible spectra, 1HNMR, and CHN analyses. Moreover, charge, bond length, bond angle, twist angle, heat of formation, and steric energy were calculated by using of the ChemOffice program, and the DFT calculations for the complexes were done. The free ligand and its metal complexes were tested in vitro against several microorganisms (Staphylococcus aurous, E. coli, Proteus vulgaris, Pseudomonas, and Klebsiella pneumoniae to assess their antimicrobial properties. Results. The study shows that these complexes have octahedral geometry; in addition, it has high activity against tested bacteria. Conclusion/Recommendations. Based on the reported results, it may be concluded that ligand acts as bidentate, neutral ligand, coordinating through one of the nitrogen and sulfur atoms.

  2. Synthesis, Characterization, Theoretical Crystal Structure, and Antibacterial Activities of Some Transition Metal Complexes of the Thiosemicarbazone (Z)-2-(pyrrolidin-2-ylidene)hydrazinecarbothioamide

    Science.gov (United States)

    Al-Amiery, Ahmed A.; Al-Majedy, Yasmien K.; Abdulreazak, Haziem; Abood, Hussain

    2011-01-01

    Problem Statement. In Iraq like most third world countries, attempts discovered new antibiotic drugs derived from thiosemicarbazide and its metal complexes and developed the branch of applied in organic chemistry. Approach. New (Z)-2-(pyrrolidin-2-ylidene)hydrazinecarbothioamide (L) was synthesized in a good yield by the reaction of pyrrolidone with thiosemicarbazide. Co(II), Ni(II), and Cu(II) complexes of (L) were prepared and characterized by FT-IR, UV/visible spectra, 1HNMR, and CHN analyses. Moreover, charge, bond length, bond angle, twist angle, heat of formation, and steric energy were calculated by using of the ChemOffice program, and the DFT calculations for the complexes were done. The free ligand and its metal complexes were tested in vitro against several microorganisms (Staphylococcus aurous, E. coli, Proteus vulgaris, Pseudomonas, and Klebsiella pneumoniae) to assess their antimicrobial properties. Results. The study shows that these complexes have octahedral geometry; in addition, it has high activity against tested bacteria. Conclusion/Recommendations. Based on the reported results, it may be concluded that ligand acts as bidentate, neutral ligand, coordinating through one of the nitrogen and sulfur atoms. PMID:21804771

  3. Crystal structure of phenyl N-(4-nitrophenylcarbamate

    Directory of Open Access Journals (Sweden)

    Y. AaminaNaaz

    2015-12-01

    Full Text Available The asymmetric unit of the title compound, C13H10N2O4, contains two independent molecules (A and B. The dihedral angle between the aromatic rings is 48.18 (14° in molecule A and 45.81 (14° in molecule B. The mean plane of the carbamate N—C(=O—O group is twisted slightly from the attached benzene and phenyl rings, making respective dihedral angles of 12.97 (13 and 60.93 (14° in A, and 23.11 (14 and 59.10 (14° in B. In the crystal, A and B molecules are arranged alternately through N—H...O hydrogen bonds and C—H...π interactions, forming chains along the a axis. The chains are further linked by C—H...O hydrogen bonds into a double-chain structure.

  4. Synthesis, characterization, X-ray crystal structure, electrochemical evaluation and anti-cancer studies of a mixed ligand Cu(II) complex of (E)-N′-((2-hydroxynaphthalen-1-yl)methylene)acetohydrazide

    Indian Academy of Sciences (India)

    Iran Sheikhshoaie; S Yousef Ebrahimipour; Mahdieh Sheikhshoaie; Maryam Mohamadi; Mehdi Abbasnejad; Hadi Amiri Rudbari; Giuseppe Bruno

    2015-12-01

    A ternary mixed ligand Cu(II) complex, [Cu(L)(Phen)], was prepared from the reaction of (E)-N′-((2-hydroxynaphthalen-1-yl)methylene)acetohydrazide [HL], Cu(NO3)2.3H2O and 1,10-Phenanthroline in 1:1:1 molar ratio. This complex was fully characterized using spectroscopic and physicochemical methods. The structure of the complex was determined by single crystal X-ray diffraction. The Cu(II) center is coordinated by two oxygen and one nitrogen donors of L2− and nitrogen atoms of the heterocyclic group. Electrochemical studies of the Cu(II) complex showed shifts in the ligand peaks as well as the appearance of new peaks after complexation. The electrochemical behavior of the Cu(II) complex was also studied using cyclic voltammetry. According to biochemical investigation (MCF-7 cells viability), anticancer activity of [Cu(L)(Phen)] was higher than those of Cu(NO3)2.3H2O, HL and 1,10-Phenanthroline.

  5. Synthesis, Characterization and Thermal Studies of Zn(II), Cd(II) and Hg(II) Complexes of N-Methyl-N-Phenyldithiocarbamate: The Single Crystal Structure of [(C6H5)(CH3)NCS2]4Hg2

    Science.gov (United States)

    Onwudiwe, Damian C.; Ajibade, Peter A.

    2011-01-01

    Zn(II), Cd(II) and Hg(II) complexes of N-methyl-N-phenyl dithiocarbamate have been synthesized and characterized by elemental analysis and spectral studies (IR, 1H and 13C-NMR). The single crystal X-ray structure of the mercury complex revealed that the complex contains a Hg centre with a distorted tetrahedral coordination sphere in which the dinuclear Hg complex resides on a crystallographic inversion centre and each Hg atom is coordinated to four S atoms from the dithiocarbamate moiety. One dithiocarbamate ligand acts as chelating ligand while the other acts as chelating bridging ligand between two Hg atoms, resulting in a dinuclear eight-member ring. The course of the thermal degradation of the complexes has been investigated using thermogravimetric and differential thermal analyses techniques. Thermogravimetric analysis of the complexes show a single weight loss to give MS (M = Zn, Cd, Hg) indicating that they might be useful as single source precursors for the synthesis of MS nanoparticles and thin films. PMID:21673933

  6. Synthesis, characterization and crystal structures of the bidentate Schiff base N,N'-bis(2-nitrocinnamaldehyde)ethylenediamine and its complex with CuNCS and triphenylphosphane.

    Science.gov (United States)

    Clegg, William; Harrington, Ross W; Barati, Kazem; Habibi, Mohammad Hossein; Montazerozohori, Morteza; Lalegani, Arash

    2015-07-01

    Reaction of copper(I) thiocyanate and triphenylphosphane with the bidentate Schiff base N,N'-bis(trans-2-nitrocinnamaldehyde)ethylenediamine {Nca2en, (1); systematic name (1E,1'E,2E,2'E)-N,N'-(ethane-1,2-diyl)bis[3-(2-nitrophenyl)prop-2-en-1-imine]}, C20H18N4O4, in a 1:1:1 molar ratio in acetonitrile resulted in the formation of the complex {(1E,1'E,2E,2'E)-N,N'-(ethane-1,2-diyl)bis[3-(2-nitrophenyl)prop-2-en-1-imine]-κ(2)N,N'}(thiocyanato-κN)(triphenylphosphane-κP)copper(I)], [Cu(NCS)(C20H18N4O4)(C18H15P)] or [Cu(NCS)(Nca2en)(PPh3)], (2). The Schiff base and copper(I) complex have been characterized by elemental analyses, IR, electronic and (1)H NMR spectroscopy, and X-ray crystallography [from synchrotron data for (1)]. The molecule of (1) lies on a crystallographic inversion centre, with a trans conformation for the ethylenediamine unit, and displays significant twists from coplanarity of its nitro group, aromatic ring, conjugated chain and especially ethylenediamine segments. It acts as a bidentate ligand coordinating via the imine N atoms to the Cu(I) atom in complex (2), in which the ethylenediamine unit necessarily adopts a somewhat flattened gauche conformation, resulting in a rather bowed shape overall for the ligand. The NCS(-) ligand is coordinated through its N atom. The geometry around the Cu(I) atom is distorted tetrahedral, with a small N-Cu-N bite angle of 81.56 (12)° and an enlarged opposite angle of 117.29 (9)° for SCN-Cu-P. Comparisons are made with the analogous Schiff base having no nitro substituents and with metal complexes of both ligands. PMID:26146396

  7. Isomorph invariance of the structure and dynamics of classical crystals

    DEFF Research Database (Denmark)

    Albrechtsen, Dan; Olsen, Andreas Elmerdahl; Pedersen, Ulf Rørbæk; Schrøder, Thomas; Dyre, J. C.

    2014-01-01

    , which is generally a good description except significantly below melting. The existence of isomorphs for crystals is validated by simulations of particles interacting via the Lennard-Jones pair potential arranged into a face-centered cubic (fcc) crystalline structure; the slow vacancy-jump dynamics of a......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...... defective fcc crystal is also shown to be isomorph invariant. In contrast, a NaCl crystal model does not exhibit isomorph invariances. Other systems simulated, though in less detail, are the Wahnström binary Lennard-Jones crystal with the MgZn2 Laves crystal structure, monatomic fcc crystals of particles...

  8. Characterization of DPOAE fine structure

    DEFF Research Database (Denmark)

    Reuter, Karen; Hammershøi, Dorte

    has recently been demonstrated to exist in low level equal-loudness contours. The character of the DPOAE fine structure depends on several parameters, i.e., level, frequencies, and frequency of the two primaries, but also level and character of the noise floor. The prevalence and character of the fine......The distortion product otoacoustic emission (DPOAE) fine structure is revealed, when measuring DPOAE with a very fine frequency resolution. It is characterized by consistent maxima and minima with notches of up to 20 dB depth. The fine structure is known also from absolute hearing thresholds, and...... structures are highly individual, and till now no standardized method has been suggested for a consistent categorization. In the present paper a method developed for the categorization of fine structures is presented. The method has been used in two previous studies on the prevalence of fine structures, 1...

  9. Electrical and structural characterizations of crystallized Al{sub 2}O{sub 3}/GaN interfaces formed by in situ metalorganic chemical vapor deposition

    Energy Technology Data Exchange (ETDEWEB)

    Liu, X., E-mail: xliu@ece.ucsb.edu; Yeluri, R.; Kim, J.; Keller, S.; Mishra, U. K. [Department of Electrical and Computer Engineering, University of California, Santa Barbara, California 93106 (United States); Jackson, C. M.; Arehart, A. R.; Ringel, S. A. [Department of Electrical and Computer Engineering, The Ohio State University, Columbus, Ohio 43210 (United States); Wu, F.; Mazumder, B.; Speck, J. S. [Materials Department, University of California, Santa Barbara, California 93106 (United States)

    2016-01-07

    Al{sub 2}O{sub 3} films were grown in situ by metalorganic chemical vapor deposition at 900 °C on GaN of both Ga- and N-face polarities. High-resolution transmission electron microscopy revealed that the Al{sub 2}O{sub 3} films were crystalline and primarily γ-phase. The Al{sub 2}O{sub 3}/Ga-GaN and Al{sub 2}O{sub 3}/N-GaN interfaces were both atomically sharp, and the latter further exhibited a biatomic step feature. The corresponding current-voltage (J-V) characteristics were measured on a metal-Al{sub 2}O{sub 3}-semiconductor capacitor (MOSCAP) structure. The leakage current was very high when the Al{sub 2}O{sub 3} thickness was comparable with the size of the crystalline defects, but was suppressed to the order of 1 × 10{sup −8} A/cm{sup 2} with larger Al{sub 2}O{sub 3} thicknesses. The interface states densities (D{sub it}) were measured on the same MOSCAPs by using combined ultraviolet (UV)-assisted capacitance-voltage (C-V), constant capacitance deep level transient spectroscopy (CC-DLTS), and constant capacitance deep level optical spectroscopy (CC-DLOS) techniques. The average D{sub it} measured by CC-DLTS and CC-DLOS were 6.6 × 10{sup 12} and 8.8 × 10{sup 12} cm{sup −2} eV{sup −1} for Al{sub 2}O{sub 3}/Ga-GaN and 8.6 × 10{sup 12} and 8.6 × 10{sup 12 }cm{sup −2} eV{sup −1} for Al{sub 2}O{sub 3}/N-GaN, respectively. The possible origins of the positive (negative) polarization compensation charges in Al{sub 2}O{sub 3}/Ga-GaN (Al{sub 2}O{sub 3}/N-GaN), including the filling of interface states and the existence of structure defects and impurities in the Al{sub 2}O{sub 3} layer, were discussed in accordance with the experimental results and relevant studies in the literature.

  10. Revisiting the blind tests in crystal structure prediction: accurate energy ranking of molecular crystals.

    Science.gov (United States)

    Asmadi, Aldi; Neumann, Marcus A; Kendrick, John; Girard, Pascale; Perrin, Marc-Antoine; Leusen, Frank J J

    2009-12-24

    In the 2007 blind test of crystal structure prediction hosted by the Cambridge Crystallographic Data Centre (CCDC), a hybrid DFT/MM method correctly ranked each of the four experimental structures as having the lowest lattice energy of all the crystal structures predicted for each molecule. The work presented here further validates this hybrid method by optimizing the crystal structures (experimental and submitted) of the first three CCDC blind tests held in 1999, 2001, and 2004. Except for the crystal structures of compound IX, all structures were reminimized and ranked according to their lattice energies. The hybrid method computes the lattice energy of a crystal structure as the sum of the DFT total energy and a van der Waals (dispersion) energy correction. Considering all four blind tests, the crystal structure with the lowest lattice energy corresponds to the experimentally observed structure for 12 out of 14 molecules. Moreover, good geometrical agreement is observed between the structures determined by the hybrid method and those measured experimentally. In comparison with the correct submissions made by the blind test participants, all hybrid optimized crystal structures (apart from compound II) have the smallest calculated root mean squared deviations from the experimentally observed structures. It is predicted that a new polymorph of compound V exists under pressure. PMID:19950907

  11. Protein structure search and local structure characterization

    Directory of Open Access Journals (Sweden)

    Ku Shih-Yen

    2008-08-01

    Full Text Available Abstract Background Structural similarities among proteins can provide valuable insight into their functional mechanisms and relationships. As the number of available three-dimensional (3D protein structures increases, a greater variety of studies can be conducted with increasing efficiency, among which is the design of protein structural alphabets. Structural alphabets allow us to characterize local structures of proteins and describe the global folding structure of a protein using a one-dimensional (1D sequence. Thus, 1D sequences can be used to identify structural similarities among proteins using standard sequence alignment tools such as BLAST or FASTA. Results We used self-organizing maps in combination with a minimum spanning tree algorithm to determine the optimum size of a structural alphabet and applied the k-means algorithm to group protein fragnts into clusters. The centroids of these clusters defined the structural alphabet. We also developed a flexible matrix training system to build a substitution matrix (TRISUM-169 for our alphabet. Based on FASTA and using TRISUM-169 as the substitution matrix, we developed the SA-FAST alignment tool. We compared the performance of SA-FAST with that of various search tools in database-scale search tasks and found that SA-FAST was highly competitive in all tests conducted. Further, we evaluated the performance of our structural alphabet in recognizing specific structural domains of EGF and EGF-like proteins. Our method successfully recovered more EGF sub-domains using our structural alphabet than when using other structural alphabets. SA-FAST can be found at http://140.113.166.178/safast/. Conclusion The goal of this project was two-fold. First, we wanted to introduce a modular design pipeline to those who have been working with structural alphabets. Secondly, we wanted to open the door to researchers who have done substantial work in biological sequences but have yet to enter the field of protein

