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Sample records for synthesis crystal structure

  1. SYNTHESIS, CHARACTERIZATION AND CRYSTAL STRUCTURES ...

    African Journals Online (AJOL)

    B. S. Chandravanshi

    The V atoms in the complexes are in octahedral coordination. Thermal stabilities of the complexes have also been studied. KEY WORDS: Oxovanadium complex, Aroylhydrazone ligand, Crystal structure, X-ray diffraction, Thermal property. INTRODUCTION. Coordination chemistry of vanadium has attracted considerable ...

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

    Indian Academy of Sciences (India)

    Home; Journals; Journal of Chemical Sciences; Volume 127; Issue 12. Hydrothermal synthesis, crystal structure and luminescence property of a three dimensional Sm(III) coordination polymer with 2,5-pyridinedicarboxylic acid. Kranthi Kumar Gangu Anima S Dadhich Saratchandra Babu Mukkamala. Volume 127 Issue 12 ...

  3. Synthesis, crystal structure, thermal analysis and dielectric

    Indian Academy of Sciences (India)

    Annual Meetings · Mid Year Meetings · Discussion Meetings · Public Lectures · Lecture Workshops · Refresher Courses · Symposia · Live Streaming. Home; Journals; Bulletin of Materials Science; Volume 39; Issue 5. Synthesis, crystal structure, thermal analysis and dielectric properties of two mixed trichlorocadmiates (II).

  4. SYNTHESIS, CHARACTERIZATION AND CRYSTAL STRUCTURE ...

    African Journals Online (AJOL)

    Preferred Customer

    Cg1, Cg2 and Cg3 are the centroids of Mo1-O2-C8-N2-N1, C9-C14 and. C1-C6 benzene rings. Figure 1. Molecular structure of the complex at 30% probability displacement. IR spectra. The hydrazone ligands showed stretching bands attributed to C=O, C=N, C–OH and NH at. 1656, 1637, 1155 and 1237, and 3211 cm–1, ...

  5. Synthesis, crystal structure, theoretical study and luminescence ...

    Indian Academy of Sciences (India)

    phenanthroline) has been synthesized and characterized by elemental analysis, infrared spectroscopy, ultraviolet-visible spectroscopy, X-ray single crystal analysis and fluorescent analysis. Its crystal structure is monoclinic with space group 2/ and ...

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

    Indian Academy of Sciences (India)

    In both the materials, the crystal structure has been determined by X-ray single crystal analysis at room temperature (293 K). The compound structures consist of K + (or NH 4 + ) cations and double chains of CdCl 6 octahedra sharing one edge extending along b -axis. The mixture of KA + /NH 4 + cations are located ...

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

    Indian Academy of Sciences (India)

    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 ...

  8. Synthesis and crystal structure of a wheel-shaped supramolecular ...

    Indian Academy of Sciences (India)

    Home; Journals; Journal of Chemical Sciences; Volume 126; Issue 5. Synthesis and crystal structure of a wheel-shaped supramolecular coordination complex. Deepak Gupta Palanisamy Rajakannu Bhaskaran Shankar Firasat Hussain Malaichamy Sathiyendiran. Special issue on Chemical Crystallography Volume 126 ...

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

    Indian Academy of Sciences (India)

    2.2 X-ray structure determination. Two transparent parallelepipedic crystals with dimensions,. 0.20 × 0.12 × 0.04 and 0.26 × 0.14 × 0.12, were chosen from the preparation. The intensity data were collected on. An APEX II diffractometer with graphite–crystal monochro- mated MoKα radiation (0.71073 Å). Lorentz and polariz-.

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

    African Journals Online (AJOL)

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

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

    Indian Academy of Sciences (India)

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

  12. Synthesis, crystal structures, hydrogen bonding graph-sets and ...

    African Journals Online (AJOL)

    Synthesis, crystal structures, hydrogen bonding graph-sets and theoretical studies of nickel (+II) co-ordinations with pyridine-2,6-dicarboxamide oxime. ... which crystallized in the monoclinic space group C2/c with a = 14.915(2), b = 0.895(2), c = 8.205(1) Å, β = 114.69(1), and Z = 4. The complex consists of discrete cations ...

  13. Synthesis, crystal structure and catecholase activity of a Ni (II ...

    Indian Academy of Sciences (India)

    Home; Journals; Journal of Chemical Sciences; Volume 126; Issue 6. Synthesis, crystal structure and catecholase activity of a Ni(II) complex derived from a tetradentate Schiff base ligand. Pradipta Kumar Basu Merry Mitra Amrita Ghosh Latibuddin Thander Chia -Her Lin Rajarshi Ghosh. Rapid Communications Volume 126 ...

  14. Synthesis, characterization, X-ray crystal structure, electrochemical ...

    Indian Academy of Sciences (India)

    DOI 10.1007/s12039-015-0978-8. 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. IRAN SHEIKHSHOAIEa, S YOUSEF EBRAHIMIPOURa,∗, MAHDIEH SHEIKHSHOAIEa,.

  15. Synthesis and crystal structure of a wheel-shaped supramolecular ...

    Indian Academy of Sciences (India)

    Synthesis and crystal structure of a wheel-shaped supramolecular coordination complex. DEEPAK GUPTA, PALANISAMY RAJAKANNU, BHASKARAN SHANKAR,. FIRASAT HUSSAIN and MALAICHAMY SATHIYENDIRAN. ∗. Department of Chemistry, University of Delhi, Delhi 110 007, India e-mail: mvdiran@yahoo.com; ...

  16. Synthesis crystal structure, photoluminescence and photocatalytic ...

    Indian Academy of Sciences (India)

    photoluminescence and photocatalytic properties of 1 were also been investigated. Keywords. Zinc; 5-(pyridyl)tetrazolato (PTZ); Single-Crystal X-Ray Crystallography. 1. Introduction. In last few years tetrazole ligands have been widely used to synthesize metal–organic and H-bonded frameworks of various topologies.1–5 ...

  17. Synthesis, crystal structure, theoretical study and luminescence ...

    Indian Academy of Sciences (India)

    performed on complex 1 to rationalize its experimental absorption spectra. Complex 1 exhibits luminescence in EtOH ... potential applications in biological systems like, devel- opment of structural and functional models for ... to react with [WOnS4−n] (n = 0-2).11,12 These reactions result in the formation of a large number of ...

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

    Science.gov (United States)

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

    2017-11-01

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

  19. Synthesis and crystal structure of chromium-bearing anhydrous wadsleyite

    Science.gov (United States)

    Sirotkina, E. A.; Bindi, L.; Bobrov, A. V.; Aksenov, S. M.; Irifune, T.

    2018-04-01

    A chromium-bearing wadsleyite (Cr- Wad) was synthesized in the model system Mg2SiO4-MgCr2O4 at 14 GPa and 1600 °C and studied from the chemical and structural point of views. Microprobe data gave the formula Mg1.930Cr0.120Si0.945O4, on the basis of 4 oxygen atoms. The crystal structure has been studied by single-crystal X-ray diffraction. The orthorhombic unit-cell parameters are: a = 5.6909(5) Å, b = 11.4640(10) Å, c = 8.2406(9) Å, V = 537.62(9) Å3, Z = 8. The structure, space group Imma, was refined to R 1 = 5.99% in anisotropic approximation using 1135 reflections with F o > 4σ( F o) and 43 parameters. Chromium was found to substitute for both Mg at the octahedral sites and Si at the tetrahedral site, according to the reaction VIMg2+ + IVSi4+ = VICr3+ + IVCr3+. On the whole, the structural topology is nearly identical to that of pure wadsleyite. The successful synthesis of Cr- Wad may be important for the thermobarometry of mantle phase associations.

  20. Synthesis, crystal structure, optical and electrochemical properties of ...

    Indian Academy of Sciences (India)

    Its molecular geometry in the ground state has also been calculated using density functional theory (DFT) at the B3LYP/6-31G∗∗ level and compared with its crystal structure. Results show that the optimized geometry can well reproduce the crystal structure. Furthermore, both absorption and emission spectra of 1 and 2 ...

  1. Synthesis, crystal structure and properties of magnesium and ...

    Indian Academy of Sciences (India)

    2015-04-01

    Apr 1, 2015 ... 2.3 X-ray crystal structure determination. Single crystal X-ray analysis of compounds 1 and 2 was done at the Sophisticated Analytical Instrument. Table 1. Crystal data and selected refinement results for (1) and (2). Empirical formula. C16H30MgO14 (1). C16H16CaO7 (2). Formula weight (g mol−1). 470.71.

  2. Synthesis, characterization and crystal structure of new nickel ...

    Indian Academy of Sciences (India)

    Abstract. A novel nickel molybdenum complex with the 2,6-pyridine dicarboxylic acid ligand was successfully synthesized and characterized by thermogravimetric analysis and single crystal X-ray crystallography. The single-crystal X-ray data revealed that the structure is a hydrated 1-D polymer with two different Ni sites.

  3. Synthesis, Characterization, Crystal Structure and Keto-enol Kinetics

    African Journals Online (AJOL)

    A crystal structure determination of Hbth (orthorhombic, Pbca, Z=8, R=0.0290) shows asymmetrical enolization on the side of the phenyl group. The preferred enol isomer of β-diketones containing more than one aromatic moiety that crystallizes in the solid state is determined by the resonance driving force stabilization of the ...

  4. Synthesis, X-ray crystal structure, DNA binding and Nuclease activity ...

    Indian Academy of Sciences (India)

    s12039-016-1125-x. Synthesis, X-ray crystal structure, DNA binding and Nuclease activity of lanthanide(III) complexes of 2-benzoylpyridine acetylhydrazone. KARREDDULA RAJA, AKKILI SUSEELAMMA and KATREDDI HUSSAIN REDDY. ∗.

  5. Synthesis and crystal structure of [chlorobis(triphenylphospino) (p ...

    Indian Academy of Sciences (India)

    X-ray Structure of new copper(I)-thiosemicarbazone complex. 187. Table 1. Crystallographic data of complex 3. Empirical Formula. C44H38Cl2CuN3P2S. Formula Weight. 837.21. Temperature (K). 293(2). Wavelength (Å). 0.71073. Crystal system. Triclinic. Crystal size (mm). 0.3 x 0.2 x 0.2. Space group. P-1. Z, calculated. 2.

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

    Indian Academy of Sciences (India)

    Abstract. Coordination polymer of Cu(II) bridged by o-phthalic acid alone is not known. The reaction of. CuCl2.2H2O with (2-butoxycarbonyl)benzoic acid yielded three dimensional coordination polymer bridged by o-phthalic acid. X-ray crystal structure shows structure with monoclinic P21/c space group. o-Phthalic acid.

  7. 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)

  8. Synthesis and Spectroscopic, Thermal and Crystal Structure Studies ...

    African Journals Online (AJOL)

    NICO

    The salt undergoes melting followed by decomposition to give gaseous products. KEYWORDS. Hydrazine, succinic acid, hydrazinium hydrogensuccinate, crystal structure, thermal studies. 1. Introduction. Dibasic acids are known to form N2H5HA, (N2H5)2A and. N2H5HA.H2A type salts (H2A = dibasic acid) with hydrazine.

  9. Synthesis, crystal structure and characterization of new biologically ...

    Indian Academy of Sciences (India)

    Sulfonamide; Cu(II) complexes; crystal structure; oxidative DNA cleavage; cytotoxic activity. 1. Introduction. The continuous demand for new ... between the base stacks of double-stranded DNA, thus showing cytotoxic effects on several ... proteins.11,12 The toxicity of Cu(II) complexes seems to be lower than classic cancer ...

  10. Synthesis and crystal structure of trinuclear potassium(I) complex ...

    African Journals Online (AJOL)

    A furazan-based trinuclear potassium(I) complex derived from the oxy-bridged bis(gem-dinitro)furazan (OBNF) and triaminoguanidinium (TGA) units was synthesized and characterized by elemental analyses, nuclear magnetic resonance (NMR) and infrared (IR) spectroscopy. The single crystal X-ray structure of the ...

  11. Potassium and magnesium succinatouranilates – Synthesis and crystal structure

    Energy Technology Data Exchange (ETDEWEB)

    Novikov, S.A., E-mail: serg.alex.novikov@gmail.com [Samara National Research University, 443086 Samara (Russian Federation); Grigoriev, M.S. [Frumkin Institute of Physical Chemistry and Electrochemistry RAS, 119071 Moscow (Russian Federation); Serezhkina, L.B.; Serezhkin, V.N. [Samara National Research University, 443086 Samara (Russian Federation)

    2017-04-15

    Single crystal X-ray diffraction has been applied to determine the structures of two new uranyl coordination polymers: K{sub 2}[(UO{sub 2}){sub 2}(C{sub 4}H{sub 4}O{sub 4}){sub 3}] (1) and [Mg(H{sub 2}O){sub 6}] [(UO{sub 2}){sub 2}(C{sub 4}H{sub 4}O{sub 4}){sub 3}]·2H{sub 2}O (2), where C{sub 4}H{sub 4}O{sub 4}{sup 2-} is succinate anion. Crystals of 1 and 2 contain polymeric complex anions [(UO{sub 2}){sub 2}(C{sub 4}H{sub 4}O{sub 4}){sub 3}]{sup 2-} with the same A{sub 2}Q{sup 02}{sub 3} crystallochemical formula (A=UO{sub 2}{sup 2+}, Q{sup 02}=C{sub 4}O{sub 4}H{sub 4}{sup 2-}), and have layered (1) or chain (2) structure. It has been found, that conformation of succinate ions is one of the factors, which affects the structure of [(UO{sub 2}){sub 2}(C{sub 4}H{sub 4}O{sub 4}){sub 3}]{sup 2-} anions. IR spectra of these new compounds are in good agreement with crystallographic data. Topological analysis of the uranium dicarboxylates with A{sub 2}Q{sup 02}{sub 3} crystallochemical formula has shown the presence of five isomers which differ from each other in coordination sequences and / or dimensionality. - Graphical abstract: Crystal structures of two new uranium(VI) coordination polymers with succinate linkers, namely K{sub 2}[(UO{sub 2}){sub 2}(C{sub 4}H{sub 4}O{sub 4}){sub 3}] (1) and [Mg(H{sub 2}O){sub 6}][(UO{sub 2}){sub 2}(C{sub 4}H{sub 4}O{sub 4}){sub 3}]·2H{sub 2}O (2), were determined by single-crystal XRD. Crystals of studied compounds are based on 2D or 1D structural units with the same composition and crystallochemical formula. Topological isomerism in A{sub 2}Q{sup 02}{sub 3} crystallochemical group and conformations of succinate anions in uranyl complexes are under discussion. - Highlights: • Two new uranium coordination polymers were synthesized. • Their structural units have the same composition and crystallochemical formula. • In spite the same composition and CCF dimensionality of units is different. • Structural features of uranyl CPs

  12. synthesis and crystal structure of trinuclear potassium(i)

    African Journals Online (AJOL)

    DCC = distance between ring centroids; α perpendicular distance of Cg(I) from ring J;. Cg ring O7N5C4C5N6, O16N11C8C9N12 and O1 thesis and crystal structure of trinuclear potassium(I) complex. Bull. Chem. Soc. Ethiop. 2017, 31(2) anions, and connects with five adjacent OBNF2– anions through seven n bonds ...

  13. Synthesis and crystal structure of [chlorobis (triphenylphospino)(p ...

    Indian Academy of Sciences (India)

    The structure of complex 3 was confirmed by X-ray crystallography. It has been found to crystallize in the triclinic system with space group P-1 and unit cell parameters: a = 10.207(5) Å, b = 13.027(5) Å, c = 16.269(5) Å, = 100.054(5)°, = 99.228(5)° and = 97.234(5)°. This complex has distorted tetrahedral geometry with ...

  14. Synthesis and crystal structure of a trihydrate of dinuclear ...

    African Journals Online (AJOL)

    A new compound, [Cd2(C7H6N2)3(C6H4O2N)4]·3H2O (1), has been prepared under mild hydrothermal conditions and structurally characterized by single crystal X-ray diffraction. The two cadmium(II) ions are bridged by a carboxyl group from one 2-pyridinecarboxylate ligand. The thermal gravimetry (TG) data indicate ...

  15. 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.

  16. Synthesis, crystal structures and luminescence properties of two metal carboxyphosphonates

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Chaonan; Feng, Pingjing; Li, Jintang, E-mail: leejt@xmu.edu.cn; Luo, Xuetao

    2017-05-15

    Two metal carboxyphosphonates, [Co{sub 2}(OOCC{sub 5}H{sub 3}NPO{sub 3}){sub 2·}(H{sub 2}O){sub 3}] (Compound1) and Zn{sub 3}[OOCC{sub 6}H{sub 3}CH(OH)PO{sub 3}]{sub 2·}2H{sub 2}O (Compound2) were successfully synthesized under the hydrothermal reactions. In compound 1, two (Co1-NO{sub 5}) octahedra link the (CPO{sub 3}) by sharing the corner, which link the two (Co2-O{sub 6}) octahedra. From a-axis the six clusters form the layer. Each layer is linked through hydrogen bond. In compound 2, the (Zn-O{sub 4}) tetrahedron and (CPO{sub 3}) tetrahedron are corner-shared, which arrange in line. From a-axis, each line forms the columnar. The thermal and luminescence properties of these compounds were investigated. - Graphical abstract: The synthesis conditions of the two compounds and the crystal morphology. Compound 1 shows the layer and the compound 2 shows the pillared-layer. - Highlights: • Two new carboxyphosphonate ligands have been prepared. • Using the two ligands, two metal carboxyphosphonates have been synthesized. • The two MOFs may be candidates for fluorescent materials.

  17. Synthesis and Crystal Structures of N-Substituted Pyrazolines

    Directory of Open Access Journals (Sweden)

    Balladka Kunhanna Sarojini

    2013-02-01

    Full Text Available Four pyrazole compounds, 3-(4-fluorophenyl-5-phenyl-4,5-dihydro-1H-pyrazole-1-carbaldehyde (1, 5-(4-bromophenyl-3-(4-fluorophenyl-4,5-dihydro-1H-pyrazole-1-carbaldehyde (2, 1-[5-(4-chlorophenyl-3-(4-fluorophenyl-4,5-dihydro-1H-pyrazol-1-yl]ethanone (3 and 1-[3-(4-fluorophenyl-5-phenyl-4,5-dihydro-1H-pyrazol-1-yl]propan-1-one (4, have been prepared by condensing chalcones with hydrazine hydrate in the presence of aliphatic acids, namely formic acid, acetic acid and propionic acid. The structures were characterized by X-ray single crystal structure determination. The dihedral angles formed between the pyrazole and the fluoro-substituted rings are 4.64(7° in 1, 5.3(4° in 2 and 4.89(6° in 3. In 4, the corresponding angles for molecules A and molecules B are 10.53(10° and 9.78(10°, respectively.

  18. Synthesis, crystal structure and photo luminescent property of a 3D ...

    Indian Academy of Sciences (India)

    Home; Journals; Journal of Chemical Sciences; Volume 125; Issue 3. Synthesis, crystal structure and photo luminescent property of a 3D metal-organic hybrid of Cd(II) constructed by two different bridging carboxylate. Biswajit Bhattacharya Rajdip Dey Debajyoti Ghoshal. Volume 125 Issue 3 May 2013 pp 661-666 ...

  19. Synthesis and crystal structure determination of YCo Fe O 3 (= 0 ...

    Indian Academy of Sciences (India)

    The results on synthesis, crystal structure determination and calculation of crystallochemical parameters of YCo1−FeO3 ( = 0, 0.33, 0.5, 0.67 and 1) perovskites are presented in this work. The compounds within this series were synthesized by solution combustion method using two different fuels: urea and citric acid.

  20. Tubular duplex alpha-cyclodextrin triply bridged with disulfide bonds: synthesis, crystal structure and inclusion complexes

    Czech Academy of Sciences Publication Activity Database

    Krejčí, Lucie; Buděšínský, Miloš; Císařová, I.; Kraus, Tomáš

    -, č. 24 (2009), s. 3557-3559 ISSN 1359-7345 R&D Projects: GA AV ČR IAA400550810; GA ČR GA203/06/1550; GA MŠk OC 172 Institutional research plan: CEZ:AV0Z40550506 Keywords : cyclodextrines * synthesis * crystal structure Subject RIV: CC - Organic Chemistry Impact factor: 5.504, year: 2009

  1. Fixation of CO2 in air: Synthesis and crystal structure of a µ3-CO3 ...

    Indian Academy of Sciences (India)

    Unknown

    *For correspondence. Fixation of CO2 in air: Synthesis and crystal structure of a. µ3-CO3-bridged tricopper(II) compound. JHUMPA MUKHERJEEa, V BALAMURUGANa, MANINDER SINGH HUNDALb and. RABINDRANATH MUKHERJEEa,*. aDepartment of Chemistry, Indian Institute of Technology, Kanpur 208 016, India.