  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. Characterization of ferroelectric single crystals with field induced phase transformations

    International Nuclear Information System (INIS)

    As new compositions of relaxor ferroelectric single crystals are developed, the full thermo-electro-mechanical behavior of each composition must be characterized to determine the linear coefficients as a function of stress, electric field and temperature, and the limitations on linear behavior imposed by field driven phase transformations. This characterization currently requires two crystal cuts, [001] and [110], each subjected to five electric field–electric displacement cycles at each of five different stress levels and five stress–strain cycles at each of five different electric field levels repeated at five temperatures. A new approach to characterizing the linear piezoelectric behavior and the nonlinear ferroelectric phase transformation behavior is proposed based on a combination of a work–energy based model of the driving forces for the phase transformation together with electric field loading while monitoring strain and electric displacement, and a measurement of mechanical compliance. The procedure for [110] single crystals is presented. [001] single crystals require a different approach due to the direction of loads driving the phase transformation. (paper)

  14. Growth and characterization of indium antimonide and gallium antimonide crystals

    Indian Academy of Sciences (India)

    N K Udayashankar; H L Bhat

    2001-10-01

    Indium antimonide and gallium antimonide were synthesized from the respective component elements using an indigenously fabricated synthesis unit. Bulk crystals of indium antimonide and gallium antimonide were grown using both the vertical and horizontal Bridgman techniques. Effect of ampoule shapes and diameters on the crystallinity and homogeneity was studied. The grown crystals were characterized using X-ray analysis, EDAX, chemical etching, Hall effect and conductivity measurements. In the case of gallium antimonide, effect of dopants (Te and In) on transport and photoluminescence properties was investigated.

  15. Characterization of single-crystal sapphire substrates by X-ray methods and atomic force microscopy

    International Nuclear Information System (INIS)

    The possibility of characterizing a number of practically important parameters of sapphire substrates by X-ray methods is substantiated. These parameters include wafer bending, traces of an incompletely removed damaged layer that formed as a result of mechanical treatment (scratches and marks), surface roughness, damaged layer thickness, and the specific features of the substrate real structure. The features of the real structure of single-crystal sapphire substrates were investigated by nondestructive methods of double-crystal X-ray diffraction and plane-wave X-ray topography. The surface relief of the substrates was investigated by atomic force microscopy and X-ray scattering. The use of supplementing analytical methods yields the most complete information about the structural inhomogeneities and state of crystal surface, which is extremely important for optimizing the technology of substrate preparation for epitaxy.

  16. Growth and characterization of single crystals for nuclear industry

    International Nuclear Information System (INIS)

    Single crystals are the key components of several instruments and devices that are being deployed in various applications in the nuclear industry. The applications range from gamma-ray background monitors using NaI(Tl) crystals to dosimeters using Li2B4O7:Cu for personal safety through more elaborate charge particle detection in the high energy physics experiments such as the Large Hadron Collider at the CERN that uses thousands of detectors based on single crystals of BGO, PbWO4 etc. In the present talk, growth and properties of several of the technologically important materials currently studied in our laboratory will be discussed. Some of these include Li6Gd(BO3)3, Li2B4O7, CsI(Tl), NaBi(WO4)2 etc. These crystals have been grown from their melts using Czochralski and Bridgman techniques. A novel technique based on the vacuum hot-pressing of nano-phase CaF2 leading to transparent ceramics will also be described. These ceramic materials show excellent thermo-luminescent properties for the dosimetry applications. Recently we observed an increase in the photoluminescence of Cu doped Li2B4O7 crystal when co-doped with Ag as Ag plays the role of a sensitizer. The growth of 20 mm diameter and 30 mm large crack-free Li6Gd(BO3)3 single crystals of undoped and 0.1% Ce will also be described. These crystals are grown along direction using the Czochralski technique. Grown crystals were characterized for their optical properties such as transmission and luminescence and results will be discussed in the talk. (author)

  17. Structural, thermal and optical studies on 2-naphthol crystals

    Energy Technology Data Exchange (ETDEWEB)

    Guru Prasad, L.; Shanmugam, G. [Department of Physics, Periyar University, Salem - 636 011 (India); Nagalakshmi, R. [Department of Physics, National Institute of Technology, Tiruchirappalli-620 015 (India); Krishnakumar, V.

    2010-10-15

    Single crystals of 2-naphthol was grown in slow evaporation solution growth technique. Grown crystals were characterized by various characterization techniques. Powder X- ray diffraction studies reveal that the grown crystal belongs to monoclinic system with noncentrosymmetric space group. Vibrational bands of the various functional groups and their significance were investigated by analyzing the vibrational spectra. Melting point and the decomposition temperature of the grown crystal was premeditated from the thermal analysis. From the UV-VIS-NIR spectrum the electronic excitation mechanism and the transmittance abilities of the crystal was studied. Theoretical value of first static hyperpolarizability was calculated and compared with urea. Second harmonic generation efficiency of the crystal is 0.6 times that of KDP. (copyright 2010 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  18. Crystal structure of the Al2CuIr phase

    International Nuclear Information System (INIS)

    A new ternary Al2CuIr phase was revealed in the Al-Cu-Ir system. It is formed below 1063 oC from the β-phase (CsCl-type structure) extending at elevated temperatures from AlIr. The crystal structure of the Al2CuIr 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: Rp = 4.45%, Rwp = 6.45%, RB = 3.69% and Rf = 2.41%.

  19. A new Salen-type azo-azomethine ligand and its Ni(II), Cu(II) and Zn(II) complexes: Synthesis, spectral characterization, crystal structure and photoluminescence studies.

    Science.gov (United States)

    Ozkan, Gozde; Kose, Muhammet; Zengin, Huseyin; McKee, Vickie; Kurtoglu, Mukerrem

    2015-11-01

    A novel Salen-type azo-azomethine ligand H2agen, 2,2'-{ethane-1,2-diylbis[nitrilomethylylidene]}bis{4-[ethylphenyldiazenyl]phenol}, formed by the 1:2M condensation of ethane-1,2-diamine with 5-[(4-ethylphenyl)diazenyl]-2-hydroxybenzaldehyde and its nickel(II), copper(II), and zinc(II) complexes were synthesized and characterized by the spectroscopic and analytical methods. The UV-vis spectra of the ligand were investigated in three organic solvents (DMSO, DMF and CHCl3). The ligand shows two absorption bands assigned to π-π(∗) and n-π(∗) transitions in the solvents used. Cu(II), and Ni(II) are tetra-coordinate binding to two phenolic oxygens and two imine nitrogens in approximate square planar geometry. Zn(II) also coordinates using the same sites like other metals but gave tetragonal configuration. Molecular structure of the Cu(II) complex [Cu(agen)] was determined by single crystal X-ray diffraction study. The X-ray data revealed that crystallographic imposed symmetry was absent for the complex molecule. In the structure, the Cu(II) ion is coordinated to two phenolate oxygen atoms and two imine nitrogen atoms of the azo-azomethine ligand with approximate square planar geometry. The ligand H2agen and its metal complexes exhibit strong blue emissions with irradiation. Fluorescence quantum yields and excited-state lifetimes for the ligand and its complexes were obtained. The H2agen ligand had a 35% quantum yield and a 3.27 ns excited-state lifetime. Complexation with metal ions caused reductions in intensities and quantum yields. PMID:26123514

  20. Crystal structures of five 6-mercaptopurine derivatives

    Science.gov (United States)

    Gomes, Lígia R.; Low, John Nicolson; Magalhães e Silva, Diogo; Cagide, Fernando; Borges, Fernanda

    2016-01-01

    The crystal structures of five 6-mercaptopurine derivatives, viz. 2-[(9-acetyl-9H-purin-6-yl)sulfan­yl]-1-(3-meth­oxy­phen­yl)ethan-1-one (1), C16H14N4O3S, 2-[(9-acetyl-9H-purin-6-yl)sulfan­yl]-1-(4-meth­oxy­phen­yl)ethan-1-one (2), C16H14N4O3S, 2-[(9-acetyl-9H-purin-6-yl)sulfan­yl]-1-(4-chloro­phen­yl)ethan-1-one (3), C15H11ClN4O2S, 2-[(9-acetyl-9H-purin-6-yl)sulfan­yl]-1-(4-bromo­phen­yl)ethan-1-one (4), C15H11BrN4O2S, and 1-(3-meth­oxy­phen­yl)-2-[(9H-purin-6-yl)sulfan­yl]ethan-1-one (5), C14H12N4O2S. Compounds (2), (3) and (4) are isomorphous and accordingly their mol­ecular and supra­molecular structures are similar. An analysis of the dihedral angles between the purine and exocyclic phenyl rings show that the mol­ecules of (1) and (5) are essentially planar but that in the case of the three isomorphous compounds (2), (3) and (4), these rings are twisted by a dihedral angle of approximately 38°. With the exception of (1) all mol­ecules are linked by weak C—H⋯O hydrogen bonds in their crystals. There is π–π stacking in all compounds. A Cambridge Structural Database search revealed the existence of 11 deposited compounds containing the 1-phenyl-2-sulfanyl­ethanone scaffold; of these, only eight have a cyclic ring as substituent, the majority of these being heterocycles. PMID:27006794

  1. Synthesis and Crystal Structure of Isosteviol Derivatives

    Institute of Scientific and Technical Information of China (English)

    Tao Jing-Chao; Tian Guo-Qiang; Zhang Yan-Bing; Wu Ya; Liu Hong-Min

    2004-01-01

    Isosteviol (ent-16-ketobeyeran-19-oic acid, I) is a tetracyclic diterpenoid with a beyerane skeleton obtained by acid hydrolysis of stevioside.1 Several tetracyclic diterpenoids, specially the kaurenes, have important biological activities. Recent studies on the microbial transformation of isosteviol have revealed that it is metabolized by Cunninghamella bainieri, Actinoplanes sp., Mucor recurvatus, and Cunninghamella blackesleeana to yield five new metabolites.2 The hydroxylation pattern of these bioactive compounds may influence their binding on to the receptors, as was proposed for the Rabdosia diterpenoids. Therefore, the introduction of hydroxyl groups or unsaturated bonds in saturated and non-hydroxylated diterpenoids, like isosteviol, may enhance existing properties or lead to new biological activities. Although some beyeranes have been subjected to biotransformations by fungi,4 there are few report in the literature related the chemical transformation of Isosteviol. In the present study, we try to develop the chemical transformation of isosteviol and other beyeranes in order to obtaining some bioactive compounds with beyerane skeleton. Seven isosteviol derivatives, Ⅱ-Ⅷ, were therefore synthesized and characterized. The X-ray crystal strcture of H(R = H) was also determined.

  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. 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

  4. 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.

    2015-01-01

    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. PMID:26423580

  5. Synthesis and characterization of a chiral dimeric copper(II) complex: Crystal structure of [Cu2(-Cl)2(HL)2].H2O(H2L = -(-)-2-[(2-hydroxy-1-phenyl-ethylimino)-methyl]-phenol)

    Indian Academy of Sciences (India)

    Chullikkattil P Pradeep; Panthapally S Zacharias; Samar K Das

    2005-03-01

    Synthesis and characterization of an optically active binuclear dichloro-bridged copper(II) complex [Cu2(-Cl)2(HL)2]$\\cdot$H2O 1 (H2L = -(-)-2-[(2-hydroxy-1-phenyl-ethylimino)-methyl]-phenol) of a Schiff-base derived from salicylaldehyde and ()-(+)-2-phenylglycinol are described. Compound 1 crystallizes in the orthorhombic chiral P212121 space group with = 4, = 10.21(2), = 11.574(3), = 25.364(9). Each copper shows square pyramidal geometry with O2NCl2 coordination and the Cu2Cl2 core geometry adopts a butterfly shape. Crystals of 1 were further characterized by elemental analysis, IR, UV-visible and EPR spectroscopy and circular dichroism (CD) studies.

  6. Characterization of ion Coulomb crystals for fundamental sciences

    Energy Technology Data Exchange (ETDEWEB)

    Okada, Kunihiro, E-mail: okada-k@sophia.ac.jp [Sophia University, Department of Physics (Japan); Ichikawa, Masanari [RIKEN Nishina Center for Accelerator-Based Science (Japan); Wada, Michiharu, E-mail: mw@riken.go.jp [Sophia University, Department of Physics (Japan)

    2015-11-15

    We performed classical molecular dynamics (MD) simulations in order to search the conditions for efficient sympathetic cooling of highly charged ions (HCIs) in a linear Paul trap. Small two-component ion Coulomb crystals consisting of laser-cooled ions and HCIs were characterized by the results of the MD simulations. We found that the spatial distribution is determined by not only the charge-to-mass ratio but also the space charge effect. Moreover, the simulation results suggest that the temperature of HCIs do not necessarily decrease with increasing the number of laser-cooled ions in the cases of linear ion crystals. We also determined the cooling limit of sympathetically cooled {sup 165}Ho{sup 14+} ions in small linear ion Coulomb crystals. The present results show that sub-milli-Kelvin temperatures of at least 10 Ho{sup 14+} ions will be achieved by sympathetic cooling with a single laser-cooled Be{sup +}.

  7. Undergraduates Improve upon Published Crystal Structure in Class Assignment

    Science.gov (United States)

    Horowitz, Scott; Koldewey, Philipp; Bardwell, James C.

    2014-01-01

    Recently, 57 undergraduate students at the University of Michigan were assigned the task of solving a crystal structure, given only the electron density map of a 1.3 Å crystal structure from the electron density server, and the position of the N-terminal amino acid. To test their knowledge of amino acid chemistry, the students were not given the…

  8. Single crystals of DPPH grown from diethyl ether and carbon disulfide solutions - Crystal structures, IR, EPR and magnetization studies

    OpenAIRE

    Zilic, Dijana; Pajic, Damir; Juric, Marijana; Molcanov, Kresimir; Rakvin, Boris; Planinic, Pavica; Zadro, Kreso

    2012-01-01

    Single crystals of the free radical 2,2-diphenyl-1-picrylhydrazyl (DPPH) obtained from diethyl ether (ether) and carbon disulfide (CS2) were characterized by the X-ray diffraction, IR, EPR and SQUID magnetization techniques. The X-ray structural analysis and IR spectra showed that the DPPH form crystallized from ether (DPPH1) is solvent free, whereas that one obtained from CS2 (DPPH2) is a solvate of the composition 4DPPH.CS2. Principal values of the g-tensor were estimated by the X-band EPR ...