  2. Synthesis, crystal structure and applications of palladium thiosalicylate complexes

    Directory of Open Access Journals (Sweden)

    S.B. Moosun

    2017-05-01

    Full Text Available Three palladium thiosalicylate complexes [Pd(tb(bipy]·3H2O (1, [Pd2(tb2(bipy2]·(dtdb2 (2 and [Pd2(tb2(phen2]·dtdb·H2O (3 (bipy = bipyridine; phen = phenanthroline were prepared from the reaction of PdCl2(CH3CN2 with dithiosalicylic acid (dtdb which underwent cleavage to form thiobenzoate anion (tb in DMF/MeOH. Square planar geometries of the complexes with a N2SO coordination type were proposed on the basis of single crystal X-ray structural study. The presence of trapped and uncoordinated dtdb was observed in complexes 2 and 3. Complexes 1–3 were evaluated as catalysts for Heck coupling reactions of methyl acrylate with iodobenzene, and showed moderate activities at a very low catalyst loading. Complex 1 was found to inhibit the growth of bacteria and scavenge free radicals efficiently.

  3. Hydrothermal Synthesis and Crystal Structure of Ionic Conductive Metal Tungstates

    Energy Technology Data Exchange (ETDEWEB)

    Shimanouchi, R F; Tsuji, T; Yagi, R; Matsumoto, Y; Nishizawa, H, E-mail: rshima@kochi-u.ac.jp [Department of Natural Science, Faculty of Science, Kochi University, 2-5-1, Akebono-cho, Kochi city, KOCHI 780 (Japan)

    2011-10-29

    Trivalent ion conducting materials with the Sc{sub 2}(WO{sub 4}){sub 3}-type crystal structure, A{sub 2}(WO{sub 4}){sub 3} (A = Sc, In, Y) and solid solutions, (Sc,In){sub 2}(WO{sub 4}){sub 3} were synthesized via an autogenous hydrothermal reaction of aqueous solutions of ScCl{sub 3}, InCl{sub 3}, Y(CH{sub 3}COO){sub 3}, and H{sub 2}WO{sub 4} in a Teflon-lined mini-autoclave for 5 h at a temperature of 523 K. Fine powder samples were pressed into discs under 50 MPa and sintered at 1273 K for 10 h. The impedance measurements of sintered materials showed the dependence of electric conductivity on the size of the conducting cation. From the precise crystallographic data obtained by Rietveld refinements of solid solutions, it was considered that the change of volume of Sc(In)O{sub 6}-octahedra and WO{sub 4}-tetrahedra.

  4. Synthesis and Crystal Structures of Two New Oxaspirocyclic Compounds

    Directory of Open Access Journals (Sweden)

    Jinhe Jiang

    2016-10-01

    Full Text Available Two new oxaspirocyclic compounds, 8-(4-(dimethylaminobenzylidene-6,10-dioxaspiro[4.5]decane-7,9-dione (1 and 8-(4-hydroxybenzylidene-6,10-dioxaspiro[4.5]decane-7,9-dione (2 have been synthesized and their structures determined by single crystal X-ray crystallography. Compound 1, C17H19NO4, belongs to the monoclinic system, space group P21/c with a = 6.2554(13 Å, b = 14.605(3 Å, c = 16.265(3 Å, β = 95.97(3°, V = 1477.9(5 Å3, Z = 4, Dc = 1.354 g/cm3, F(000 = 640, μ(MoKa = 0.097 mm−1, the final R = 0.0570 and wR = 0.1667. Compound 2, C15H14O5, is also of the monoclinic system, space group P21/c with a = 10.739(2 Å, b = 18.348(4 Å, c = 6.7799(14 Å, β = 104.20(3°, V = 1295.1(5 Å3, Z = 4, Dc = 1.407 g/cm3, F(000 = 608, μ(MoKa = 0.106 mm−1, the final R = 0.0568 and wR = 0.1739. Some C–H···O intra- and intermolecular hydrogen bonds and π··· π stacking interactions are both observed in the two lattice structures. The difference between them is that one type of C–H···π supramolecular interaction (1 and one type of O–H···O intermolecular hydrogen bond (2 are observed.

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

    Science.gov (United States)

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

    2015-11-01

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

  6. 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.

  7. Template Synthesis of Noble Metal Nanocrystals with Unusual Crystal Structures and Their Catalytic Applications.

    Science.gov (United States)

    Fan, Zhanxi; Zhang, Hua

    2016-12-20

    Noble metal nanocrystals own high chemical stability, unique plasmonic and distinctive catalytic properties, making them outstanding in many applications. However, their practical applications are limited by their high cost and scarcity on the earth. One promising strategy to solve these problems is to boost their catalytic performance in order to reduce their usage amount. To realize this target, great research efforts have been devoted to the size-, composition-, shape- and/or architecture-controlled syntheses of noble metal nanocrystals during the past two decades. Impressively, recent experimental studies have revealed that the crystal structure of noble metal nanocrystals can also significantly affect their physicochemical properties, such as optical, magnetic, catalytic, mechanical, electrical and electronic properties. Therefore, besides the well-established size, composition, shape, and architecture control, the rise of crystal structure-controlled synthesis of noble metal nanocrystals will open up new opportunities to further improve their functional properties, and thus promote their potential applications in energy conversion, catalysis, biosensing, information storage, surface enhanced Raman scattering, waveguide, near-infrared photothermal therapy, controlled release, bioimaging, biomedicine, and so on. In this Account, we review the recent research progress on the crystal structure control of noble metal nanocrystals with a template synthetic approach and their crystal structure-dependent catalytic properties. We first describe the template synthetic methods, such as epitaxial growth and galvanic replacement reaction methods, in which a presynthesized noble metal nanocrystal with either new or common crystal structure is used as the template to direct the growth of unusual crystal structures of other noble metals. Significantly, the template synthetic strategy described here provides an efficient, simple and straightforward way to synthesize unusual

  8. Synthesis and crystal structure of trans-[Ni(pyzdcH)M 2 (H 2 O) 2 ...

    African Journals Online (AJOL)

    Synthesis and crystal structure of trans-[Ni(pyzdcH)M 2 (H 2 O) 2 ] based on pyrazine-2,3-dicarboxylic acid. ... Bulletin of the Chemical Society of Ethiopia ... The determined structure of the title compound C24H20Ni2N8O20 consists of the mononuclear trans-[Ni(pyzdc)2(H2O)2], (pyzdc = pyrazine-2,3- dicarboxylate).

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

    Directory of Open Access Journals (Sweden)

    Guoxiong Hua

    2016-12-01

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

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

    Indian Academy of Sciences (India)

    The fingerprint plots demonstrate that these weak non-bonding interactions are important for stabilizing the crystal packing. Keywords. Distorted trigonal pyramidal geometry; anti-conformation; steric hindrance; sql type topology; fingerprint plots. 1. Introduction. Ag(I) being soft acid is often used for coordination to soft bases ...

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

    Indian Academy of Sciences (India)

    The 2-D polymeric complex (I) has the formula [Ag(phSE)(NO3)]n, which has been crystallized ..... complex (I). Figure 4. (a) Ball-n-stick model; (b) Polyhedral representation of 2-D sheet or network as shown in ab plane of complex (I). Figure 5. (a) π-π interactions .... integration allows the separation of contribution from.

  12. Synthesis, characterization and crystal structure of new nickel ...

    Indian Academy of Sciences (India)

    School of Chemistry, University College of Science, University of Tehran, Tehran, Iran. Email: alnema@khayam.ut.ac.ir ... nation polymers and coordination complexes, is a suit- able building block for supramolecular ..... Kianpour G, Salavati-Niasari M and Emadi H 2013. Precipitation synthesis and characterization of cobalt.

  13. Synthesis, characterization, crystal structure and DNA-binding study ...

    Indian Academy of Sciences (India)

    BOLIN

    SYNOPSIS. Synthesis and characterization of four mononuclear eight coordinated cadmium(II) complexes with newly explored carboxamide derivatives and study of interaction with calf-thymus DNA are reported. The results suggest that neutral complexes 2a and 2b bind to DNA in an intercalative mode. On the other hand, ...

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

    Indian Academy of Sciences (India)

    The unit cell structure of the complex is shown in figure 3. The structure shows that the butoxy group from the ligand is lost during the formation of the complex and phthalic acid acts as a bridging ligand in the com- plex. Each Cu(II) ion is coordinated with four phtha- late ligands completing an octahedral structure with six.

  15. Synthesis and crystal structure of a wheel-shaped supramolecular ...

    Indian Academy of Sciences (India)

    elucidation of the structure of the final product. The details of the structural parameters and the non-covalent ... tra for 1 and the bulk product were recorded on a. Bruker AMX-400 FT-NMR spectrometer. ICPMS was .... certed fashion to complete the ring structure (figure 2).6. Examples of metal-based trigonal-prisms were ...

  16. short communication synthesis and crystal structure of a polymeric

    African Journals Online (AJOL)

    Preferred Customer

    Cg1 is the centroid of C1-C2-C3-C4-C5-C6. IR spectra of the complex. The infrared spectrum of the complex was consistent with the structure as determined by X-ray diffraction. Features corresponding to benzene ring puckering exist in the region between 820 and 600 cm-1. Asymmetric and symmetric C–O stretching.

  17. Synthesis and structural characterization of CsNiP crystal

    Indian Academy of Sciences (India)

    Unknown

    Fluck and Issleib 1965). However, studies of these alka- line metal phosphides gained momentum since last three decades (Johnson and Jeitschlo 1972; Barz et al 1983;. Muller et al 1983; Schnering et al 1999). In recent years, structural data of phosphides also were reported (Shan- non 1976; Jeitschlo and Braun 1977; ...

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

    Indian Academy of Sciences (India)

    The structure consists of 4-c uninodal net where Point symbol for Ag (I) ion and net is (44.62) with sql type topology. X-ray diffraction analysis and Hirshfeld surface analysis give rise to comparable results but in Hirshfeld surface analysis, twothird times more close contacts are obtained. The fingerprint plots demonstrate that ...

  19. Synthesis, Crystal structure and Characterization of a New Oxalate ...

    Indian Academy of Sciences (India)

    O, N–H...O hydrogen bonds which connect ionic entities and water molecules and also by π–π stack- ing interactions between the rings of 3,5-dimethylpyrazole cations. Hence, both coordinated and uncoordinated water molecules play an important role in the hydrogen-bonding system and stabilize the structure. Keywords.

  20. Synthesis, characterization and crystal structure of new nickel ...

    Indian Academy of Sciences (India)

    ductive, luminescent, magnetic, porous, chiral or nonlinear optical materials. The most useful strategy to construct such materials is to employ appropriate bridging ..... C and 8 h were nanoparticles with size of 35–45 nm and confirmed by TEM. Further increase in thermal decomposition time led to nanosheet-like structures.

  1. Synthesis of a mixed-valent tin nitride and considerations of its possible crystal structures.

    Science.gov (United States)

    Caskey, Christopher M; Holder, Aaron; Shulda, Sarah; Christensen, Steven T; Diercks, David; Schwartz, Craig P; Biagioni, David; Nordlund, Dennis; Kukliansky, Alon; Natan, Amir; Prendergast, David; Orvananos, Bernardo; Sun, Wenhao; Zhang, Xiuwen; Ceder, Gerbrand; Ginley, David S; Tumas, William; Perkins, John D; Stevanovic, Vladan; Pylypenko, Svitlana; Lany, Stephan; Richards, Ryan M; Zakutayev, Andriy

    2016-04-14

    Recent advances in theoretical structure prediction methods and high-throughput computational techniques are revolutionizing experimental discovery of the thermodynamically stable inorganic materials. Metastable materials represent a new frontier for these studies, since even simple binary non-ground state compounds of common elements may be awaiting discovery. However, there are significant research challenges related to non-equilibrium thin film synthesis and crystal structure predictions, such as small strained crystals in the experimental samples and energy minimization based theoretical algorithms. Here, we report on experimental synthesis and characterization, as well as theoretical first-principles calculations of a previously unreported mixed-valent binary tin nitride. Thin film experiments indicate that this novel material is N-deficient SnN with tin in the mixed ii/iv valence state and a small low-symmetry unit cell. Theoretical calculations suggest that the most likely crystal structure has the space group 2 (SG2) related to the distorted delafossite (SG166), which is nearly 0.1 eV/atom above the ground state SnN polymorph. This observation is rationalized by the structural similarity of the SnN distorted delafossite to the chemically related Sn3N4 spinel compound, which provides a fresh scientific insight into the reasons for growth of polymorphs of metastable materials. In addition to reporting on the discovery of the simple binary SnN compound, this paper illustrates a possible way of combining a wide range of advanced characterization techniques with the first-principle property calculation methods, to elucidate the most likely crystal structure of the previously unreported metastable materials.

  2. Synthesis, crystal structures and spectral characterization of chiral 4-R-1,2,4-triazoles

    Science.gov (United States)

    Gural'skiy, Il'ya A.; Reshetnikov, Viktor A.; Omelchenko, Irina V.; Szebesczyk, Agnieszka; Gumienna-Kontecka, Elzbieta; Fritsky, Igor O.

    2017-01-01

    1,2,4-triazoles attract attention as actively used medications and ligands for constructing coordination architectures. In this paper we describe four optically active 4-substituted 1,2,4-triazoles that have been prepared by Bayer's synthesis from the corresponding aliphatic chiral amines. This approach tends to be universal towards different triazoles and permits to conserve a homochirality of substrates. Novel asymmetric molecules have been characterized by spectroscopic techniques and their structures have been retrieved from the single crystal X-ray analysis. Chiro-optical studies of these heterocycles have been made by means of circular dichroism spectroscopy.

  3. Synthesis and Crystal Structure of Ethyl 2-(benzo[d]oxazol-2-yl)-5 ...

    African Journals Online (AJOL)

    dihydroisoxazole-4-carboxylate (5) was synthesized and studied by the single crystal X-ray diffraction method. Its structure was confirmed by IR, 1H and 13C NMR spectroscopy, microanalyses, and X-ray single crystal structure determination.

  4. Synthesis and crystal structure determination of Br2SeIBr ...

    Indian Academy of Sciences (India)

    Unknown

    Abstract. In this paper polyhalogen–chalcogen Br2SeIBr was synthesized and the crystal structure was de- termined by single crystal X-ray diffraction method. This compound was prepared in the temperature range. 150–50°C which was brownish-red in colour and crystallized in monoclinic crystal system and space group.

  5. Synthesis and Single Crystal X-Ray Structure Determination of 3,3',5 ...

    African Journals Online (AJOL)

    Single crystal structure determination at 100 K revealed needle-like crystals in an orthorhombic crystal system. The asymmetric unit of the cell consists of an isolated chloride ion, one half of a tetrahedral [MnCl4]2- anion, a [H2Me4bpz]2+ dication and one half of a molecule of water. Keywords: Crystal Engineering, Hydrogen ...

  6. Heteroaryl Chalcones: Design, Synthesis, X-ray Crystal Structures and Biological Evaluation

    Directory of Open Access Journals (Sweden)

    Hoong-Kun Fun

    2013-10-01

    Full Text Available Chalcone derivatives have attracted increasing attention due to their numerous pharmacological activities. Changes in their structures have displayed high degree of diversity that has proven to result in a broad spectrum of biological activities. The present study highlights the synthesis of some halogen substituted chalcones 3(a–i containing the 5-chlorothiophene moiety, their X-ray crystal structures and the evaluation of possible biological activities such as antibacterial, antifungal and reducing power abilities. The results indicate the tested compounds show a varied range of inhibition values against all the tested microbial strains. Compound 3c with a p-fluoro substituent on the phenyl ring exhibits elevated antimicrobial activity, whereas the compounds 3e and 3f displayed the least antimicrobial activities. The compounds 3d, 3e, 3f and 3i showed good ferric and cupric reducing abilities, and the compounds 3b and 3c showed the weakest reducing power in the series.

  7. Synthesis, X-ray crystal structure and theoretical calculations of antileishmanial neolignan analogues

    International Nuclear Information System (INIS)

    Nascimento, Josenaide P. do; Santos, Lourivaldo S.; Carmo, Maria Carolina L. do; Brasil, Davi S.B.; Alves, Claudio N.; Santos, Regina Helena A.; Tozzo, Erica; Ferreira, Janaina G.

    2010-01-01

    The synthesis and X-ray crystal diffraction structure of two analogues of neolignans, 2-(4-chlorophenyl)-1-phenylethanone (20) and 2-[(4-chlorophenyl)thio]-1-(3,4-dimethoxyphenyl) propan-1-one (12) is described. The compound 12 presents activity against intracellular Leishmania donovani and Leishmania amazonensis amastigotes that cause cutaneous and visceral leishmaniasis. In addition, the density functional theory (DFT) with the B3LYP hybrid functional was employed to calculate a set of molecular descriptors for nineteen synthetic analogues of neolignans with antileishmanial activities. Afterwards, the stepwise discriminant analysis was performed to investigate possible relationship between the molecular descriptors and biological activities. Through this analysis the compounds were classified into two groups active and inactive according to their degree of biological activities, and the more important properties were charges on some key atoms, electronic affinity and ClogP. (author)

  8. Synthesis, X-ray crystal structure and theoretical calculations of antileishmanial neolignan analogues

    Energy Technology Data Exchange (ETDEWEB)

    Nascimento, Josenaide P. do; Santos, Lourivaldo S.; Carmo, Maria Carolina L. do; Brasil, Davi S.B.; Alves, Claudio N., E-mail: nahum@ufpa.b [Universidade Federal do Para (UFPA), Belem, PA (Brazil). Inst. de Ciencias Exatas e Naturais; Santos, Regina Helena A.; Tozzo, Erica; Ferreira, Janaina G. [Universidade de Sao Paulo (IQSC/USP), Sao Carlos, SP (Brazil). Inst. de Quimica

    2010-07-01

    The synthesis and X-ray crystal diffraction structure of two analogues of neolignans, 2-(4-chlorophenyl)-1-phenylethanone (20) and 2-[(4-chlorophenyl)thio]-1-(3,4-dimethoxyphenyl) propan-1-one (12) is described. The compound 12 presents activity against intracellular Leishmania donovani and Leishmania amazonensis amastigotes that cause cutaneous and visceral leishmaniasis. In addition, the density functional theory (DFT) with the B3LYP hybrid functional was employed to calculate a set of molecular descriptors for nineteen synthetic analogues of neolignans with antileishmanial activities. Afterwards, the stepwise discriminant analysis was performed to investigate possible relationship between the molecular descriptors and biological activities. Through this analysis the compounds were classified into two groups active and inactive according to their degree of biological activities, and the more important properties were charges on some key atoms, electronic affinity and ClogP. (author)

  9. New bismuth borophosphate Bi4BPO10: Synthesis, crystal structure, optical and band structure analysis

    International Nuclear Information System (INIS)

    Babitsky, Nicolay A.; Leshok, Darya Y.; Mikhaleva, Natalia S.; Kuzubov, Aleksandr A.; Zhereb, Vladimir P.; Kirik, Sergei D.