  9. Macro-to-micro structural proteomics: native source proteins for high-throughput crystallization.

    Directory of Open Access Journals (Sweden)

    Monica Totir

    Full Text Available Structural biology and structural genomics projects routinely rely on recombinantly expressed proteins, but many proteins and complexes are difficult to obtain by this approach. We investigated native source proteins for high-throughput protein crystallography applications. The Escherichia coli proteome was fractionated, purified, crystallized, and structurally characterized. Macro-scale fermentation and fractionation were used to subdivide the soluble proteome into 408 unique fractions of which 295 fractions yielded crystals in microfluidic crystallization chips. Of the 295 crystals, 152 were selected for optimization, diffraction screening, and data collection. Twenty-three structures were determined, four of which were novel. This study demonstrates the utility of native source proteins for high-throughput crystallography.

  10. Origin of complex crystal structures of elements at pressure

    OpenAIRE

    Ackland, G. J.; Macleod, I. R.; Degtyareva, O

    2003-01-01

    We present a unifying theory for the observed complex structures of the sp-bonded elements under pressure based on nearly free electron picture (NFE). In the intermediate pressure regime the dominant contribution to crystal structure arises from Fermi-surface Brillouin zone (FSBZ) interactions - structures which allow this are favoured. This simple theory explains the observed crystal structures, transport properties, the evolution of internal and unit cell parameters with pressure. We illust...

  11. Calcium Oxalate Crystals in Eucalypt Ectomycorrhizae: Morphochemical Characterization

    OpenAIRE

    Pylro, Victor Satler; de Freitas, André Luiz Moreira; Otoni, Wagner Campos; da Silva, Ivo Ribeiro; Borges, Arnaldo Chaer; Costa, Maurício Dutra

    2013-01-01

    Ectomycorrhizal fungi are ubiquitous in forest ecosystems, benefitting plants principally by increasing the uptake of water and nutrients such as calcium from the soil. Previous work has demonstrated accumulation of crystallites in eucalypt ectomycorrhizas, but detailed morphological and chemical characterization of these crystals has not been performed. In this work, cross sections of acetic acid-treated and cleared ectomycorrhizal fragments were visualized by polarized light microscopy to e...

  12. Structural features of Ge(Ga) single crystals grown by the floating zone method in microgravity

    Science.gov (United States)

    Prokhorov, I. A.; Zakharov, B. G.; Senchenkov, A. S.; Egorov, A. V.; Camel, D.; Tison, P.

    2008-11-01

    Structural features of the Ge(Ga) single crystal grown by the floating zone (FZ) method in microgravity environment aboard the FOTON-9 spacecraft are investigated by methods of X-ray topography, double-crystal diffractometry, selective chemical etching and spreading resistance measurements. It is established that the crystal structure is characterized by the presence of an incompletely melted region and defects caused by its formation. Growth striations revealed in regrown part of the crystal, testify to development of non-stationary capillary Marangoni convection in melt at the realized parameters of FZ remelting under space conditions. Periodicity of the growth striations is compared to frequency characteristics of heat flux pulsations through the crystallization front, found as a result of numerical simulation of melt hydrodynamics.

  13. Crystal structure of triphenyl(vinylphosphonium tetraphenylborate

    Directory of Open Access Journals (Sweden)

    Joseph L. Bradfield

    2014-10-01

    Full Text Available The title ionic salt, C21H20P+·C24H20B−, crystallized with two independent vinyltriphenylphosphonium cations and two independent tetraphenylborate anions per asymmetric unit. These four independent moieties contain nearly perfect tetrahedral symmetry about their respective central C atoms. In the crystal, there are no π-stacking or other intermolecular interactions present.

  14. PLANAR OPTICAL WAVEGUIDES WITH PHOTONIC CRYSTAL STRUCTURE

    DEFF Research Database (Denmark)

    2003-01-01

    Planar optical waveguide comprising a core region and a cladding region comprising a photonic crystal material, said photonic crystal material having a lattice of column elements, wherein at least a number of said column elements are elongated substantially in an axial direction for said core...

  15. Nano-sized AlPO4-5 Crystals: Synthesis and characterization

    Directory of Open Access Journals (Sweden)

    A. Hassanvand

    2011-12-01

    Full Text Available Molecular sieves and zeolites are materials whose crystalline frameworks form nanometer or subnanometer pores. A variety of different crystal structures are known having a range of pore sizes. Because the pore sizes are usually smaller than 2 nm, they are classified as microporous materials. Synthesis of microporous materials is usually conducted by the high temperature treatment (80-200 °C of aqueous synthesis gels. The process of heating aqueous mixtures to elevated temperatures for crystallization is typically described as hydrothermal synthesis. A hydrothermal treatment has been used to synthesize nano-sized AlPO4-5 (AFI crystals. The treatment involved three main steps: (1 to prepare a synthesis gel and let it get well mixed, then filling autoclave with the gel and sealing it; (2 crystallization at 180 ◦C for 6 h; and (3 Calcination at 600 ◦C for 4 h to separate template materials. The crystals have been structurally characterized using X-ray diffraction (XRD, scanning electron microscope (SEM, energy dispersive X-ray analysis (EDAX. The analyses show an acceptable fitness to the referred pattern. The SEM analysis and Scherer equation revealed that the size of the obtained AlPO4-5 crystals was about 65 nm.

  16. Fabrication of FCC Structure Colloidal Photonic Crystals and Characteration of Band-Gap Measured%FCC结构胶体光子晶体的制备及其带隙特性测量

    Institute of Scientific and Technical Information of China (English)

    闫海涛; 王鸣; 葛益娴; 喻平; 刘青

    2009-01-01

    基于对光纤传输特性和胶体光子晶体制备方法的研究,提出了用外加电场控制的方法制备光子带隙位于通讯波段的FCC结构的胶体光子晶体,并用光纤系统测试胶体光子晶体的带隙特性.采用RSOFT模拟了胶体光子晶体的带隙,分析了带隙位于通讯波段时所需的胶体微球的基本参量(微球折射率和直径).采用自组装的方法,用步进电机控制玻璃基片向上的拉升速率.速率为5 μm/s,同时外加一电场.用扫描电镜观测胶体晶体的表面形貌,并设计了单模光纤系统测量胶体光子晶体的带隙特性.测试的透射谱线表明胶体光子晶体的带隙中心波长为1552 nm.测试结果和模拟结果具有很好的一致性,误差只有2 nm.%Based on the transmission characteration of optical fiber and the methods of fabrication colloidal photonic crystals, electric field-controlled method is used to fabricate colloidal photonic crystals with the photonic band-gap (PBG) in communications wavelength. RSOFT is used to simulate PBG characteration of colloidal photonic crystals and the parameters of colloidal microsphere are obtained. By the self-assembled method, the stepping motor is used to control the glass substrate, with the rate of 5 μm/s. At the same time an electric field is applied in the process of the colloidal crystals growth. The scanning electron microscopy is used to observe the surface of colloidal photonic crystals. An optical fiber system is designed to test PBG center wavelength of colloidal photonic crystals. Transmission spectrum shows the PBG of this colloidal crystals at 1552 nm. The agreement is very good between the experimental results and the simulation results, with the error of only 2 nm.

  17. Crystallization behavior and microstructural characterization of drug/polymer systems

    Science.gov (United States)

    Zhu, Qing

    Solid dispersions of the active pharmaceutical ingredient (API) in a polymeric matrix have received extensive attention as a potential approach to increase the dissolution rate of the API. Among different types of solid dispersions, polyethylene glycol (PEG) based semicrystalline solid dispersions have attracted considerable interest, for the reason that PEG enables the delivery of most APIs with low aqueous solubility. However, there are still limitations that restrict the application of this technique for drug formulations. One main concern is the reproducibility of the physicochemical properties of the solid dispersions during scale-up and storage. Additionally, the mechanism by which the dissolution rate is enhanced is still unclear. These are all related to the microstructure of the solid dispersions. Therefore, the purpose of this project is to have a fundamental understanding of the crystallization behavior and microstructural evolution of API/PEG solid dispersions. The model API was comelted with PEG and solidified at predetermined temperatures. The effect of the physicochemical properties of the APIs, polymer matrix and preparation conditions on the crystallization behavior and structure were investigated, using wide-angle X-ray scattering, small-angle X-ray scattering, scanning electron microscopy, atomic force microscopy and second harmonic imaging microscopy. When API/PEG solid dispersions were formed using different APIs, it was found that, for the fast crystallizing APIs (e.g. naproxen), the interaction between the API and the PEG matrix slowed down the crystallization rate of naproxen. For the slow crystallizing APIs (e.g. ibuprofen), crystalline PEG acted as heterogeneous nuclei to speed up the onset of crystallization. It was also found that, APIs with strong interaction in PEG (e.g. Naproxen/PEG) favored the interlamellar incorporation of naproxen in PEG matrix before naproxen crystallized. When the naproxen/PEG solid dispersions are prepared at

  18. Structural variety in zinc telluro-phosphates: syntheses, crystal structures and characterizations of Sr2Zn3Te2P2O14, Pb2Zn3Te2P2O14 and Ba2Zn2TeP2O11.

    Science.gov (United States)

    Xia, Mingjun; Li, R K

    2016-05-01

    Three new zinc telluro-phosphates, Sr2Zn3Te2P2O14 (1), Pb2Zn3Te2P2O14 (2) and Ba2Zn2TeP2O11 (3), were grown by flux method, and their crystal structures were solved by X-ray diffraction method. Although all three crystals crystallize into the same space group P21/c with similar chemical compositions, they exhibit different topology structure types. 1 features a two-dimensional layered structure with the connection of TeO4 and (Zn3TeP2O18)(16-) 12-membered rings (MRs), which are composed of planar square and tetrahedral configuration ZnO4 groups, tetrahedral PO4 and seesaw TeO4. Due to lone-pair Coulomb repulsion of Pb(2+), the structure of 2, which is also composed of unbalanced seesaw TeO4 and ZnO4 groups and distorted PO4 tetrahedra, is slightly different from that of its analog 1. Compound 3 exhibits a complicated three-dimensional network with (Zn2PO9)(9-) 6-MRs and (Zn2Te2O10)(8-) 8-MRs built from distorted tetrahedral ZnO4 and PO4 groups and trigonal pyramidal TeO3 units. According to UV-vis-NIR diffuse reflectance spectra, compounds 1, 2 and 3 are highly transparent in the range of 450 to 2500 nm with a UV cut-off of 275 nm, 330 nm and 278 nm, respectively. In addition, the characterizations, including thermal analyses, XPS measurement and dipole moment calculations, are also reported. PMID:27046132

  19. 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.

  20. Prediction of new crystal structures under extreme conditions

    OpenAIRE

    Schärf, Daniel

    2014-01-01

    One of the most important challenges in chemistry and material science is the connection between the contents of a compound and its chemical and physical properties. In solids, these are greatly influenced by the crystal structure.rnrnThe prediction of hitherto unknown crystal structures with regard to external conditions like pressure and temperature is therefore one of the most important goals to achieve in theoretical chemistry. The stable structure of a compound is the global minimum of t...

  1. Synthesis, spectral characterization, and crystal structure of mononuclear mercury(II) complex [Hg((3,4-MeO-Bza).sub.2./sub.En)I.sub.2./sub.

    Czech Academy of Sciences Publication Activity Database

    Khalaji, A.D.; Grivan, G.; Rezaei, M.; Fejfarová, Karla; Dušek, Michal

    2013-01-01

    Roč. 39, č. 1 (2013), s. 104-108. ISSN 1070-3284 R&D Projects: GA ČR(CZ) GAP204/11/0809 Grant ostatní: AVČR(CZ) Praemium Academiae Institutional research plan: CEZ:AV0Z10100521 Keywords : mercury (II) * Schiff base * single crystal * structure analysis Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 0.629, year: 2013

  2. Functional substitution of coordination polyhedron in crystal structure of silicates

    Institute of Scientific and Technical Information of China (English)

    叶大年; 马哲生; 赫伟; 李哲; 施倪承; D.Pushcharovsky

    2002-01-01

    On the bases of the study of comparative crystal chemistry of silicates it has been concluded that the octahedra and square pyramids of Ti-0 and Zr-O play functional role of tetrahedra of Si-O in the construction of crystal structures. Therefore, those silicates may be named titano-and zircono-silicates. Because of the functional similarity of coordination polyhedra, the structures of cristobalite and feldspar have been compared with those of perovskite and garnet, respectively. As a new concept, the functional replacement of tetrahedra by octahedra and/or pyramids is defined by the authors of this paper for favorable comparison of relative crystal structures.

  3. Synthesis and peculiarities of the cesium zeolite crystal structure (cesite)

    International Nuclear Information System (INIS)

    An attempt is made to synthesize cesium zeolite by introduction of amorphous seed crystals which correspond by composition with cesium-containing zeolite into the aluminosilicate gel, since this method can produce zeolite with a crystal structure it would not adopt under the usual conditions. It is seen that during crystablization upon introduction of a seed crystal the cesium content in zeolite decreases. A more complete structural elucidation of zeolite obtained by the suggested method was carried out by x0ray and IR spectral analyses. The data of x-ray analysis showed that the structures of synthesized zeolite and binary octagonal pores are similar

  4. Structural, spectral and mechanical studies of bimetallic crystal: cadmium manganese thiocyanate single crystals

    Science.gov (United States)

    Manikandan, M.; Vijaya Prasath, G.; Bhagavannarayan, G.; Vijayan, N.; Mahalingam, T.; Ravi, G.

    2012-09-01

    A nonlinear optical bimetallic thiocyanate complex crystal, cadmium manganese thiocyanate (CMTC) has been successfully synthesized. The growth of single crystals of cadmium manganese thiocyanate has been accomplished from aqueous solution using slow evaporation method. The presence of manganese and cadmium in the synthesized material was confirmed through energy dispersive spectrum (EDS) analysis. Structural analysis was carried out using powder X-ray diffractometer (PXRD) and crystalline perfection of the grown crystals was ascertained by high-resolution X-ray diffraction (HRXRD) analysis. Fourier transform infrared (FTIR) spectrum was taken to confirm the functional groups. The transmittance spectrum of the crystal in the UV-visible region has been recorded and the cutoff wavelength has been determined. The dielectric measurements for the crystals were performed for various frequencies and temperatures. The mechanical properties were evaluated by Vickers microhardness testing, which reveals hardness and stiffness constant of the crystals.