    2015-01-01

    New bismuth borophosphate Bi 4 BPO 10 was obtained by spontaneous crystallization from the melt of correspondent composition at 804 °C. Crystal structure with orthorhombic lattice parameters: a = 22.5731(3) Å, b = 14.0523(2) Å, c = 5.5149(1) Å, V = 1749.34(4), Z = 8, SG Pcab was determined by X-ray powder diffraction technique. The [Bi 2 O 2 ] 2+ -layers, which are typical for bismuth oxide compounds, transform into cationic endless strips of 4 bismuth atoms width directed along the c-axis in Bi 4 BPO 10 . The strips combining stacks are separated by flat triangle [BO 3 ] 3− -anions within stacks. Neighboring stacks are separated by tetrahedral [PO 4 ] 3− -anions and shifted relatively to each other. Bismuth atoms are placed in 5–7 vertex oxygen irregular polyhedra. Bi 4 BPO 10 is stable up to 812 °C, then melts according to the peritectic law. The absorption spectrum in the range 350–700 nm was obtained and the width of the forbidden band was estimated as 3.46 eV. The band electronic structure of Bi 4 BPO 10 was modeled using DFT approach. The calculated band gap (3.56 eV) is in good agreement with the experimentally obtained data. - Graphical abstract: Display Omitted - Highlights: • New bismuth borophosphate with composition Bi 4 BPO 10 was synthesized. • The crystal structure was determined by X-ray powder diffraction technique. • Bismuth-oxygen part [Bi 4 O 3 ] 6+ forms endless strips of 4 bismuth atoms width. • Electronic structure was modeled by DFT method. • The calculated band gap (3.56 eV) is very close to the experimental one (3.46 eV)

  10. Copper coordination polymers constructed from thiazole-5-carboxylic acid: Synthesis, crystal structures, and structural transformation

    Energy Technology Data Exchange (ETDEWEB)

    Meundaeng, Natthaya; Rujiwatra, Apinpus [Department of Chemistry, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand); Prior, Timothy J., E-mail: t.prior@hull.ac.uk [Chemistry, University of Hull, Kingston upon Hull HU6 7RX (United Kingdom)

    2017-01-15

    We have successfully prepared crystals of thiazole-5-carboxylic acid (5-Htza) (L) and three new thiazole-5-carboxylate-based Cu{sup 2+} coordination polymers with different dimensionality, namely, 1D [Cu{sub 2}(5-tza){sub 2}(1,10-phenanthroline){sub 2}(NO{sub 3}){sub 2}] (1), 2D [Cu(5-tza){sub 2}(MeOH){sub 2}] (2), and 3D [Cu(5-tza){sub 2}]·H{sub 2}O (3). These have been characterized by single crystal X-ray diffraction and thermogravimetry. Interestingly, the 2D network structure of 2 can directly transform into the 3D framework of 3 upon removal of methanol molecules at room temperature. 2 can also undergo structural transformation to produce the same 2D network present in the known [Cu(5-tza){sub 2}]·1.5H{sub 2}O upon heat treatment for 2 h. This 2D network can adsorb water and convert to 3 upon exposure to air. - Highlights: • Rare examples of coordination polymers of thiazole-5-carboxylic acid were prepared. • Non-covalent interactions play a key role on the assembly of the complexes in solid state. • Structural transformation of a 2D framework to a 3D upon removal of methanol is observed.

  11. Synthesis and Crystal Structure of a New Hydrated Benzimidazolium Salt Containing Spiro Structure

    Directory of Open Access Journals (Sweden)

    Wulan Zeng

    2017-10-01

    Full Text Available A new hydrated benzimidazolium salt containing spiro structure was obtained when benzimidazole is added to ethyl alcohol of 1,5-dioxaspiro[5.5]undecane-2,4-dione and trimethoxymethane. The title compound (C19H21O8 (C7H7N2 (0.5H2O was characterized by elemental analysis, IR, UV-Vis, and single-crystal X-ray diffraction. The result shows that it belongs to the triclinic system, space group P-1, with a = 11.017(2 Å, b = 11.424(2 Å, c = 11.650(2 Å, α = 70.60(3°, β = 71.00(3°, γ = 67.64(3°, Mr = 505.51, V = 1245.2(5 Å, Z = 2, Dc = 1.348 g/cm3, F(000 = 534, μ(MoKa = 0.102 mm−1. There exist two types of hydrogen bonds in the crystal. (C19H21O8− anions and (C7H7N2+ cations are linked by N–H···O hydrogen bonds, while (C19H21O8− anions and free water are linked by O–H···O hydrogen bonds. All of the above hydrogen bonds form a one-dimensional (1D-chained structure. The 1D chains further links the molecule into a three-dimensional (3D-layered structure.

  12. Crystal Engineering: Synthesis and Structural Analysis of Coordination Polymers with Wavelike Properties

    Directory of Open Access Journals (Sweden)

    Matasebia T. Munie

    2011-10-01

    Full Text Available Supramolecular coordination polymers with wavelike structures have been synthesized by self-assembly and their structures analyzed using the sine trigonometric function. Slow evaporation of a methylene chloride-methanol solution of a 1:1 molar mixture of [M(tmhd2], where M = Co or Ni, and quinoxaline; a 1:2:1 molar mixture of [M(acac2], where M = Co or Ni, 2,2,6,6-tetramethyl-3,5-heptadione and quinoxaline; or a 1:2:1 molar mixture of [Co(acac2], dibenzoylmethane, and quinoxaline, yielded the crystalline coordination polymers. In the presence of the nitrogenous base, ligand scrambling occurs yielding the most insoluble product. The synthesis and structures of the following wavelike polymers are reported: trans-[Co(DBM2(qox]n·nH2O (2, trans-[Co(tmhd2(qox]n (3, trans-[Ni(tmhd2(qox]n (4, where DBM− = dibenzoylmethanate, tmhd− = 2,2,6,6-tetramethyl-3,5-heptadionate, and qox = quinoxaline. The wavelike structures are generated by intramolecular steric interactions and crystal packing forces between the chains. Some of the tert-butyl groups show a two-fold disorder. The sine function, φ = A sin 2πx/λ, where φ = distance (Ǻ along the polymer backbone, λ = wavelength (Ǻ, A = amplitude (Ǻ, x = distance (Ǻ along the polymer axis, provides a method to approximate and visualize the polymer structures.

  13. A robust microfluidic device for the synthesis and crystal growth of organometallic polymers with highly organized structures.

    Science.gov (United States)

    Liu, Xiao; Yi, Qiaolian; Han, Yongzhen; Liang, Zhenning; Shen, Chaohua; Zhou, Zhengyang; Sun, Jun-Liang; Li, Yizhi; Du, Wenbin; Cao, Rui

    2015-02-02

    A simple and robust microfluidic device was developed to synthesize organometallic polymers with highly organized structures. The device is compatible with organic solvents. Reactants are loaded into pairs of reservoirs connected by a 15 cm long microchannel prefilled with solvents, thus allowing long-term counter diffusion for self-assembly of organometallic polymers. The process can be monitored, and the resulting crystalline polymers are harvested without damage. The device was used to synthesize three insoluble silver acetylides as single crystals of X-ray diffraction quality. Importantly, for the first time, the single-crystal structure of silver phenylacetylide was determined. The reported approach may have wide applications, such as crystallization of membrane proteins, synthesis and crystal growth of organic, inorganic, and polymeric coordination compounds, whose single crystals cannot be obtained using traditional methods. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Synthesis and single crystal structure analysis of 3,3',5,5'-tetramethyl ...

    African Journals Online (AJOL)

    The asymmetric units consist of tetrahedral [CoCl4]2- anions and tetramethyl bipyrazolium [H2Me4bpz]2+ dications and one water molecule which are connected through N—H····Cl and N—H····O hydrogen bond networks in the crystal lattice. Keywords: Crystal structure, Hydrogen bond and crystal engineering ...

  15. Synthesis, crystal structure, physicochemical properties of hydrogen bonded supramolecular assembly of N,N-diethylanilinium-3, 5-dinitrosalicylate crystal

    Science.gov (United States)

    Rajkumar, M.; Chandramohan, A.

    2017-12-01

    An organic salt, N,N-diethylanilinium 3,5-dinitrosalicylate was synthesized and single crystals grown by employing the slow solvent evaporation solution growth technique in methanol-acetone (1:1) mixture. The electronic transitions of the salt crystal were studied by UV-Visible spectrum. The optical transmittance window and lower wavelength cut-off of grown crystal have been identified by UV-Vis-NIR studies. The FT-IR spectrum was recorded to confirm the presence of various functional groups in the grown crystal. 1H and 13C NMR spectrum were recorded to establish the molecular structure of the title crystal. Single crystal X-ray diffraction data indicated that the crystal belongs to monoclinic crystal system with P21/n space group. The thermal stability of the crystal was established by TG/DTA studies. The mechanical properties of the grown crystal were studied by Vickers' microhardness technique. The dielectric studies indicated that the dielectric constant and dielectric loss decrease exponentially with frequency at different temperatures.

  16. Inhibiting NF-κB-inducing kinase (NIK): discovery, structure-based design, synthesis, structure-activity relationship, and co-crystal structures.

    Science.gov (United States)

    Li, Kexue; McGee, Lawrence R; Fisher, Ben; Sudom, Athena; Liu, Jinsong; Rubenstein, Steven M; Anwer, Mohmed K; Cushing, Timothy D; Shin, Youngsook; Ayres, Merrill; Lee, Fei; Eksterowicz, John; Faulder, Paul; Waszkowycz, Bohdan; Plotnikova, Olga; Farrelly, Ellyn; Xiao, Shou-Hua; Chen, Guoqing; Wang, Zhulun

    2013-03-01

    The discovery, structure-based design, synthesis, and optimization of NIK inhibitors are described. Our work began with an HTS hit, imidazopyridinyl pyrimidinamine 1. We utilized homology modeling and conformational analysis to optimize the indole scaffold leading to the discovery of novel and potent conformationally constrained inhibitors such as compounds 25 and 28. Compounds 25 and 31 were co-crystallized with NIK kinase domain to provide structural insights. Copyright © 2013 Elsevier Ltd. All rights reserved.

  17. Synthesis, Crystal Structure and Anti-ischaemic Activity of (E)-1-{4 ...

    African Journals Online (AJOL)

    chloro- phenyl)prop-2-en-1-one (C28H29ClN2O3, Mr = 476.98) (5) was synthesized and studied by the single crystal X-ray diffraction method. Its structure was confirmed by 1HNMR, 13CNMR,HRMSand X-ray single crystal structure ...

  18. High-pressure synthesis, crystal structure and magnetic properties of TlCrO3 perovskite.

    Science.gov (United States)

    Yi, Wei; Matsushita, Yoshitaka; Katsuya, Yoshio; Yamaura, Kazunari; Tsujimoto, Yoshihiro; Presniakov, Igor A; Sobolev, Alexey V; Glazkova, Yana S; Lekina, Yuliya O; Tsujii, Naohito; Nimori, Shigeki; Takehana, Kanji; Imanaka, Yasutaka; Belik, Alexei A

    2015-06-21

    TlMO(3) perovskites (M(3+) = transition metals) are exceptional members of trivalent perovskite families because of the strong covalency of Tl(3+)-O bonds. Here we report on the synthesis, crystal structure and properties of TlCrO(3) investigated by Mössbauer spectroscopy, specific heat, dc/ac magnetization and dielectric measurements. TlCrO(3) perovskite is prepared under high pressure (6 GPa) and high temperature (1500 K) conditions. The crystal structure of TlCrO(3) is refined using synchrotron X-ray powder diffraction data: space group Pnma (no. 62), Z = 4 and lattice parameters a = 5.40318(1) Å, b = 7.64699(1) Å and c = 5.30196(1) Å at 293 K. No structural phase transitions are found between 5 and 300 K. TlCrO(3) crystallizes in the GdFeO(3)-type structure similar to other members of the perovskite chromite family, ACrO(3) (A(3+) = Sc, In, Y and La-Lu). The unit cell volume and Cr-O-Cr bond angles of TlCrO(3) are close to those of DyCrO(3); however, the Néel temperature of TlCrO(3) (TN≈ 89 K) is much smaller than that of DyCrO(3) and close to that of InCrO(3). Isothermal magnetization studies show that TlCrO(3) is a fully compensated antiferromagnet similar to ScCrO(3) and InCrO(3), but different from RCrO(3) (R(3+) = Y and La-Lu). Ac and dc magnetization measurements with a fine step of 0.2 K reveal the existence of two Néel temperatures with very close values at T(N2) = 87.0 K and T(N1) = 89.3 K. Magnetic anomalies near T(N2 )are suppressed by static magnetic fields and by 5% iron doping.

  19. Synthesis, crystal structure, spectral and thermal properties of 4-dimethylaminopyridinium salicylate monohydrate

    Science.gov (United States)

    Arunkumar, A.; Ramasamy, P.

    2013-06-01

    4-dimethylaminopyridinium salicylate monohydrate (DMAPSA) was synthesized and its crystal structure was determined using single crystal X-ray diffraction analysis. From the crystal structure analysis it can be inferred that the crystal belongs to monoclinic system with space group of P21/n. Investigation has been carried out to assign the vibrational frequencies of the grown crystals by FTIR spectral studies. 1H and 13C FT-NMR has been recorded to elucidate the molecular structure. The molecular mass of DMAPSA has been measured using mass spectroscopic analysis. The thermal stability and thermal decomposition of DMAPSA have been investigated by means of thermogravimetric analysis and differential thermal analysis. The melting point of crystal was observed as 172 °C by melting point apparatus. Fluorescence spectra were taken for the excitation wavelength of 240 nm.

  20. Synthesis, growth, crystal structure, optical and third order nonlinear optical properties of quinolinium derivative single crystal: PNQI

    Science.gov (United States)

    Karthigha, S.; Krishnamoorthi, C.

    2018-03-01

    An organic quinolinium derivative nonlinear optical (NLO) crystal, 1-ethyl-2-[2-(4-nitro-phenyl)-vinyl]-quinolinium iodide (PNQI) was synthesized and successfully grown by slow evaporation solution growth technique. Formation of a crystalline compound was confirmed by single crystal X-ray diffraction. The quinolinium compound PNQI crystallizes in the triclinic crystal system with a centrosymmetric space group of P-1 symmetry. The molecular structure of PNQI was confirmed by 1H NMR and 13C NMR spectral studies. The thermal properties of the crystal have been investigated by thermogravimetric (TG) and differential scanning calorimetry (DSC) studies. The optical characteristics obtained from UV-Vis-NIR spectral data were described and the cut-off wavelength observed at 506 nm. The etching study was performed to analyse the growth features of PNQI single crystal. The third order NLO properties such as nonlinear refractive index (n2), nonlinear absorption coefficient (β) and nonlinear susceptibility (χ (3)) of the crystal were investigated using Z-scan technique at 632.8 nm of Hesbnd Ne laser.

  1. Synthesis and crystal structure of the quaternary compound AgFe{sub 2}GaTe{sub 4}

    Energy Technology Data Exchange (ETDEWEB)

    Delgado, Gerzon E., E-mail: gerzon@ula.ve [Laboratorio de Cristalografía, Departamento de Química, Facultad de Ciencias, Universidad de Los Andes, Mérida 5101 (Venezuela, Bolivarian Republic of); Quintero, Eugenio; Tovar, Rafael; Grima-Gallardo, Pedro; Quintero, Miguel [Centro de Estudio de Semiconductores, Departamento de Física, Facultad de Ciencias, Universidad de Los Andes, Mérida 5101 (Venezuela, Bolivarian Republic of)

    2014-11-15

    Highlights: • New quaternary compound. • Synthesis from solid state reaction. • Crystal structure. • Rietveld refinement. - Abstract: The crystal structure of the quaternary compound AgFe{sub 2}GaTe{sub 4}, belonging to the system I–II{sub 2}–III–VI{sub 4}, was characterized by Rietveld refinement using X-ray powder diffraction data. The powder pattern was composed by 84.5% of the principal phase AgFe{sub 2}GaTe{sub 4} and 15.5% of the secondary phase FeTe. This material crystallizes with stannite structure in the tetragonal space group I-42m (N° 121), Z = 2, unit cell parameters a = 6.3409(2) Å, c = 12.0233(4) Å, V = 483.42(3) Å{sup 3}, and is isostructural with CuFe{sub 2}InSe{sub 4}.

  2. Synthesis, Crystal Structure and in vitro DNA Binding Studies of Combretastatin A-4 Analogue

    Directory of Open Access Journals (Sweden)

    Masood Ahmad Rizvi

    2015-12-01

    Full Text Available Synthesis of a novel Combretastatin A-4 analogue using Schiff’s reaction of benzil and 4-aminoantipyrine has been achieved under solvent free conditions. The structure of compound was examined spectroscopically and confirmed from single crystal diffraction studies. The synthesized Combretastatin A-4 analogue was investigated for its DNA binding ability as the plausible mechanism for its antitumor activity. The binding propensity of the synthesized compound with calf-thymus (CT DNA was monitored with absorption and emission spectrophotometric titrations. The calculations predict a binding constant of 7.24×104 for the complex of the synthesized compound with CT DNA which is comparable in magnitude to that of DNA binding of bactericidal drug enoxacin and typical intercalation indicator ethidium bromide (EB. Competitive binding studies of the synthesized compound with EB using fluorescence titration reveal that it displaces the DNA-bound EB and binds in intercalative mode which was further supported by circular dichroism (CD spectroscopy. The probable site and binding energy of the compound with DNA was further theoretically investigated by molecular docking studies. The significant DNA binding ability of the synthesized Combretastatin A4 analogue as revealed from this study could be related to the anticancer activity of the Combretastatin A4.

  3. Synthesis and structural characterization of Na2MnP2O7 crystal

    Indian Academy of Sciences (India)

    Unknown

    The starting mixture consists of manganese oxide, 85% orthophos- phoric acid and 2⋅5–5 M NaOH solution which acts as a mineralizer. Na2MnP2O7 crystals could be synthesized under the following molar ratio. Na2O : MnO : P2O5 = 3–5 : 0⋅5–0⋅75 : 12–16. The following reaction explains the synthesis of the compound.

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

  5. Synthesis, growth, structural, optical and thermal properties of a new organic salt crystal: 3-nitroanilinium trichloroacetate

    Science.gov (United States)

    Selvakumar, E.; Chandramohan, A.; Anandha Babu, G.; Ramasamy, P.

    2014-09-01

    A new organic non-linear optical salt 3-nitroanilinium trichloroacetate has been synthesized and single crystals grown by slow solvent evaporation solution growth technique at room temperature using methanol as the solvent. The 1H and 13C Nuclear magnetic resonance spectra were recorded to establish the molecular structure of the title salt. The crystal structure of the title crystal has been determined by single crystal X-ray diffraction analysis and it belongs to monoclinic crystal system with non-centrosymmetric space group P21. Fourier transform infrared spectral study has been carried out to confirm the presence of various functional groups. The optical transmittance spectrum was recorded in the range 200-2500 nm, to find the optical transmittance window and lower cut off wavelength. The thermo gravimetric and differential thermal analyses were carried out to establish the thermal stability of the title crystal. The second harmonic generation in the title crystal was confirmed by the modified Kurtz-Perry powder test employing the Nd: YAG laser as the source for infrared radiation.

  6. Synthesis and crystal structure of 1-[2-(3-ethyl-2,2 ...

    African Journals Online (AJOL)

    The title compound 1-[2-(3-ethyl-2,2-dimethylcyclobutyl)acetyl]-3-phenylthiourea has been synthesized and its crystal structure was studied. The crystal belongs to triclinic system, space group P-1, a = 10.200(2) Ǻ, b = 12.395(3) Å, c = 15.679(3) Å, α = 92.99(2)o, β = 106.00(3)o, γ = 111.95(3)o, V = 1740.4(6) Å3, Z = 2, ...

  7. The crystal structure of escherichia coli MoaB suggests a probable role in molybdenum cofactor synthesis

    International Nuclear Information System (INIS)

    Sanishvili, R.; Beasley, S.; Skarina, T; Glesne, D; Joachimiak, A; Edwards, A; Savchenko, A.; Univ. Health Network; Univ. of Toronto

    2004-01-01

    The crystal structure of Escherichia coli MoaB was determined by multiwavelength anomalous diffraction phasing and refined at 1.6 Angstrom resolution. The molecule displayed a modified Rossman fold. MoaB is assembled into a hexamer composed of two trimers. The monomers have high structural similarity with two proteins, MogA and MoeA, from the molybdenum cofactor synthesis pathway in E. Coli, as well as with domains of mammalian gephyrin and plant Cnx1, which are also involved in molybdopterin synthesis. Structural comparison between these proteins and the amino acid conservation patterns revealed a putative active site in MoaB. The structural analysis of this site allowed to advance several hypothesis which can be tested in further studies

  8. Synthesis and crystal structure of the first Sc-Nb-O-N phases

    Energy Technology Data Exchange (ETDEWEB)

    Orthmann, Steven; Lerch, Martin [Institut fuer Chemie, Technische Universitaet Berlin (Germany)

    2017-11-17

    Synthesis of phase-pure materials in the system Sc-Nb-O-N is challenging. In this contribution we report on the preparation of the first scandium niobium oxide nitrides via reaction of water-saturated gaseous ammonia or an ammonia-oxygen mixture with amorphous scandium niobium oxides. Two new phases were obtained: rutile-type ScNb{sub 4}O{sub 7}N{sub 3}, which crystallizes in space group P4{sub 2}/mnm, and an anion-deficient fluorite-type Sc{sub 2}Nb(O,N,⬜){sub 6} phase crystallizing in space group Fm anti 3m. (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  9. Constitutional Isomers of Pentahydroxy-Functionalized Pillar[5]arenes: Synthesis, Characterization, and Crystal Structures.