  5. Structural, spectral and mechanical studies of bimetallic crystal: cadmium manganese thiocyanate single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Manikandan, M.; Vijaya Prasath, G.; Mahalingam, T.; Ravi, G. [Alagappa University, Department of Physics, Karaikudi (India); Bhagavannarayan, G.; Vijayan, N. [National Physical Laboratory, Materials Characterization Division, New Delhi (India)

    2012-09-15

    A nonlinear optical bimetallic thiocyanate complex crystal, cadmium manganese thiocyanate (CMTC) has been successfully synthesized. The growth of single crystals of cadmium manganese thiocyanate has been accomplished from aqueous solution using slow evaporation method. The presence of manganese and cadmium in the synthesized material was confirmed through energy dispersive spectrum (EDS) analysis. Structural analysis was carried out using powder X-ray diffractometer (PXRD) and crystalline perfection of the grown crystals was ascertained by high-resolution X-ray diffraction (HRXRD) analysis. Fourier transform infrared (FTIR) spectrum was taken to confirm the functional groups. The transmittance spectrum of the crystal in the UV-visible region has been recorded and the cutoff wavelength has been determined. The dielectric measurements for the crystals were performed for various frequencies and temperatures. The mechanical properties were evaluated by Vickers microhardness testing, which reveals hardness and stiffness constant of the crystals. (orig.)

  6. A SAPO-11 Silicoaluminophosphate Molecular Sieve with Stable Crystal Structure

    Institute of Scientific and Technical Information of China (English)

    Yue Ming LIU; Feng Mei ZHANG; Hai Hong WU; Hai Jiao ZHANG; Jian Guo YANG; Xing Tian SHU; Ming Yuan HE

    2004-01-01

    A SAPO-11 silicoaluminophosphate molecular sieve with stable crystal structure was synthesized for the first time. After removing template by calcination, its crystal space group still retains Icm2 which the as-synthesized has. The catalyst deriving from the present SAPO-11materials shows higher isomerization selectivity and higher paraffin hydroisomerization yield than those reported elsewhere.

  7. Crystal structure of homoisocitrate dehydrogenase from Schizosaccharomyces pombe

    Energy Technology Data Exchange (ETDEWEB)

    Bulfer, Stacie L.; Hendershot, Jenna M.; Trievel, Raymond C. (Michigan); (UCSF)

    2013-09-18

    Lysine biosynthesis in fungi, euglena, and certain archaebacteria occurs through the {alpha}-aminoadipate pathway. Enzymes in the first steps of this pathway have been proposed as potential targets for the development of antifungal therapies, as they are absent in animals but are conserved in several pathogenic fungi species, including Candida, Cryptococcus, and Aspergillus. One potential antifungal target in the {alpha}-aminoadipate pathway is the third enzyme in the pathway, homoisocitrate dehydrogenase (HICDH), which catalyzes the divalent metal-dependent conversion of homoisocitrate to 2-oxoadipate (2-OA) using nicotinamide adenine dinucleotide (NAD{sup +}) as a cofactor. HICDH belogns to a family of {beta}-hydroxyacid oxidative decarboxylases that includes malate dehydrogenase, tartrate dehydrogenase, 6-phosphogluconate dehydrogenase, isocitrate dehydrogenase (ICDH), and 3-isopropylmalte dehydrogenase (IPMDH). ICDH and IPMDH are well-characterized enzymes that catalyze the decarboxylation of isocitrate to yield 2-oxoglutarate (2-OG) in the citric acid cycle and the conversion of 3-isopropylmalate to 2-oxoisovalerate in the leucine biosynthetic pathway, respectively. Recent structural and biochemical studies of HICDH reveal that this enzyme shares sequence, structural, and mechanistic homology with ICDH and IPMDH. To date, the only published structures of HICDH are from the archaebacteria Thermus thermophilus (TtHICDH). Fungal HICDHs diverge from TtHICDH in several aspects, including their thermal stability, oligomerization state, and substrate specificity, thus warranting further characterization. To gain insights into these differences, they determined crystal structures of a fungal Schizosaccharomyces pombe HICDH (SpHICDH) as an apoenzyme and as a binary complex with additive tripeptide glycyl-glycyl-glycine (GGG) to 1.55 {angstrom} and 1.85 {angstrom} resolution, respectively. Finally, a comparison of the SpHICDH and TtHICDH structures reveal differences in

  8. Crystal Structure of 7,3'-Dihydroxy-4'-methoxyisoflavone

    Institute of Scientific and Technical Information of China (English)

    丁兰; 王明盛; 郭国聪; 汪汉卿

    2004-01-01

    The title compound 7,3'-dihydroxy-4'-methoxyisoflavone isolated from the stems of Eremosparton songoricum was characterized by IR,1H-NMR,13C-NMR,H1-H1COSY,HMQC,HMBC and EIMS,and its crystal structure was determined by single-crystal X-ray diffraction with the following data: C16H12O5,monoclinic,P21/c,Z = 4,a = 9.926(8),b = 17.091(5),c = 8.001(4)A ',β = 99.07(3)A,V = 1340(1)A3,Mr = 284.26,Dc = 1.409 g/cm3,F(000) = 592,μ = 0.106 mm-1,R = 0.065 and Wr = 0.1337 for 2084 observed reflections (I > 2.0б(I)).The molecular backbone of the compound includes a benzopyrone and a phenyl ring,and the dihedral angle between them is 50.21o.The molecules form extensive networks through the intra-and intermolecular hydrogen bonds.

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

    International Nuclear Information System (INIS)

    By means of X-ray structure analysis, the crystal structure of neodymium gallium perovskite (NGP) single crystals (NdGaO3) being used as a substrate for HTSC film epitaxy has been refined and the position of atoms has been determined. The possibility of YBa2Cu3O7-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 LaGaO3 and LaAlO3 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)

  10. Structural and mechanical studies of cadmium manganese thiocyanate crystal

    Science.gov (United States)

    Manikandan, M. R.; Vijayaprasath, G.; babu, G. Anandha; Bhagavannarayan, G.; Vijayan, N.; Ravi, G.

    2012-06-01

    Single crystals of cadmium manganese thiocyanate (CMTC) have been synthesized successfully and grown by slow evaporation method. The structural perfection of the grown crystals has been analyzed by High resolution X-ray diffraction (HRXRD), which shows the crystalline perfection of the grown crystal is quite good. Optical behavior was assessed by UV-Vis analysis and found that no absorption in the UV visible region and it may be useful for second harmonic applications. The mechanical hardness of the grown crystals was studied and Vicker's microhardness, Stiffness constant was calculated.

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

    International Nuclear Information System (INIS)

    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 C11, C12 and C44 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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Y.W.; Li, S.J.; Obbard, E.G.; Wang, H.; Wang, S.C. [Shenyang National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, 72 Wenhua Road, Shenyang 110016 (China); Hao, Y.L., E-mail: ylhao@imr.ac.cn [Shenyang National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, 72 Wenhua Road, Shenyang 110016 (China); Yang, R. [Shenyang National Laboratory for Materials Science, Institute of Metal Research, Chinese Academy of Sciences, 72 Wenhua Road, Shenyang 110016 (China)

    2011-05-15

    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 < 1 1 0> crystal shows significant elastic asymmetry in tension and compression. > The <1 0 0> crystal exhibits weak nonlinear elasticity with large elastic strain {approx}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 <1 0 0>, <1 1 0> and <1 1 1> oriented single crystals, and C{sub 11}, C{sub 12} and C{sub 44} of 57.2, 36.1 and 35.9 GPa respectively. Uniaxial testing revealed asymmetrical elastic behaviors of the <1 1 0> crystals: tension caused elastic softening with a large reversible strain of {approx}4% and a stress plateau of {approx}250 MPa, whereas compression resulted in gradual elastic stiffening with much smaller reversible strain. The <1 0 0> crystals exhibited weak nonlinear elasticity with a large elastic strain of {approx}2.5% and a high strength, approaching {approx}20% and {approx}30% of its ideal shear and ideal tensile strength respectively. The <1 1 1> crystals showed linear elasticity with a small elastic strain of {approx}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.

  13. Preparation, Crystal Structure, and Thermal Analysis of Carbohydrazide Trinitrophloroglucinolate

    Institute of Scientific and Technical Information of China (English)

    LIU Zhen-hua; ZHANG Tong-lai; HU Xiao-chun; ZHANG Jian-guo; YANG Li; QIAO Xiao-jing

    2008-01-01

    A new compound (CHZ)(HTNPG).0.5H2O was synthesized by mixing carbohydrazide(CHZ) and trinitrophloroglucinol(TNPG) and characterized by elemental analysis and Fourier transform infrared (FTIR) spectrum.Its crystal structure was determined by single crystal X-ray diffraction analysis.The crystal belongs to triclinic system,P1 space group,with a=0.45578(9) nm,b=1.0142(2) nm,c=1.3041(3) nm,a=86.53(3)°,β=99.56(3)°,γ=81.94(3)°,V=0.5958(2) nm3,Z=2,Dc=2.008 g/cm3,R1=0.0476,and wR2=O.1139.The compound is a di-substituted salt of TNPG,which consists of a cation (CHZ)2+ and an anion (HTNPG)2-.The thermal analysis of the compound was studied by means of differential scanning calorimetry(DSC) and thermogravimetry-derivative thermogravimetry(TG-DTG).Under nitrogen atmosphere at a heating rate of 10 ℃/min,the thermal decomposition of the compound contained one endothermic process of dehydrating stage and two intense exothermic decomposition processes in a temperature range of 140--232℃ on the DSC trace.The decomposition products of the title compound are nearly gaseous products.The existing complicated hydrogen bond networks and electrostatic attraction between (CHZ)2+ and (HTNPG)2-enhance the thermal stability of the title compound.

  14. Synthesis, Crystal Structure, and DFT Study of N′-(2,4-Dinitrophenyl-2-Fluorobenzohydrazide

    Directory of Open Access Journals (Sweden)

    Aamer Saeed

    2013-01-01

    Full Text Available A new hydrazide derivative N′-(2,4-dinitrophenyl-2-fluorobenzohydrazide was synthesized and characterized by NMR and IR spectroscopy. The molecular structure was also studied by X-ray diffraction, and the results of the optimized molecular structure are presented and compared with density functional methods with 631-G basis set. The calculated results show that the optimized geometry can well reproduce the crystal structural parameters, for example, bond lengths and angles show good agreement with the experimental data.

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

    International Nuclear Information System (INIS)

    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

  16. Acquisition of Single Crystal Growth and Characterization Equipment

    Energy Technology Data Exchange (ETDEWEB)

    Maple, M. Brian; Zocco, Diego A.

    2008-12-09

    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

  17. Structure of crystallized layers by laser annealing of (100) and (111) self-implanted silicon samples

    International Nuclear Information System (INIS)

    Channeling effect techniques with a 2.0 MeV He+ Rutherford backscattering and transmission electron microscopy were used to characterize the crystallized layers after Q-switched ruby laser irradiation of 4,000 Angstroem thick amorphous layer on (100) and (111) underlined crystal substrates. At a laser energy density of 2.5 J/cm2 the crystal layer on the (111) specimen contains a large density of stacking-faults, that on (100) specimen contains a very small amount of screw dislocation lines. High quality single-crystal layers have been obtained after irradiation at 3.5 J/cm2. From a comparison with the growth rate and defect structure observed in thermally annealed implanted-amorphous layers, we propose that crystal growth by 50 ns pulse laser annealing occurs by melting the amorphous layer. (orig.)

  18. Synthesis, growth, structure determination and optical properties of chalcone derivative single crystal

    Science.gov (United States)

    Karthi, S.; Girija, E. K.

    2014-04-01

    Acquiring large nonlinear optical (NLO) efficient organic material is essential for the development of optoelectronics and photonic devices. Chalcone is the donor - Π - acceptor - Π - donor (D-Π-A-Π-D) type conjugated molecule with appreciable hyperpolarizability of potential interest in NLO applications. The addition of vinyl and electron donor groups in the chalcone molecule may enhance the second harmonic generation (SHG) efficiency. Here we report the synthesis, crystal growth and characterization of a chalcone derivative 1-(4-methylphenyl)-5-(4-methoxyphenyl)-penta-2,4-dien-1-one (MPMPP). The MPMPP crystal was grown by slow evaporation solution growth technique from acetone. The grown crystal structure was studied by single crystal X-ray diffraction. The SHG efficiency of the grown crystal was determined by Kurtz and Perry method.

  19. Synthesis, growth, structure determination and optical properties of chalcone derivative single crystal

    Energy Technology Data Exchange (ETDEWEB)

    Karthi, S., E-mail: girijaeaswaradas@gmail.com; Girija, E. K., E-mail: girijaeaswaradas@gmail.com [Department of Physics, Periyar University, Salem - 636011 (India)

    2014-04-24

    Acquiring large nonlinear optical (NLO) efficient organic material is essential for the development of optoelectronics and photonic devices. Chalcone is the donor - Π - acceptor - Π - donor (D-Π-A-Π-D) type conjugated molecule with appreciable hyperpolarizability of potential interest in NLO applications. The addition of vinyl and electron donor groups in the chalcone molecule may enhance the second harmonic generation (SHG) efficiency. Here we report the synthesis, crystal growth and characterization of a chalcone derivative 1-(4-methylphenyl)-5-(4-methoxyphenyl)-penta-2,4-dien-1-one (MPMPP). The MPMPP crystal was grown by slow evaporation solution growth technique from acetone. The grown crystal structure was studied by single crystal X-ray diffraction. The SHG efficiency of the grown crystal was determined by Kurtz and Perry method.

  20. 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)

    Two rare-earth compounds containing selenium atoms, La(HSeO3)(SeO4) with a new open framework structure and KNd(SeO4)2 with a layered structure, have been synthesized under ''sol-gel'' hydrothermal conditions for the first time. Single-crystals of La(HSeO3)(SeO4) crystallize in the monoclinic system (P21, 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 LaOx (x=9,10) and SeO4 groups, which are connected via SeO3-uints to the 3D structure. The crytal structure of KNd(SeO4)2 (monoclinc, P21/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 NdO9 polyhedra forming layers which are further decorated with SeO4 tetrahedra. The K+ ions occupy the interspaces of these layers and provide the charge balance

  1. Growth and characterization of the nonlinear optical single crystal: L-lysine acetate

    Science.gov (United States)

    Sun, Z. H.; Zhang, G. H.; Wang, X. Q.; Cheng, X. F.; Liu, X. J.; Zhu, L. Y.; Fan, H. L.; Yu, G.; Xu, D.

    2008-05-01

    Single crystals of L-lysine acetate, an organic nonlinear optical (NLO) material, were grown by the controlled evaporation of its aqueous solutions. Its solubility in aqueous solution was determined gravimetrically. The grown crystals were characterized by the single-crystal diffraction, X-ray powder diffraction, Fourier transform infrared and Raman spectra. The structure analysis reveals that it belongs to the monoclinic crystallographic system, space group P2 1, with cell parameters: a=5.420(2) Å, b=7.542(4) Å, c=12.653(1) Å, β=91.73(1)°, Z=2 and V=516.8 Å 3. Experiments of thermogravimetric (TG) and differential thermal analysis (DTA) were carried out to study its thermal properties. The optical behaviours, including transmission spectrum and second harmonic generation (SHG), were investigated to study its linear and NLO properties.