    Science.gov (United States)

    Al-Azemi, Talal F; Vinodh, Mickey; Alipour, Fatemeh H; Mohamod, Abdirahman A

    2017-10-20

    We herein report the preparation of constitutional isomers of pentahydroxy-functionalized pillar[5]arenes via the deprotection of their benzylated derivatives by catalytic hydrogenation. The structures of the obtained isomers were then established using single crystal X-ray diffraction. We also found that the yield distribution of the different constitutional isomers was dependent on the nature of the substitution, as revealed by HPLC analysis of the crude mixture. Finally, further characterization of the separated constitutional isomers indicated that they possess different melting points, NMR spectra, crystal structures, and stacking patterns in the solid state.

  10. Synthesis, Crystal Structure, and DFT Calculations of 1,3-Diisobutyl Thiourea

    Directory of Open Access Journals (Sweden)

    Ataf A. Altaf

    2015-01-01

    Full Text Available 1,3-Diisobutyl thiourea was synthesized and characterized by single crystal X-ray diffraction. It gives a monoclinic (α = γ = 90 and β  ≠ 90 structure with the space group P21/c. The unit cell dimensions are a = 11.5131 (4 Å, b = 9.2355 (3 Å, c = 11.3093 (5 Å, α = 90°, β = 99.569° (2, γ = 90°, V = 1185.78 (8 Å3, and Z = 4. The crystal packing is stabilized by intermolecular (N–H⋯S hydrogen bonding in the molecules. The optimized geometry and Mullikan's charges of the said molecule calculated with the help of DFT using B3LYP-6-311G model support the crystal structure.

  11. Synthesis, characterization and crystal structures of oxovanadium(V complexes derived from similar aroylhydrazone ligands

    Directory of Open Access Journals (Sweden)

    X-Z Zhang

    2015-10-01

    Full Text Available Reaction of [VO(acac2] (acac = acetylacetonate with N’-(5-chloro-2-hydroxybenzylidene-3-methoxybenzohydrazide (H2L1 and N’-(2-hydroxy-4-methoxybenzylidene-4-nitrobenzohydrazide (H2L2 in methanol affords methanol-coordinated mononuclear oxovanadium(V complexes, [VOL1(OMe(MeOH] (1 and [VOL2(OMe(MeOH] (2, respectively. The complexes were characterized by elemental analysis, FT-IR, 1H NMR and 13C NMR spectra. Crystal and molecular structures of the complexes were determined by single crystal X-ray diffraction method. Single crystal X-ray structural studies indicate that the hydrazone ligands coordinate to the VO core through enolate oxygen, phenolate oxygen and azomethine nitrogen. The V atoms in the complexes are in octahedral coordination. Thermal stabilities of the complexes have also been studied. DOI: http://dx.doi.org/10.4314/bcse.v29i3.10

  12. Na3Tb(PO4)2: Synthesis, crystal structure and greenish emitting properties

    Science.gov (United States)

    Zhao, Dan; Ma, Zhao; Liu, Bao-Zhong; Zhang, Rui-Juan; Wu, Zhi-Qiang; Wang, Jian; Duan, Pei-Gao

    2018-03-01

    A anhydrous orthoborate Na3Tb(PO4)2 has been prepared and its crystal structure was determined by X-Ray diffraction of a non-merohedral twinned single crystal. The results show that the compound crystallizes in monoclinic space group C2/c and the structure features a 3D framework containing PO4, NaO6, NaO7, NaO8 and TbO8 polyhedra. Under near-UV excitation (370 nm), Na3Tb(PO4)2 shows intense characteristic emission bands of Tb3+ (490 nm, 543 nm, 585 nm and 620 nm) with the CIE coordinate of (0.3062, 0.5901), corresponding to greenish color. The excitation spectrum covers a wide range from 340 nm to 390 nm, which indicates that phosphor Na3Tb(PO4)2 can be efficiently activated by near-UV LED ship.

  13. Synthesis, crystal structure and photo luminescent property of a 3D ...

    Indian Academy of Sciences (India)

    isonicotinate)2(suc)2]n. Empirical formula. C20H16Cd3N2O12. Formula weight. 813.58 ..... SMART and SAINT, Bruker AXS Inc, Madison, WI. 1998. 47. Sheldrick G M 1997 SHELXS-97 Program for solution of crystal structures, University of Gottingen, ...

  14. A pyrrolo-tetrathiafulvalene cage: Synthesis and X-ray crystal structure

    DEFF Research Database (Denmark)

    Nielsen, Kent A.; Jeppesen, Jan O.; Levillain, Eric

    2002-01-01

    A novel type of tetrathiafulvalene-cage 4 containing three monopyrrolo-tetrathiafulvalene units has been prepared employing a general and efficient synthetic approach. X-ray crystal structure analysis revealed that the cage is able to accommodate solvent molecules within a cavity in the solid state....

  15. Synthesis and crystal structure determination of YCo1−xFexO3 (x ...

    Indian Academy of Sciences (India)

    citric acid. It was found that iron-containing perovskites, obtained by citric acid as a fuel are of better quality and crystallinity. All the compounds crystallize in Pnma space group with Z = 4. According to the structure and the calculated crystallochemical parameters, the coordination number of Y3+ in these perovskites is 8. The.

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

    Czech Academy of Sciences Publication Activity Database

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

    2015-01-01

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

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

    Czech Academy of Sciences Publication Activity Database

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

    2016-01-01

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

  18. Synthesis and crystal structure of tischendorfite, Pd8Hg3Se9

    Czech Academy of Sciences Publication Activity Database

    Laufek, F.; Vymazalová, A.; Drábek, J.; Navrátil, Jiří; Drahokoupil, Jan

    2014-01-01

    Roč. 26, č. 1 (2014), s. 157-162 ISSN 0935-1221 Institutional support: RVO:68378271 Keywords : tischendorfite * crystal structure * Pd-Hg selenides Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.483, year: 2014

  19. Synthesis and crystal structure of lithium beryllium deuteride Li2BeD4.

    Science.gov (United States)

    Bulychev, Boris M; Shpanchenko, Roman V; Antipov, Evgeny V; Sheptyakov, Denis V; Bushmeleva, Svetlana N; Balagurov, Anatoly M

    2004-10-04

    Single-phase ternary deuteride Li(2)BeD(4) was synthesized by a high-pressure high-temperature technique from LiD and BeD(2). The crystal structure of Li(2)BeD(4) was solved from X-ray and neutron powder diffraction data. The compound crystallizes in the monoclinic space group P2(1)/c with lattice parameters a = 7.06228(9) A, b = 8.3378(1) A, c = 8.3465(1) A, beta =93.577(1) degrees, and Z = 8. Its structure contains isolated BeD(4) tetrahedra and Li atoms that are located in the structure interstices. Li(2)BeD(4) does not undergo any structural phase transitions at temperatures down to 8 K.

  20. Synthesis and crystal structure of [(NH4)(CH3H6)[UO2(SeO3)2

    International Nuclear Information System (INIS)

    Marukhnov, A.V.; Pushkin, D.V.; Serezhkina, L.B.; Peresypkina, E.V.; Virovets, A.V.

    2009-01-01

    Synthesis and X-ray structural analysis of monocrystals (NH 4 )(CN 3 H 6 ) [UO 2 (SeO 3 ) 2 ] (I) have been conducted. The compound is crystallized in triclinic lattice, a=7.0051(2), b=9.4234(3), c=9.5408(3) A, α=88.727(1), β=70.565(1), γ=77.034(1) Deg, sp. gr. P1-bar, Z=2, R=0.0224. Basic structural units of crystals I form chains of the [UO 2 (SeO 3 ) 2 ] 2- composition related to the crystallochemical group AB 2 B 11 (A=UO 2 2+ , B 2 =SeO 3 2- , B 11 =SeO 3 2- ) of uranyl complexes. Uranium-containing complexes is combined in three-dimensional frame by ammonium and guanidinium ions as well as by the systems of hydrogen bonds

  1. Acid indium strontium phosphate SrIn2[PO3(OH)]4: synthesis and crystal structure

    International Nuclear Information System (INIS)

    Rusakov, D.A.; Bobylev, A.P.; Komissarova, L.N.; Filaretov, A.A.; Danilov, V.P.

    2007-01-01

    Acid indium-strontium phosphate SrIn 2 [PO 3 (OH)] 4 is synthesized and characterized. Crystal structure and lattice parameters ate determined. In atoms in SrIn 2 [PO 3 (OH)] 4 structure are in distorted InO 6 octahedrons and form with PO 3 (OH) tetrahedrons mixed paraskeleton {In 2 [PO 3 (OH)] 4 } 3∞ 2- with emptinesses occupied by big Sr 2+ cations. The compound is thermally stable up to 400 Deg C [ru

  2. Synthesis, crystal structure, Hirshfeld surfaces analysis and anti-ischemic activity of cinnamide derivatives

    Science.gov (United States)

    Zhong, Jian-gang; Han, Jia-pei; Li, Xiao-feng; Xu, Yi; Zhong, Yan; Wu, Bin

    2018-02-01

    Two cinnamide derivatives, namely, (E)-1-(4-(bis(4-methylphenyl)- methyl)piperazin-1-yl)-3-(3,4-diethoxyphenyl)prop-2-en-1-one (5) and (E)-1-(4-(bis- (4-fluorophenyl)methyl)piperazin-1-yl)-3-(4-methoxyphenyl)prop-2-en-1-one (6), have been synthesized and characterized by IR spectra, High resolution mass spectra, 1H NMR spectra, 13C NMR spectra. The compound 5 is a novel compound and has never been reported in the literature. Their crystal structures were studied by single-crystal X-ray diffraction. They all crystallize in the monoclinic system. The single-crystal X-ray revealed that compound 5 has infinite X-shaped 1-D polymeric chains structure and compound 6 has a layered 3-D structure by intermolecular interactions. Hirshfeld surface analysis demonstrated the presence of H⋯H, O⋯H, C⋯H, F⋯H, Csbnd H⋯π and π⋯π intermolecular interactions. In addition, the MTT assay results indicated that the compounds 5 and 6 display effective activities against neurotoxicity which is induced by glutamine in PC12 cells. The in vivo experiment indicated that the compound 6 has a good protective effect on cerebral infarction.