  2. Improving nanocavity switching using Fano resonances in photonic crystal structures

    DEFF Research Database (Denmark)

    Heuck, Mikkel; Kristensen, Philip Trøst; Elesin, Yuriy;

    2013-01-01

    We present a simple design for achieving Fano resonances in photonic crystal coupled waveguide-cavity structures. A coupled mode theory analysis shows an order of magnitude reduction in switching energy compared to conventional Lorentz resonances....

  3. Molecular and Crystal Structures of Three Berberine Derivatives

    OpenAIRE

    Jiří Dostál; Zdirad Žák; Marek NeÄÂas; Milan PotáÄÂek; Stanislav Man

    2001-01-01

    Berberine azide, berberine thiocyanate, and 8-cyano-8H-berberine were prepared from berberine chloride, a quaternary protoberberine alkaloid. The molecular and crystal structures of all compounds are reported and discussed.

  4. Molecular and Crystal Structures of Three Berberine Derivatives

    Directory of Open Access Journals (Sweden)

    Jiří Dostál

    2001-04-01

    Full Text Available Berberine azide, berberine thiocyanate, and 8-cyano-8H-berberine were prepared from berberine chloride, a quaternary protoberberine alkaloid. The molecular and crystal structures of all compounds are reported and discussed.

  5. Crystal Structure, Electron Spin Resonance, and Magnetic Exchange Coupling in Bis(μ-chloro)bis[cyclopentadienyl(triethylphosphane)vanadium(II)

    NARCIS (Netherlands)

    Nieman, J.; Teuben, J.H.; Hulsbergen, F.B.; Graaff, R.A.G. de; Reedijk, J.

    1987-01-01

    The X-ray structure and magnetic characterization (ESR, susceptibility) of the dinuclear vanadium(II) compound [CpVCl(PEt3)]2 are described. The title compound crystallizes in the monoclinic space group as purple-red crystals, with cell dimensions of a = 12.760 (5) Å, b = 12.616 (7) Å, c = 17.707 (7

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

    International Nuclear Information System (INIS)

    Colorless crystals of ThSiO4 (huttonite) (1) and (Ca0.5Na0.5)2NaThSi8O20 (2) have been synthesized by the solid-state reactions of ThO2, CaSiO3, and Na2WO4 at 1073 K. Green crystals of (Ca0.5Na0.5)2NaUSi8O20 (3) have been synthesized by the solid-state reactions of UO2, CaSiO3, and Na2WO4 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 ThO9 polyhedra and SiO4 tetrahedra. Compounds 2 and 3 are isostructural and they crystallize in a steacyite-type structure. The structure consists of discrete pseudocubic [Si8O20]8− polyanions, which are connected by An4+ cations into a three-dimensional framework. Each An atom coordinates to eight monodentate [Si8O20]8− moieties in a square antiprismatic geometry. Na+ and Ca2+ 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 (Ca0.5Na0.5)2NaAnSi8O20 (An=Th, U), which contain pseudocubic [Si8O20]8− polyanions and eight-coordinate An4+ cations. - Highlights: • Single crystal growth of three tetravalent actinide silicates from melts. • Single-crystal structures and Raman spectra of (Ca0.5Na0.5)2NaAnSi8O20 (An=Th, U). • First report of Raman spectrum of huttonite on single crystal samples

  7. Allophycocyanin and phycocyanin crystal structures reveal facets of phycobilisome assembly.

    Science.gov (United States)

    Marx, Ailie; Adir, Noam

    2013-03-01

    X-ray crystal structures of the isolated phycobiliprotein components of the phycobilisome have provided high resolution details to the description of this light harvesting complex at different levels of complexity and detail. The linker-independent assembly of trimers into hexamers in crystal lattices of previously determined structures has been observed in almost all of the phycocyanin (PC) and allophycocyanin (APC) structures available in the Protein Data Bank. In this paper we describe the X-ray crystal structures of PC and APC from Synechococcus elongatus sp. PCC 7942, PC from Synechocystis sp. PCC 6803 and PC from Thermosynechococcus vulcanus crystallized in the presence of urea. All five structures are highly similar to other PC and APC structures on the levels of subunits, monomers and trimers. The Synechococcus APC forms a unique loose hexamer that may show the structural requirements for core assembly and rod attachment. While the Synechococcus PC assembles into the canonical hexamer, it does not further assemble into rods. Unlike most PC structures, the Synechocystis PC fails to form hexamers. Addition of low concentrations of urea to T. vulcanus PC inhibits this proteins propensity to form hexamers, resulting in a crystal lattice composed of trimers. The molecular source of these differences in assembly and their relevance to the phycobilisome structure is discussed. PMID:23201474

  8. Synthesis and Crystal Structure of Tetra(o-cyanobenzyl)tin

    Institute of Scientific and Technical Information of China (English)

    KUANG Dai-Zhi; JIANG Jiang-Ping; FENG Yong-Lan; ZHANG Fu-Xing; WANG Jian-Qiu; LUO Yi-Ming

    2008-01-01

    The tetra(o-eyanobenzyl)tin compound has been synthesized by the reaction of eyanobenzyl chloride with tin, and its molecular structure was characterized by elemental analysis,IR spectra, 1H NMR and X-ray diffraction. Crystal data for this compound: monoclinie, space group C2/c, M, = 583.24, a = 1.9629(2), b = 1.05967(13), c = 1.41249(18) nm, β = 118.180(2)°, V =2.5898(5) nm3, Z = 4, Dc =1.496 g/cm3, μ(MoKa) = 1.015 cm-1, F(000) = 1176, R = 0.0189, wR =0.0497 (observed reflections with Ⅰ 2σ(Ⅰ)) and R = 0.0218, wR = 0.0513 (all reflections).The molecular structure adopts a distorted tetrahedral geometry around the tin atom. The Sn…N weak interaction between the Sn and N atoms of cyano forms an intermolecular H-bonding, and the bond length is 0.3570 nm; the interaction between hydrogen of methylene and benzene ring of benzyl forms C-H…C with its bond length of 0.2817 nm; and the interaction among hydrogen of benzene ring and carbon of cyano forms Ph-H…C bond (0.2897 nm) of the σ…π interaction. A 3D chain structure is formed by the above weak intermolecular interactions.

  9. Synthesis and characterization of aluminum and gallium complexes of heterocyclic thiosemicarbazones. crystal structures of Me2M[SC4H3CHNNC(S)SCH3] (M=Al, Ga)

    International Nuclear Information System (INIS)

    The synthesis and characterization of the monomeric group 13 heterocyclic thiosemicarbazone complexes Me2M[SC4H3CHNNC(S)SCH3] (M=Al (2), Ga (3)) are described. Compounds 2-3 were prepared using MMe3 (M=Al, Ga) in toluene with 2-thiophenecarboxaldehyde-S-methyldithiocarbazate under anaerobic conditions. These complexes have been characterized by 1H NMR, 13C NMR, elemental analyses, and single-crystal X-ray diffraction. 2 crystallizes in the monoclinic space group P21/c with unit cell parameters a=10.2930(5) A, b=18.564 (1) A, c=7.3812(6) A, V=1347.9(2) A3, Dcalc=1.342 gcm-3 for Z=4, 9281 reflections with Ibca with unit cell parameters a=13.340(3) A, b=19.9070(5) A, c=11.3690(2) A, V=2673.88(9) A3, Dcalc=1.511 gcm-3 for Z=8, 17004 reflections with I>3σ(I), R1=0.0480 and wR2=0.0524. Compound 3 is a monomeric gallium compound with a weak interaction between the pendant thiophene and the gallium center

  10. Synthesis and characterization of aluminum and gallium complexes of heterocyclic thiosemicarbazones. crystal structures of Me{sub 2}M[SC{sub 4}H{sub 3}CHNNC(S)SCH{sub 3}] (M=Al, Ga)

    Energy Technology Data Exchange (ETDEWEB)

    Kang, Young Jin; Yoo, Byung Woo; Kang, Sang Ook; Ko, Jae Jung [Korea Univ., Chochiwon (Korea, Republic of); Kang, Seung Joo [Korea National University of Education, Chongwon (Korea, Republic of)

    1998-01-01

    The synthesis and characterization of the monomeric group 13 heterocyclic thiosemicarbazone complexes Me{sub 2}M[SC{sub 4}H{sub 3}CHNNC(S)SCH{sub 3}] (M=Al (2), Ga (3)) are described. Compounds 2-3 were prepared using MMe{sub 3} (M=Al, Ga) in toluene with 2-thiophenecarboxaldehyde-S-methyldithiocarbazate under anaerobic conditions. These complexes have been characterized by {sup 1}H NMR, {sup 13}C NMR, elemental analyses, and single-crystal X-ray diffraction. 2 crystallizes in the monoclinic space group P2{sub 1}/c with unit cell parameters a=10.2930(5) A, b=18.564 (1) A, c=7.3812(6) A, V=1347.9(2) A{sup 3}, D{sub calc}=1.342 gcm{sup -3} for Z=4, 9281 reflections with I<3{sigma} (I), R1=0.0500 and wR2=0.0526. 3 crystallizes in the orthorhombic space group P{sub bca} with unit cell parameters a=13.340(3) A, b=19.9070(5) A, c=11.3690(2) A, V=2673.88(9) A{sup 3}, D{sub calc}=1.511 gcm{sup -3} for Z=8, 17004 reflections with I>3{sigma}(I), R1=0.0480 and wR2=0.0524. Compound 3 is a monomeric gallium compound with a weak interaction between the pendant thiophene and the gallium center.

  11. Structural inhomogeneities in crystals of YBa2Cu3O7-δ

    International Nuclear Information System (INIS)

    Structural inhomogeneities in crystals of YBa2Cu3O7-δ are characterized using high resolution x-ray diffraction. Rocking curves and a high resolution specular radial scan show features indicating that the crystals are not truly single. The high resolution radial scan of a crystal that had a superconducting transition width of only one-half Kelvin, as determined by ac susceptibility, and appeared to be free of gross defects, when examined with conventional x-ray diffraction techniques, shows a distribution in the c-axis lattice parameter. These results suggest that crystals with sharp transitions should be carefully examined for the presence of structural anomalies which might influence the superconductive properties

  12. Synthesis and Properties of Triphenylgermanium Heteroaromatic Carboxylates and Crystal Structure of Triphenylgermanium 2-Furoate

    Institute of Scientific and Technical Information of China (English)

    YIN,Han-Dong(尹汉东); WANG,Chuan-Hua(王传华); WANG,Yong(王勇); ZHANG,Ru-Fen(张如芬); MA,Chun-Lin(马春林); TAO,Xu-Quan(陶绪全)

    2001-01-01

    Ten triphenylgermaanium heteroaromatic carboxylates Ph3GeO2CR ( where R = 2-furanyl, 2-furanvinyl, 2-(5-tert-butyl) furonyl, 2-thiophenyl, 2-pyridinyl, 3-pyridinyl, 4-pyridinyl, 3-indolyl, 3-indolyhnethyl, 3-indolylpropyl) were synthesized by the reaction of sodium heteroaromatic carboxylates with the triphenylgermanium chloride. All compounds were characterized by elemental analysis, 1H NMR and MS spectra. The empounds were tested against two human tumour cell lines: MCF-7 and WiDr. The results showed that they had high activities. The crystal structure of triphenyler-mananium 2-furoate was determined by X-ray single crystal diffration. The crystal belongs to monoclinic with space grop P 21/c, a=1.1945(4), t=0.9934(3), c=1.6284(5)nm, β=91.59(5), Z=4. In this crystal, the structure consists of discrete molecule containing four-cnordinate germanimm atom in a distored tetrahedron.

  13. Crystallization and X-ray structure determination of a thermoalkalophilic lipase from Geobacillus SBS-4S

    International Nuclear Information System (INIS)

    Crystallization and the structure determination at 1.6 Å resolution of LIPSBS, a thermoalkalophilic lipase from Geobacillus strain SBS-4S, are described. The crystals belonged to orthorhombic space group P212121. A thermoalkalophilic lipase (LIPSBS) from the newly isolated Geobacillus strain SBS-4S which hydrolyzes a wide range of fatty acids has been characterized. In the present study, the crystallization of purified LIPSBS using the sitting-drop vapour-diffusion method and its X-ray diffraction studies are described. The crystals belonged to the orthorhombic space group P212121, with unit-cell parameters a = 55.13, b = 71.75, c = 126.26 Å. The structure was determined at 1.6 Å resolution by the molecular-replacement method using the lipase from G. stearothermophilus L1 as a model

  14. Quasiequilibrium Characterization of Mixed-Ion Coulomb Crystals

    Science.gov (United States)

    Okada, Kunihiro; Ichikawa, Masanari; Wada, Michiharu; Schuessler, Hans A.

    2015-11-01

    We demonstrate the application of reliable methods to determine both the average micromotion energies and the number of sympathetically cooled ions (SCIs) embedded in mixed-ion Coulomb crystals in a linear Paul trap. The number of the SCIs and the micromotion energies for the observed mixed-ion crystals are determined by comparing experimentally obtained images with molecular-dynamics simulations, where the kinetic energies of SCIs trapped in rf fields are averaged in cold elastic collisions between the laser-cooled ions and virtual very light atoms. This combined method quickly achieves the quasiequilibrium state of large mixed Coulomb crystals with over 103 ions, regardless of the initial conditions, and shows that the previously used pseudopotential-based adiabatic approximations should be replaced by such molecular-dynamics simulations. In addition, a pattern-matching recognition procedure is introduced which objectively ascertains the number of ions. We also apply the presented characterization method to determine the reaction-rate constant between slow acetonitrile molecules and sympathetically cooled Ne+ ions at a translational temperature lower than 10 K.

  15. 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

  16. 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...

  17. Structural characterization of electrodeposited boron

    Indian Academy of Sciences (India)

    Ashish Jain; C Ghosh; T R Ravindran; S Anthonysamy; R Divakar; E Mohandas; G S Gupta

    2013-12-01

    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 patterns and the power spectrum calculated from the lattice images from thin regions of the sample. Raman spectroscopic examination was carried out to study the nature of bonding and the allotropic form of boron obtained after electrodeposition. The results obtained from transmission electron microscopy showed the presence of nanocrystallites embedded in an amorphous mass of boron. Raman microscopic studies showed that amorphous boron could be converted to its crystalline form at high temperatures.

  18. Growth and characterization of an organometallic tri-allylthiourea complex nonlinear optical crystals

    Science.gov (United States)

    Perumal, R.; Moorthy Babu, S.

    2008-04-01

    A novel family of allylthiourea metal complexes was identified for photonic applications with allylthiourea serving as a double ligand, and II (B) group metals were chosen as a co-ordination metal. This family belongs to an island-type organometallic category. A series of optically negative nonlinear optical (NLO) crystals (ATCC, ATCB, ATMC and ATMB) have been prepared. Their SHG efficiency was an order of magnitude higher than that of the well-known organic crystal, urea. The properties of allylthiourea complex with central atom Cd were compared with the crystals with another central atom Hg. The latter has longer transparency cut-off wavelength, higher thermal stability and SHG efficiencies. These organometallic tri-allylthiourea complex crystals were grown from the aqueous solution by temperature-lowering technique. Comprehensive studies of synthesis, solubility, crystal growth and the general properties including structural, spectral, optical and thermal properties were analyzed by conducting various characterization techniques. They were synthesized in the de-ionized water and the solubilities of each material were determined by employing thermogravimetric analysis. The growth conditions were analyzed in terms of the pH value of the mother solution because it plays a vital role during the growth. Their structural properties were examined by recording the powder X-ray diffraction pattern. The crystal formation and the metal co-ordination were confirmed by the spectral analysis. The transmission spectrum of these crystals shows a wide transparent UV-vis-NIR band. The thermal behavior of these complexes was studied from the thermal studies. Their NLO efficiencies were analyzed through the Kurt'z technique.

  19. Cationic coordination compound Cs2Hg3I8 for IR NLO material: Synthesis, crystal growth and characterizations

    International Nuclear Information System (INIS)

    Single crystals Cs2Hg3I8 of dimensions 5 × 3 × 4   mm3 were grown by solution growth method at room temperature and structurally characterized by single crystal X – ray diffraction. Cs2Hg3I8 compound crystallizes in a noncentrosymmetric space group Cm with the crystal data of a = 7.4415 Å, b = 21.6629 Å, c = 7.6726 Å, α, β = 90°, γ = 108.05° and Z = 2. The grown crystals were characterized by powder X – ray diffraction analysis and the various diffraction planes are indexed. The presence of functional groups was identified qualitatively by Fourier transform infrared and FT – Raman spectral analyses. Ultraviolet – visible spectral analyses shows that the crystal has low UV cut off at 388 nm combined with very good transparency of 98 % in a wide range. The optical band gap was estimated to be 3 eV. Mechanical hardness of the grown crystal Cs2Hg3I8 was determined. The dielectric response of the crystal with varying frequencies was studied. Differential scanning calorimetry (DSC) analysis shows that the grown crystal has very good thermal stability up to 97.5°C

  20. Synthesis and structural characterization of actinide oxalate compounds

    International Nuclear Information System (INIS)

    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)

  1. Analysis of the crystal structure of a tetragonal RbD2PO4 single crystal

    International Nuclear Information System (INIS)

    Tetragonal RbD2PO4 single crystals, which are colorless and transparent, are synthesized from tetragonal RbH2PO4 crystals. A ferroelectric transition temperature was found to be 235 K from the temperature dependence of the structure factor F0 in neutron diffraction. Deuteriums in a paraelectric phase are in disordered array. Hydrogen bonds in the monoclinic structure form two-dimensional array in the bc plane, but in the tetragonal structure these display three-dimensional array. The distribution of deuterium was studied by Fourier analysis method. The crystal structure of tetragonal RbD2PO4 at a paraelectric phase was analyzed on the basis of neutron diffraction experiments, and the movement for PO4 tetrahedral was studied. The results for the tetragonal RbD2PO4 were compared with those for the monoclinic structure. (Y. Kazumata)

  2. Crystal structure and genesis of the hydrated analog of rastsvetaevite

    Science.gov (United States)

    Rastsvetaeva, R. K.; Aksenov, S. M.; Rozenberg, K. A.

    2015-11-01

    The crystal structure of the hydrated analog of the mineral rastsvetaevite (tentatively called "hydrorastsvetaevite"), which was found by A.P. Khomyakov in ultraagpaitic pegmatites at the Rasvumchorr Mountain of the Khibiny alkaline massif (Kola Peninsula), has been determined by single crystal X-ray diffraction. The trigonal unit-cell parameters are as follows: a = 14.2812(2) Å, c = 60.533(5) Å, V = 10691.54(3) Å3, sp. gr. R3 m. The structure was refined to R = 5.9% in the isotropic and anisotropic approximation of atomic displacement parameters based on 2068 ref lections with | F| > 3σ( F). "Hydrorastsvetaevite" is on the whole analogous to other 24-layer representatives of the eudialyte group (called "megaeudialytes"), but is characterized by a high potassium content and is distinguished from other potassium-rich minerals (rastsvetaevite, davinciite, and andrianovite) by low sodium and alkaline-earth metal content, as well as by a high degree of hydration accompanied by the insertion of H3O groups, which partially or completely replace large cations. The idealized formula of "hydrorastsvetaevite" ( Z = 3) is (Na11(H3O)11K6(H2O)1.5Sr)Ca12Fe3Na2MnZr6Si52O144(OH)4.5Cl3.5(H2O)0.5. In alkaline pegmatites, "hydrorastsvetaevite" occurs as a secondary mineral developed from the original rastsvetaevite through decationation and hydration. The characteristic features of the genesis of eudialyte-group minerals containing potassium as a species-forming cation are discussed in terms of the concept of transformational mineral species. an]Mis||Original Russian Text R.K. Rastsvetaeva, S.M. Aksenov, K.A. Rozenberg, 2015, published in Kristallografiya, 2015, Vol. 60, No. 6, pp. 897-905.

  3. Improved Synthesis and Crystal Structure of Dalcetrapib

    Directory of Open Access Journals (Sweden)

    Frank Richter

    2012-10-01

    Full Text Available An improved synthesis of the Cholesteryl Ester Transfer Protein inhibitor dalcetrapib is reported. The precursor disulfide was reduced (a by Mg/MeOH or (b by EtSH/DBU/THF. The resulting thiol was acylated (a by a known procedure or (b in a one-pot process. Impurities were removed (a by dithiothreitol (DTT or (b by oxidation using H2O2. Dalcetrapib crystallized in space group P21/c.

  4. Improved Synthesis and Crystal Structure of Dalcetrapib

    OpenAIRE

    Frank Richter; Sven Nerdinger; Herwig Schottenberger; Volker Kahlenberg; Gerhard Laus

    2012-01-01

    An improved synthesis of the Cholesteryl Ester Transfer Protein inhibitor dalcetrapib is reported. The precursor disulfide was reduced (a) by Mg/MeOH or (b) by EtSH/DBU/THF. The resulting thiol was acylated (a) by a known procedure or (b) in a one-pot process. Impurities were removed (a) by dithiothreitol (DTT) or (b) by oxidation using H2O2. Dalcetrapib crystallized in space group P21/c.

  5. Growth and characterization of L-histidine nitrate single crystal, a promising semiorganic NLO material

    International Nuclear Information System (INIS)

    Bulk single crystal, L-histidine nitrate (LHN), was obtained by the temperature-lowering method. The solubility curve of LHN was measured in distilled water. The LHN crystal was characterized by single-crystal X-ray diffraction, FT-IR spectra, thermal analyses, UV-vis spectra, microhardness and optical property. The transmission spectra of LHN crystal show lower UV cutoff wavelength lies at 320 nm. SHG intensity of LHN crystal is 1.5 times greater than that of KDP

  6. 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.

  7. 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.

  8. Single crystals of DPPH grown from diethyl ether and carbon disulfide solutions - Crystal structures, IR, EPR and magnetization studies

    Science.gov (United States)

    Žilić, Dijana; Pajić, Damir; Jurić, Marijana; Molčanov, Krešimir; Rakvin, Boris; Planinić, Pavica; Zadro, Krešo

    2010-11-01

    Single crystals of the free radical 2,2-diphenyl-1-picrylhydrazyl (DPPH) obtained from diethyl ether (ether) and carbon disulfide (CS2) were characterized by the X-ray diffraction, IR, EPR and SQUID magnetization techniques. The X-ray structural analysis and IR spectra showed that the DPPH form crystallized from ether (DPPH1) is solvent free, whereas that one obtained from CS2 (DPPH2) is a solvate of the composition 4DPPH·CS2. Principal values of the g-tensor were estimated by the X-band EPR spectroscopy at room and low (10 K) temperatures. Magnetization studies revealed the presence of antiferromagnetically coupled dimers in both types of crystals. However, the way of dimerization as well as the strength of exchange couplings are different in the two DPPH samples, which is in accord with their crystal structures. The obtained results improved parameters accuracy and enabled better understanding of properties of DPPH as a standard sample in the EPR spectrometry.

  9. 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.

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

    International Nuclear Information System (INIS)

    Graphical abstract: One-dimensional single-crystal multiferroic composites composed of PbTiO3 nanofiber-CoFe2O4 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 PbTiO3 (PTO) nanofiber-CoFe2O4 (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)

  11. 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)

  12. Single crystal synthesis methods dedicated to structural investigations of very low solubility mixed-actinide oxalate coordination polymers

    International Nuclear Information System (INIS)

    Two crystal growth methods dedicated to very low solubility actinide coordination polymers have been developed and applied to the synthesis of mixed actinide(IV) actinide(IV) or actinide(IV)-actinide(III) oxalate single crystals of a size (typically 100-300 μm) suitable for isolating them and examining their crystal structure. These methods have been optimized on mixed systems composed of U(IV) and lanthanide (surrogate of trivalent actinides) and then assessed on U(IV) Am(III), Pu(IV)-Am(III), and U(IV) Pu(IV) mixtures. Three types of single crystals characterized by different structures have been obtained according to the synthesis and the chemical conditions. This is the first time that these well-known or recently discovered key compounds are formed by crystal growth methods specifically developed for actinide crystal handling (i.e., in glove boxes), thus enabling direct structural studies on transuranium element systems and acquisition of basic data. Characterization by X-ray diffraction, UV-visible solid spectroscopy, thermal ionization mass spectroscopy (TIMS), energy-dispersive X-ray spectroscopy (EDS), and inductively coupled plasma atomic emission spectroscopy (ICP-AES) demonstrates the potentialities and complementarity of the two crystal growth methods for obtaining the targeted mixed oxalates (actinide oxidation state and presence of both metallic ions in the crystal). More generally, this development opens broad prospects for single crystal synthesis of novel actinide organic frameworks and their structural description. (authors)

  13. Crystal structure, nucleic-acid binding properties, and dimerization model of Pur-alpha

    OpenAIRE

    Graebsch, Almut

    2010-01-01

    This study characterizes Pur-α structurally and functionally. Pur-α is a highly conserved RNA- and DNA-binding protein involved in a multitude of cellular processes such as transcription, replication, cell cycle control, and mRNA transport. No homologous proteins with known structures are available. X-ray crystallography is often hampered by the lack of diffraction-quality protein crystals. This study demonstrates how this bottleneck was overcome by the combination of iterative use of sens...

  14. Thermal characterization of nanoscale phononic crystals using supercell lattice dynamics

    Directory of Open Access Journals (Sweden)

    Bruce L. Davis

    2011-12-01

    Full Text Available The concept of a phononic crystal can in principle be realized at the nanoscale whenever the conditions for coherent phonon transport exist. Under such conditions, the dispersion characteristics of both the constitutive material lattice (defined by a primitive cell and the phononic crystal lattice (defined by a supercell contribute to the value of the thermal conductivity. It is therefore necessary in this emerging class of phononic materials to treat the lattice dynamics at both periodicity levels. Here we demonstrate the utility of using supercell lattice dynamics to investigate the thermal transport behavior of three-dimensional nanoscale phononic crystals formed from silicon and cubic voids of vacuum. The periodicity of the voids follows a simple cubic arrangement with a lattice constant that is around an order of magnitude larger than that of the bulk crystalline silicon primitive cell. We consider an atomic-scale supercell which incorporates all the details of the silicon atomic locations and the void geometry. For this supercell, we compute the phonon band structure and subsequently predict the thermal conductivity following the Callaway-Holland model. Our findings dictate that for an analysis based on supercell lattice dynamics to be representative of the properties of the underlying lattice model, a minimum supercell size is needed along with a minimum wave vector sampling resolution. Below these minimum values, a thermal conductivity prediction of a bulk material based on a supercell will not adequately recover the value obtained based on a primitive cell. Furthermore, our results show that for the relatively small voids and void spacings we consider (where boundary scattering is dominant, dispersion at the phononic crystal unit cell level plays a noticeable role in determining the thermal conductivity.

  15. Crystal structure of 3-carbamothioylpyridinium thiocyanate

    OpenAIRE

    Hasna Bouchareb; Mhamed Boudraa; Sofiane Bouacida; Hocine Merazig; El Hossain Chtoun

    2015-01-01

    In the cation of the title salt, C6H7N2S+·SCN−, the C=S bond is oriented trans with respect to the C—C=N fragment in the pyridine ring. The planes of the aromatic ring and the thioamide fragment of the cation make a dihedral angle of 38.31 (4)°. In the crystal, the components are linked by N—H...S and N—H...N, hydrogen bonds, forming a two-dimensional network parallel to (10-1).

  16. Crystal structure of 3-carbamothioylpyridinium thiocyanate

    Directory of Open Access Journals (Sweden)

    Hasna Bouchareb

    2015-01-01

    Full Text Available In the cation of the title salt, C6H7N2S+·SCN−, the C=S bond is oriented trans with respect to the C—C=N fragment in the pyridine ring. The planes of the aromatic ring and the thioamide fragment of the cation make a dihedral angle of 38.31 (4°. In the crystal, the components are linked by N—H...S and N—H...N, hydrogen bonds, forming a two-dimensional network parallel to (10-1.

  17. Synthesis and crystal structure of Mo7Sn12Zn40 - a cubic compound with icosahedra

    International Nuclear Information System (INIS)

    Single phase samples of the new intermetallic compound Mo7Sn12Zn40 are synthesized from the elements at 1023 K. Mo7Sn12Zn40 crystallizes cubic (Fm3c) with a = 25.447 A. The complex crystal structure is characterized by two different polyhedra of high symmetry, which are built up by two shells. Besides chiral polyhedra MoZn14Sn24 there are nearly undistorted Mackay polyhedra Mo13Zn42 of symmetry lh, which are connected to a 3D net via Zn6 octahedra. Thereby twelve icosahedra MoZn10Sn2, which form the homogeneous cubic ''bauverband'' cP2[12i] condense to a ''supericosahedron''. The crystal structure can be regarded as a model structure for the crystallisation of intermetallic phases and shows a remarkable self similarity. (orig.)

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

    International Nuclear Information System (INIS)

    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

  19. Structural characterization of indium oxide nanostructures: a Raman analysis

    Energy Technology Data Exchange (ETDEWEB)

    Berengue, Olivia M; Rodrigues, Ariano D; Chiquito, Adenilson J [Departamento de Fisica, Universidade Federal de Sao Carlos, CEP 13565-905, CP 676, Sao Carlos, Sao Paulo (Brazil); Dalmaschio, Cleocir J; Leite, Edson R [Laboratorio Interdisciplinar de EletroquImica e Ceramicas, Departamento de Quimica, Universidade Federal de Sao Carlos, CEP 13565-905, CP 676, Sao Carlos, Sao Paulo (Brazil); Lanfredi, Alexandre J C, E-mail: olimb@df.ufscar.b [Centro de Engenharia, Modelagem e Ciencias Sociais Aplicadas-Universidade Federal do ABC, CEP 09210-170, Santo Andre, Sao Paulo (Brazil)

    2010-02-03

    In this work we report on structural and Raman spectroscopy measurements of pure and Sn-doped In{sub 2}O{sub 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.

  20. Structural characterization of indium oxide nanostructures: a Raman analysis

    International Nuclear Information System (INIS)

    In this work we report on structural and Raman spectroscopy measurements of pure and Sn-doped In2O3 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.

  1. 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.

  2. Optical and thermal control of domain structures in ferroelectric crystals

    OpenAIRE

    Brown, Paul Thomas

    1999-01-01

    This thesis presents the results of investigations into the thermal and optical control of ferroelectric domains within lithium tantalate and strontium barium niobate crystals. The aim of the work was to develop techniques for optically pattering domain inverted structures within ferroelectric crystals. Initial studies involving strontium barium niobate revealed an enhanced temperature sensitivity for transient repoling occurring at room temperatures for this material. This has important...

  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. Boron-oxygen polyanion in the crystal structure of tunellite

    Science.gov (United States)

    Clark, J.R.

    1963-01-01

    The crystal structure of tunellite, SrO??3B2O 3??4H2O, with infinite sheets of composition n[B6O9(OH)2]2-, has cations and water molecules in the spaces within the sheets. Adjacent sheets are held together by hydrogen bonding through the water molecules. The boron-oxygen polyanions provide the first example in hydrated borate crystals of one oxygen linked to three borons.

  5. 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.

  6. 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)

    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 oC, and exclusively xylobiose at 90 oC 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.

  7. Crystallization and initial crystallographic characterization of the Corynebacterium glutamicum nitrilotriacetate monooxygenase component A

    OpenAIRE

    KIM, KYUNG-JIN; Kim, Sujin; Lee, Sujin; Kang, Beom Sik; Lee, Heung-Soo; Oh, Tae-Kwang; Kim, Myung Hee

    2006-01-01

    The Corynebacterium glutamicum NTA monooxygenase component A protein, which plays the central role in NTA biodegradation, was crystallized. The initial X-ray crystallographic characterization is reported.

  8. Pure and Nd added NBT-BT single crystals - Growth and their characterization

    Science.gov (United States)

    Sundari, S. Shanmuga; Baskar, K.; Dhanasekaran, R.

    2014-04-01

    The lead free piezoelectric materials are secured an important place in the field of material science and engineering. In the present work single crystals of sodium bismuth titanate- barium titanate (0.94NBT-0.06BT) and 0.6 wt % of Nd added NBT-BT has been grown by flux method. The addition of 0.6 wt% of Nd shows the inhomogeneity in melt and the crystals collected from the top, middle and bottom portions of the crucible have been characterized for their structural and dielectric properties. The Nd concentration is found to be more in the crystals grown from the bottom portion of crucible and it was confirmed by optical and structural analysis. After the addition of Nd the color of the crystal changes form pale yellow to muddy green. The depolarization temperature (Td) and the temperature where the dielectric constant reaches its maximum (Tm) are increased from 442 K to 475 K and 595 K and 628 K respectively after the addition the of Nd in NBT-BT.

  9. Characterizing Internet Worm Infection Structure

    CERN Document Server

    Wang, Qian; Chen, Chao

    2010-01-01

    Internet worm infection continues to be one of top security threats. Moreover, worm infection has been widely used by botnets to recruit new bots and construct P2P-based botnets. In this work, we attempt to characterize the network structure of Internet worm infection and shed light on the micro-level information of "who infects whom." Our work quantifies the infection ability of individual hosts and reveals the key characteristics of the underlying topologies formed by worm infection, i.e., the number of children and the generation of the Internet worm infection family tree. Specifically, we first analyze the infection tree of a wide class of worms, for which a new victim is compromised by each existing infected host with equal probability. We find that the number of children has asymptotically a geometric distribution with parameter 0.5. We also discover that the generation follows closely a Poisson distribution and the average path length of the worm infection family tree increases approximately logarithmi...

  10. On automation of the procedure for crystal structure model refinement

    International Nuclear Information System (INIS)

    The methods of automation of the procedure for crystal structure model refinement from experimental diffraction data, implemented in the ASTRA program package, are described. Such tools as statistical tests, parameter scanning, and data scanning reduce the time necessary for structural investigation. At strong correlations between parameters, especially when the data set is limited, parameter scanning has an advantage over the full-matrix refinement.

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

    International Nuclear Information System (INIS)

    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 (Td) of polyethylene glycol octadecyl ether [HO(CH2CH2O)nC18H37, 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. Td increases rapidly with increasing the number of repeat units. C18En are a series of promising polymeric PCMs

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

    Energy Technology Data Exchange (ETDEWEB)

    Meng, Jie-yun; Tang, Xiao-fen; Li, Wei; Shi, Hai-feng [Tianjin Municipal Key Lab of Fiber Modification and Functional Fiber, School of Material Science and Engineering, Tianjin Polytechnic University, Tianjin 300387 (China); Zhang, Xing-xiang, E-mail: zhangpolyu@yahoo.com.cn [Tianjin Municipal Key Lab of Fiber Modification and Functional Fiber, School of Material Science and Engineering, Tianjin Polytechnic University, Tianjin 300387 (China)

    2013-04-20

    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{sub d}) of polyethylene glycol octadecyl ether [HO(CH{sub 2}CH{sub 2}O){sub n}C{sub 18}H{sub 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{sub d} increases rapidly with increasing the number of repeat units. C18En are a series of promising polymeric PCMs.

  13. Crystal engineering with thioureas: A structure-based inquiry

    Science.gov (United States)

    Paisner, Kathryn A.

    2011-12-01

    Structural trends applicable to crystal engineering were studied in three classes of thiourea-based compounds. The aim of the study was to identify, predict, and ultimately design reliable single-molecule structural features, which could then be used to engineer crystals with desirable properties. In one class of compounds, this goal was achieved: N-alkyl and N-aryl derivatives of N,N'-bis(3-thioureidopropyl)piperazine adopted an identical conformation in the solid state, which resulted in near-identical crystal packing. A second class of closely related compounds, N-substituted tris(2-thioureidoethyl)amines, showed no such reliability in the solid state, likely because the parent structure lacked hydrogen-bonding functionalities sufficient to control intramolecular structure. In the third class of compounds that we studied, 1-benzoyl-3-(2-pyridyl)thioureas, substitution patterns were often predictive of molecular conformation; however, these intramolecular trends did not lead to recognizable crystal packing motifs. Nevertheless, certain physical properties observed in this last class of compounds---color, solubility, and often crystallinity---were conformer-specific, interestingly without any apparent relevance to crystal lattice structure. Solution-state and solid-state conformational trends in these 1-benzoyl-3-(2-pyridyl)thioureas have been documented, and speculations as to the source of color in one of the two observed conformations have been noted.

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

    International Nuclear Information System (INIS)

    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

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

    Energy Technology Data Exchange (ETDEWEB)

    Schultz-Heienbrok, Robert [Institut für Chemie und Biochemie/Kristallographie, Freie Universität Berlin (Germany); Remmel, Natascha; Klingenstein, R. [Kekule-Institut für Organische Chemie und Biochemie, Rheinische Friedrich-Wilhelms-Universität Bonn (Germany); Rossocha, Maksim [Institut für Chemie und Biochemie/Kristallographie, Freie Universität Berlin (Germany); Sandhoff, Konrad [Kekule-Institut für Organische Chemie und Biochemie, Rheinische Friedrich-Wilhelms-Universität Bonn (Germany); Saenger, Wolfram [Institut für Chemie und Biochemie/Kristallographie, Freie Universität Berlin (Germany); Maier, Timm, E-mail: timm.maier@mol.biol.ethz.ch [Institut für Chemie und Biochemie/Kristallographie, Freie Universität Berlin (Germany); Institute for Molecular Biology and Biophysics, Swiss Federal Institute of Technology, ETH Zürich (Switzerland)

    2006-02-01

    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.

  16. Fabrication and characterization of size-controlled single-crystal-like PZT nanofibers by sol–gel based electrospinning

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Juan; Gao, Qian; He, Haiyan; Li, Xiang, E-mail: xiang.li@zju.edu.cn; Ren, Zhaohui; Liu, Yong; Shen, Ge; Xu, Gang; Zhang, Xiwen; Han, Gaorong, E-mail: hgr@zju.edu.cn

    2013-12-05

    Highlights: •Single-crystal-like PZT nanofibers were fabricated by electrospinning and calcination. •Fiber diameter was precisely controlled by solution viscosity and electrospinning parameters. •Pyrolysis is a key factor for fabrication of single-crystal-like structure. -- Abstract: Size-controlled single-crystal-like lead zirconate titanate (PbZr{sub 0.52}Ti{sub 0.48}O{sub 3}, PZT) ceramic fibers have been successfully prepared by sol–gel based electrospinning and subsequent calcination process, and their morphology, crystal structure have been characterized at nanoscale. The fiber diameter can be precisely controlled from ∼50 to 540 nm by varying the PVP concentration and electrospinning process parameters. The crystal structure of the nanofibers pyrolyzed at 400 °C for 0.5 h and calcined at 650 °C for 2 h is proved to be single-crystal-like tetragonal perovskite phase. A formation mechanism is also discussed based on the thermal decomposition process, effect of the calcination and pyrolysis procedure, using the thermogravimetry/differential scanning caborimetry (TG/DSC), X-ray diffraction (XRD) and transmission electron microscopy (TEM). It is found that the pyrolysis procedure is a critical factor for the fabrication of single-crystal-like structure PZT nanofibers using electrospinning.

  17. X-Ray Microdiffraction Characterization of Deformation Heterogeneities in BCC Crystals

    International Nuclear Information System (INIS)

    The deformation behavior of BCC metals is being investigated by x-ray microdiffraction measurements (mu XRD) for the purpose of characterizing the dislocation structure that results from uniaxial compression experiments. The high brilliance synchrotron source at the Advanced Light Source (Lawrence Berkeley National Lab) and the micron resolution of the focusing optics allow for the mapping of Laue diffraction patterns across a sample. These measurements are then analyzed in order to map the distribution of residual stresses in the crystal. An important finding is the observation of Laue spot ''streaking'', which indicates localized rotations in the lattice. These may represent an accumulation of same-sign dislocations. Theoretical modeling of the diffraction response for various slip systems is presented, and compared to experimental data. Preliminary results include orientation maps from a highly strained Ta bicrystal and a less highly strained Mo single crystal. The orientation maps of the bicrystal indicate a cell-like structure of dense dislocation walls. This deformation structure is consistent with previous OIM studies of the same crystal. The results suggest that mu XRD may be a particularly useful tool for microscale studies of deformation patterns in a multi-scale investigation of the mechanisms of deformation that ranges from macroscopic deformation tests to high resolution TEM studies of dislocation structures

  18. High-pressure studies on molecular crystals-relations between structure and high-pressure behavior

    Energy Technology Data Exchange (ETDEWEB)

    Orgzall, Ingo [Institut fuer Duennschichttechnologie und Mikrosensorik e.V., Kantstrasse 55, D-14513 Teltow (Germany); Emmerling, Franziska [Bundesanstalt fuer Materialforschung und -pruefung, Richard-Willstaetter-Strasse 11, D-12489 Berlin (Germany); Schulz, Burkhard [Institut fuer Physik, Universitaet Potsdam, Am Neuen Palais 10, D-14469 Potsdam (Germany); Franco, Olga [Heinrich-Heine-Universitaet Duesseldorf, Institut fuer Physikalische Chemie II, Universitaetsstrasse 1, Gebaeude 26.42.02, D-40225 Duesseldorf (Germany)], E-mail: orgzall@uni-potsdam.de, E-mail: franziska.emmerling@bam.de, E-mail: buschu@uni-potsdam.de, E-mail: olga.franco@uni-duesseldorf.de

    2008-07-23

    This paper summarizes attempts to understand structure-property relationships for a large class of aromatic diphenyl-1,3,4-oxadiazole molecules. Starting from the investigation of the crystal structure several common packing motifs as well as characteristic differences are derived. Many different molecules show a rather planar conformation in the solid state. A stronger intermolecular twist is only observed for compounds with substituents occupying the ortho-positions of the phenyl rings. Most crystal structures are characterized by the formation of stacks leading to intense {pi}-{pi} acceptor-donor interactions between oxadiazole and phenyl rings. High-pressure investigations result in a soft compression behavior typical for organic molecular crystals. The bulk behavior may be described by the Murnaghan equation of state with similar coefficients (bulk modulus and its pressure derivative) for nearly all investigated compounds but also for related substances. The compression shows a strong anisotropy resulting from the specific features and packing motifs of the crystal structure. This is clearly indicated by a corresponding strain analysis. Additionally to the crystal structure the Raman spectrum was also investigated under increasing pressure. The different pressure behavior of external and internal modes reflects the difference between intra- and intermolecular interactions.

  19. High-pressure studies on molecular crystals-relations between structure and high-pressure behavior

    International Nuclear Information System (INIS)

    This paper summarizes attempts to understand structure-property relationships for a large class of aromatic diphenyl-1,3,4-oxadiazole molecules. Starting from the investigation of the crystal structure several common packing motifs as well as characteristic differences are derived. Many different molecules show a rather planar conformation in the solid state. A stronger intermolecular twist is only observed for compounds with substituents occupying the ortho-positions of the phenyl rings. Most crystal structures are characterized by the formation of stacks leading to intense π-π acceptor-donor interactions between oxadiazole and phenyl rings. High-pressure investigations result in a soft compression behavior typical for organic molecular crystals. The bulk behavior may be described by the Murnaghan equation of state with similar coefficients (bulk modulus and its pressure derivative) for nearly all investigated compounds but also for related substances. The compression shows a strong anisotropy resulting from the specific features and packing motifs of the crystal structure. This is clearly indicated by a corresponding strain analysis. Additionally to the crystal structure the Raman spectrum was also investigated under increasing pressure. The different pressure behavior of external and internal modes reflects the difference between intra- and intermolecular interactions

  20. Scintillation characterization of thallium-doped lithium iodide crystals

    Energy Technology Data Exchange (ETDEWEB)

    Khan, Sajid [Department of Physics, Kyungpook National University, Daegu 702-701 (Korea, Republic of); Kim, H.J., E-mail: hongjoo@knu.ac.kr [Department of Physics, Kyungpook National University, Daegu 702-701 (Korea, Republic of); Kim, Y.D. [Center for Underground Physics, Institute for Basic Science (IBS), Daejon 305-811 (Korea, Republic of)

    2015-09-01

    The paper discusses scintillation and luminescence properties of thallium-doped LiI crystals, grown by the Bridgman technique. X-ray induced emission spectrum is obtained between 380 nm and 600 nm, and is attributed to the Tl{sup +} ion. The photoluminescence measurement with the excitation wavelength of 305 nm revealed a similar emission spectrum. Light yield, energy resolution and scintillation decay time profiles were studied under 662 keV ({sup 137}Cs) γ-ray excitation. A maximum light yield of 14,000±1400 ph/MeV and two exponential decay time components were obtained. - Highlights: • Luminescence and scintillation characterization of LiI(Tl) crystals are presented. • Broad emission bands peaking at 470 nm were observed under X-ray and UV excitation. • The best energy resolution was found to be 8.5% (FWHM) for 0.5% Tl-concentration. • Light yield of 14,000±1400 ph/MeV was observed for 0.5% Tl under γ-ray excitation. • Decay time spectra shows two decay components under γ-ray excitation.

  1. Synthesis and Characterization of Titanosilicate with the Structure of Umbite

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    A zeolitic titanosilicate with the composition of K2TiSi3O9*H2O, a structural analogue of natural mineral umbite K2ZrSi3O9*H2O, was hydrothermally synthesized in the SiO2-TiO2-K2O-H2O system and characterized by means of powder X-ray diffraction, SEM, IR and thermal analysis. The effects of TiO2/SiO2 and OH-/SiO2 ratios on the crystallization of the umbite were discussed. The influence of the organic additives on the morphology of the crystal was also investigated and the crystals with different shapes were obtained.

  2. Structural Characterization of Crystalline Ice Nanoclusters

    Science.gov (United States)

    Blake, David

    2000-01-01

    Water ice nanoclusters are useful analogs for studying a variety of processes that occur within icy grains in the extraterrestrial environment. The surface of ice nanoclusters prepared in the laboratory is similar to the surface of interstellar ice grains. In cold molecular clouds, the silicate cores of interstellar grains are typically approx. 100 nm in diameter and have a coating of impure amorphous water ice. Depositional, thermal and radiolytic processes leave the surface and subsurface molecules in a disordered state. In this state, structural defects become mobile and reactions of trapped gases and small molecules can occur. The large surface area of nanocluster deposits relative to their bulk allows for routine observation of such surface-mediated processes. Furthermore, the disordered surface and subsurface layers in nanocluster deposits mimic the structure of amorphous ice rinds found on interstellar dust grains. Transmission Electron Microscopy (TEM has been used tn characterize the crystallinity, growth mechanism, and size distribution of nanoclusters formed from a mixture of water vapor with an inert carrier gas that has been rapidly cooled to 77K. E M imaging reveals a Gaussian size distribution around a modal diameter that increases from approx. 15 to 30 nm as the percentage of water vapor within the mixture increases from 0.5 to 2.007, respectively . TEM bright and dark field imaging also reveals the crystalline nature of the clusters. h4any of the clusters show a mosaic structure in which crystalline domains originate at the center Other images show mirror planes that are separated by approx. 10 nm. Electron diffraction patterns of these clusters show that the clusters are composed of cubic ice with only a small hexagonal component. Further, the crystalline domain size is approximately the same as the modal diameter suggesting that the clusters are single crystals.

  3. Crystal structure of 1-(4-formylbenzylidenethiosemicarbazone

    Directory of Open Access Journals (Sweden)

    Rosa Carballo

    2014-09-01

    Full Text Available The asymmetric unit of the title compound, C9H9N3OS, contains two approximately planar molecules (r.m.s. deviations for 14 non-H atoms = 0.094 and 0.045 Å, with different conformations. In one of them, the C=O group is syn to the S atom and in the other it is anti. Each molecule features an intramolecular N—H...N hydrogen bond, which generates an S(5 ring. In the crystal, molecules are linked by N—H...O and N—H...S hydrogen bonds, generating discrete networks; the syn molecules form [010] chains and the anti molecules form (100 sheets.

  4. 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.

  5. Crystal structure of 2-[(dichloromethanesulfonyl]pyridine

    Directory of Open Access Journals (Sweden)

    Zhiqiu Chen

    2014-12-01

    Full Text Available The asymmetric unit of the title compound, C6H5Cl2NO2S, contains two molecules with similar conformations (r.m.s. overlay fit for the non-H atoms = 0.067 Å. Atoms attached to the pendent Csp3—S bond are arranged in a staggered conformation with one of the Cl atoms anti to the C atom in the aromatic ring [C—S—C—Cl torsion angles = 178.41 (11 and −176.70 (13°]. In the crystal, molecules are linked by C—H...N and C—H...O hydrogen bonds, generating a three-dimensional network, and weak aromatic π–π stacking is also observed [centroid–centroid separation = 3.8902 (17 Å].

  6. Divalent europium doped and un-doped calcium iodide scintillators: Scintillator characterization and single crystal growth

    International Nuclear Information System (INIS)

    The alkaline-earth scintillator, CaI2:Eu2+, was initially discovered around 1964 by Hofstadter, Odell, and Schmidt. Serious practical problems quickly arose, however, that were associated with the growth of large monolithic single crystals of this material due to its lamellar, mica-like structure. As a result of its theoretically higher light yield, CaI2:Eu2+ has the potential to exceed the excellent scintillation performance of SrI2:Eu2+. In fact, theoretical predictions for the light yield of CaI2:Eu2+ scintillators suggested that an energy resolution approaching 2% at 662 keV could be achievable. As in the case of the early SrI2:Eu2+ scintillator, the performance of CaI2:Eu2+ scintillators has traditionally suffered due, at least in part, to outdated materials synthesis, component stoichiometry/purity, and single-crystal-growth techniques. Based on our recent work on SrI2:Eu2+ scintillators in single-crystal form, we have developed new techniques that are applied here to CaI2:Eu2+ and pure CaI2 with the goal of growing large un-cracked crystals and, potentially, realizing the theoretically predicted performance of the CaI2:Eu2+ form of this material. Calcium iodide does not adhere to modern glassy carbon Bridgman crucibles—so there should be no differential thermal-contraction-induced crystal/crucible stresses on cooling that would result in crystal cracking of the lamellar structure of CaI2. Here we apply glassy carbon crucible Bridgman growth, high-purity growth-charge compounds, our molten salt processing/filtration technique, and extended vacuum-melt-pumping methods to the growth of both CaI2:Eu2+ and un-doped CaI2. Large scintillating single crystals were obtained, and detailed characterization studies of the scintillation properties of CaI2:Eu2+ and pure CaI2 single crystals are presented that include studies of the effects of plastic deformation of the crystals on the scintillator performance

  7. Combined crystal structure prediction and high-pressure crystallization in rational pharmaceutical polymorph screening

    Science.gov (United States)

    Neumann, M. A.; van de Streek, J.; Fabbiani, F. P. A.; Hidber, P.; Grassmann, O.

    2015-07-01

    Organic molecules, such as pharmaceuticals, agro-chemicals and pigments, frequently form several crystal polymorphs with different physicochemical properties. Finding polymorphs has long been a purely experimental game of trial-and-error. Here we utilize in silico polymorph screening in combination with rationally planned crystallization experiments to study the polymorphism of the pharmaceutical compound Dalcetrapib, with 10 torsional degrees of freedom one of the most flexible molecules ever studied computationally. The experimental crystal polymorphs are found at the bottom of the calculated lattice energy landscape, and two predicted structures are identified as candidates for a missing, thermodynamically more stable polymorph. Pressure-dependent stability calculations suggested high pressure as a means to bring these polymorphs into existence. Subsequently, one of them could indeed be crystallized in the 0.02 to 0.50 GPa pressure range and was found to be metastable at ambient pressure, effectively derisking the appearance of a more stable polymorph during late-stage development of Dalcetrapib.

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

    Science.gov (United States)

    Jin, Geng Bang; Soderholm, L.

    2015-01-01

    Colorless crystals of ThSiO4 (huttonite) (1) and (Ca0.5Na0.5)2NaThSi8O20 (2) have been synthesized by the solid-state reactions of ThO2, CaSiO3, and Na2WO4 at 1073 K. Green crystals of (Ca0.5Na0.5)2NaUSi8O20 (3) have been synthesized by the solid-state reactions of UO2, CaSiO3, and Na2WO4 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 ThO9 polyhedra and SiO4 tetrahedra. Compounds 2 and 3 are isostructural and they crystallize in a steacyite-type structure. The structure consists of discrete pseudocubic [Si8O20]8- polyanions, which are connected by An4+ cations into a three-dimensional framework. Each An atom coordinates to eight monodentate [Si8O20]8- moieties in a square antiprismatic geometry. Na+ and Ca2+ 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.

  10. 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.

  11. Compact Couplers for Photonic Crystal Laser-Driven Accelerator Structures

    International Nuclear Information System (INIS)

    Photonic crystal waveguides are promising candidates for laser-driven accelerator structures because of their ability to confine a speed-of-light mode in an all-dielectric structure. Because of the difference between the group velocity of the waveguide mode and the particle bunch velocity, fields must be coupled into the accelerating waveguide at frequent intervals. Therefore efficient, compact couplers are critical to overall accelerator efficiency. We present designs and simulations of high-efficiency coupling to the accelerating mode in a three-dimensional photonic crystal waveguide from a waveguide adjoining it at 90o. We discuss details of the computation and the resulting transmission. We include some background on the accelerator structure and photonic crystal-based optical acceleration in general.

  12. Structural relaxation in a glassy liquid crystal: MBBA

    International Nuclear Information System (INIS)

    Combined neutron and Raman scattering measurements were performed to analyze the solid polymorphic modifications of a typical nematic liquid crystal substance, MBBA. A glassy solid phase, classified as oriented molecular glass (OMG) may be produced by fast cooling from the nematic phase. A sequence of irreversible phase transitions was observed on reheating OMG. Four different solid modifications were found: two structurally relaxed amorphous 'mesophases' and two crystalline ones. A distinct modification can be found by slow crystallization from the nematic phase and it can be transformed reversibly into an other crystal structure by further cooling. The role of medium range order in the non-crystalline phases and the structural relaxation of the OMG state were analyzed. (author)

  13. Static and dynamic structure analyses of polymer crystals

    International Nuclear Information System (INIS)

    Recent development in static and dynamic structure analyses of polymer crystals has been reviewed. Various methods were developed to enhance the reliability of static structure analysis. Usage of synchrotron high-energy X-ray beam allowed us to increase the total number of observed X-ray reflections by one order. Wide-angle neutron diffraction revealed the hydrogen atomic positions accurately, making it possible to evaluate the mechanical property of polymer crystals quantitatively. Time-resolved measurements of wide-angle and small-angle X-ray scatterings as well as infrared and Raman spectra have revealed the structural revolution processes as seen in the studies of isothermal crystallization and mechanical deformation processes. (author)

  14. Free-Standing Photonic Crystal Films with Gradient Structural Colors.

    Science.gov (United States)

    Ding, Haibo; Liu, Cihui; Ye, Baofen; Fu, Fanfan; Wang, Huan; Zhao, Yuanjin; Gu, Zhongze

    2016-03-23

    Hydrogel colloidal crystal composite materials have a demonstrated value in responsive photonic crystals (PhCs) via controllable stimuli. Although they have been successfully exploited to generate a gradient of color distribution, the soft hydrogels have limitations in terms of stability and storage caused by dependence on environment. Here, we present a practical strategy to fabricate free-standing PhC films with a stable gradient of structural colors using binary polymer networks. A colloidal crystal hydrogel film was prepared for this purpose, with continuously varying photonic band gaps corresponding to the gradient of the press. Then, a second polymer network was used to lock the inside non-close-packed PhC structures and color distribution of the hydrogel film. It was demonstrated that our strategy could bring about a solution to the angle-dependent structural colors of the PhC films by coating the surface with special microstructures. PMID:26962967

  15. Studies on the growth and characterization of tris (glycine) calcium(ΙΙ) dichloride-a nonlinear optical crystal

    International Nuclear Information System (INIS)

    A systematic characterization of a novel nonlinear optical material tris (glycine) calcium(ΙΙ) dichloride (TGCC) is performed. The solubility and metastable zone width of TGCC were studied. TGCC single crystal of dimensions 34x23x5 mm3 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.

  16. Comment on the paper: Synthesis, growth and characterization of cadmium manganese thiocyanate (CMTC) crystal

    OpenAIRE

    Srinivasan, Bikshandarkoil R.

    2015-01-01

    The authors of the title paper (Spectrochim. Acta 79A (2011) 340-343) report the crystal growth of cadmium manganese thiocyanate CdMn(SCN)4 and its characterization by single crystal X-ray diffraction and infrared spectrum. Many points of criticism, concerning the crystal growth and reported experimental data are highlighted in this report.

  17. Structure and properties of MTiOXO sub 4 crystals

    CERN Document Server

    Latham, T J

    2000-01-01

    linked to chains of particular atoms along the three crystallographic axes. Dielectric measurements of a series of arsenate crystals and various doped phosphate crystals demonstrate that MTiOXO sub 4 isomorphs exhibit dielectric relaxation of a non-Debye type and appear to conform to the hopping charge-carrier and low frequency dispersion response models. A reduction in the ionic conductivity is observed in the arsenate crystals and phosphate crystals doped with trivalent ions. Arrhenius plots indicate that the activation energies of the mixed cation arsenate crystals are significantly higher than the other KTiOPO sub 4 isomorphs. This observation suggests that the modified oxygen framework in these mixed arsenate crystals contributes intrinsically to the large activation energies required for ionic conduction. This thesis is a study of the structural, optical and electrical properties of MTiOXO sub 4 crystals, where M is a monovalent cation such as K, Rb etc and X is P or As. Low and high-temperature single-...

  18. 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 a

  19. 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.

  20. Tris(dithiocarboxylato)indium(III): Thermal studies and crystal structure of [In(S2Ctol)3

    Indian Academy of Sciences (India)

    Shamik Ghoshal; Nisha P Kushwah; Manoj K Pal; Vimal K Jain; Munirathinam Nethaji

    2008-05-01

    Tris(dithiocarboxylato)indium(III), [In{S2CAr}3] (Ar = phenyl or -tolyl) have been synthesized and characterized. The molecular structure of [In(S2Ctol)3] established by single crystal X-ray diffraction revealed a distorted octahedral geometry with symmetrically chelating dithiocarboxylate groups. These complexes on thermolysis gave -In2S3 which was characterized by XRD and EDX.