  3. Synthesis, crystal structure, and activity of pyrazole-based inhibitors of p38 kinase.

    Science.gov (United States)

    Graneto, Matthew J; Kurumbail, Ravi G; Vazquez, Michael L; Shieh, Huey-Sheng; Pawlitz, Jennifer L; Williams, Jennifer M; Stallings, William C; Geng, Lifeng; Naraian, Ashok S; Koszyk, Francis J; Stealey, Michael A; Xu, Xiangdong D; Weier, Richard M; Hanson, Gunnar J; Mourey, Robert J; Compton, Robert P; Mnich, Stephen J; Anderson, Gary D; Monahan, Joseph B; Devraj, Rajesh

    2007-11-15

    A series of pyrazole inhibitors of p38 mitogen-activated protein (MAP) kinase were designed using a binding model based on the crystal structure of 1 (SC-102) bound to p38 enzyme. New chemistry using dithietanes was developed to assemble nitrogen-linked substituents at the 5-position of pyrazoles. Calculated log D was used in tandem with structure-based design to guide medicinal chemistry strategy and improve the in vivo activity of a series of molecules. The crystal structure of an optimized inhibitor, 4 (SC-806), in complex with p38 enzyme was obtained to confirm the hypothesis that the addition of a basic nitrogen to the molecule induces an interaction with Asp112 of p38 alpha. A compound identified from this series was efficacious in an animal model of rheumatic disease.

  4. Antimicrobial profile of some novel keto esters: Synthesis, crystal structures and structure-activity relationship studies.

    Science.gov (United States)

    Khan, Imtiaz; Saeed, Aamer; Arshad, Mohammad Ifzan; White, Jonathan Michael

    2016-01-01

    Rapid increase in bacterial resistance has become a major public concern by escalating alongside a lack of development of new anti-infective drugs. Novel remedies in the battle against multidrug-resistant bacterial strains are urgently needed. So, in this context, the present work is towards the investigation of antimicrobial efficacy of some novel keto ester derivatives, which are prepared by the condensation of substituted benzoic acids with various substituted phenacyl bromides in dimethylformamide at room temperature using triethylamine as a catalyst. The structural build-up of the target compounds was accomplished by spectroscopic techniques including FTIR, (1)H and (13)C NMR spectroscopy and mass spectrometry. The purity of the synthesized compounds was ascertained by elemental analysis. The molecular structures of compounds (4b) and (4l) were established by X-ray crystallographic analysis. The prepared analogues were evaluated for their antimicrobial activity against Gram-positive (Staphylococcus aureus, Micrococcus leuteus) and Gram-negative (Pseudomonas picketti, Salmonella setuball) bacteria and two fungal pathogenic strains (Aspergillus niger, Aspergillus flavus), respectively. Among the screened derivatives, several compounds were found to possess significant activity but (4b) and (4l) turned out to be lead molecules with remarkable antimicrobial efficacy. The structure-activity relationship analysis of this study also revealed that structural modifications on the basic skeleton affected the antimicrobial activity of the synthesized compounds.

  5. High-pressure synthesis and crystal structure of the strontium tungstate Sr3W2O9.

    Science.gov (United States)

    Urushihara, Daisuke; Asaka, Toru; Fukuda, Koichiro; Sakurai, Hiroya

    2018-02-01

    The strontium tungstate compound Sr 3 W 2 O 9 was prepared by a high-pressure synthesis technique. The crystal structure was determined by single-crystal X-ray diffraction and transmission electron microscopy. The structure was found to be a hettotype structure of the high-pressure phase of Ba 3 W 2 O 9 , which has corner-sharing octahedra with a trigonal symmetry. Sr 3 W 2 O 9 has a monoclinic unit cell of C2/c symmetry. One characteristic of the structure is the breaking of the threefold rotation symmetry existing in the high-pressure phase of Ba 3 W 2 O 9 . The substitution of Sr at the Ba site results in a significant shortening of the interlayer distances of the [AO 3 ] layers (A = Ba, Sr) and causes a distortion in the crystal structure. In Sr 3 W 2 O 9 , there is an off-centre displacement of W 6+ ions in the WO 6 octahedra. Such a displacement is also observed in the high-pressure phase of Ba 3 W 2 O 9 .

  6. Synthesis, Crystal Structure, and Chemical-Bonding Analysis of BaZn(NCN2

    Directory of Open Access Journals (Sweden)

    Alex J. Corkett

    2017-12-01

    Full Text Available The ternary carbodiimide BaZn(NCN2 was prepared by a solid-state metathesis reaction between BaF2, ZnF2, and Li2NCN in a 1:1:2 molar ratio, and its crystal structure was determined from Rietveld refinement of X-ray data. BaZn(NCN2 represents the aristotype of the LiBa2Al(NCN4 structure which is unique to carbodiimide/cyanamide chemistry and is well regarded as being constructed from ZnN4 tetrahedra, sharing edges and vertices through NCN2− units to form corrugated layers with Ba2+ in the interlayer voids. Structural anomalies in the shape of the cyanamide units are addressed via IR spectrometry and DFT calculations, which suggest the presence of slightly bent N=C=N2− carbodiimide units with C2v symmetry. Moreover, chemical-bonding analysis within the framework of crystal orbital Hamilton population (COHP reveals striking similarities between the bonding interactions in BaZn(NCN2 and SrZn(NCN2 despite their contrasting crystal structures. BaZn(NCN2 is only the second example of a ternary post-transition metal carbodiimide, and its realization paves the way for the preparation of analogues featuring divalent transition metals at the tetrahedral Zn2+ site.

  7. Synthesis and crystal structures of a novel layered silicate SSA-1 and its microporous derivatives by topotactic transformation.

    Science.gov (United States)

    Takahashi, S; Kurita, Y; Ikeda, T; Miyamoto, M; Uemiya, S; Oumi, Y

    2016-10-18

    The synthesis of a novel layered silicate SSA-1 (SSA: silicate synthesized with a quaternary amine) was achieved in the SiO 2 -H 2 O-TEAOH (TEAOH: tetraethylammonium hydroxide - as an organic structural directing agent) system. The crystal structure of SSA-1 involved two silicate layers composed of bre [10T]-type CBU (Composite Building Unit) and TEAOH in interlayers. The topotactic transformation of SSA-1 by calcination was examined, resulting in a porous material (PML-1: porous material transformed from a layered silicate) with a 108 m 2 g -1 BET surface area and 0.035 cm 3 g -1 pore volume. PML-1 is a siliceous microporous material with silanols in the framework and possesses unique properties, such as hydrophilicity, in spite of all its silica composition. The most reasonable crystal structure of PML-1 was successfully determined on the basis of the crystal structure of SSA-1 by a combination of manual modelling, PXRD pattern simulation, DFT optimization and Rietveld analysis. Additionally, an interlayer expanded siliceous zeolite SSA-1 (IEZ-SSA-1) was also successfully prepared by silylation using trichloro(methyl)silane under acidic conditions. IEZ-SSA-1 showed hydrophilicity or hydrophobicity properties by changing the functional group of the pillar part in the interlayer. Additionally, IEZ-SSA-1 showed a large gas adsorption property (537 m 2 g -1 and 0.21 cm 3 g -1 ).

  8. Synthesis, Crystal Structure, and Topology-Symmetry Analysis of a New Modification of NaIn[IO3]4

    Science.gov (United States)

    Belokoneva, E. L.; Karamysheva, A. S.; Dimitrova, O. V.; Volkov, A. S.

    2018-01-01

    Crystals of new iodate NaIn[IO3]4 were prepared by the hydrothermal synthesis. The unit cell parameters are a = 7.2672(2) Å, b = 15.2572(6) Å, c = 15.0208(6) Å, β = 101.517(3)°, sp. gr. P21/ c. The formula was determined during the structure determination and refinement of a twinned crystal based on a set of reflections from the atomic planes of the major individual. The refinement with anisotropic displacement parameters was performed for both twin components to the final R factor of 0.050. The In and Na atoms are in octahedral coordination formed by oxygen atoms. The oxygen octahedra are arranged into columns by sharing edges, and the columns are connected by isolated umbrella-like [IO3]- groups to form layers. The new structure is most similar to the isoformular iodate NaIn[IO3]4, which crystallizes in the same sp. gr. P21/ c and is structurally similar, but has a twice smaller unit cell and is characterized by another direction of the monoclinic axis. The structural similarity and difference between the two phases were studied by topologysymmetry analysis. The formation of these phases is related to different combinations of identical one-dimensional infinite chains of octahedra.

  9. Synthesis and crystal structure of (Ag,Pd).sub.22./sub.Se.sub.6./sub..

    Czech Academy of Sciences Publication Activity Database

    Laufek, F.; Vymazalová, A.; Chareev, D.A.; Kristavchuk, A.V.; Drahokoupil, Jan; Voronin, M.V.

    2013-01-01

    Roč. 28, č. 1 (2013), s. 13-17 ISSN 0885-7156 Institutional research plan: CEZ:AV0Z10100520 Keywords : (Ag,Pd) 22 Se 6 * Rietveld refinement * crystal structure * Ag-Pd-Se system * X-ray powder Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.586, year: 2013 http://journals.cambridge.org/action/displayAbstract?fromPage=online&aid=8858941

  10. Synthesis and Crystal Structure of Diaqua(1,10-Phenanthroline-N,N′)(Thiosulfato-O,S)Manganese(II). Biological Properties.

    OpenAIRE

    Brezeanu, Maria; Badea, Mikaela; Morgant, Georges; Viossat, Bernard; Bouttier, Sylvie; Fourniat, Jacky; Marinescu, Dana; Huy, Dung Nguyen

    1998-01-01

    The synthesis of diaqua(1,10-phenanthroline-N,N′)(thiosulfato-O,S)manganese(ll) [Mn(phen)(S2O3)(H2O)2] was investigated. Its structure was determined by single crystal X-ray diffraction from 2418 reflections (I > 3 σ(I)) to a final value of R = 0.047 and Rw = 0.054. Crystal data are as follows : space group P2 1; a = 10.356(3), b = 7.097(3), c = 20.316(2) Å, β = 94.29(2)°, V = 1489.1(8) , Å3, Z = 2. There are two independent title compounds in the asymetric unit. Each manganese atom has a dis...

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

  12. Perovskite-type SrTi1-xNbx(O,N)3 compounds: Synthesis, crystal structure and optical properties

    International Nuclear Information System (INIS)

    Maegli, Alexandra; Yoon, Songhak; Otal, Eugenio; Karvonen, Lassi; Mandaliev, Peter; Weidenkaff, Anke

    2011-01-01

    The synthesis, crystal structure, thermal stability and absorbance spectra of perovskite-type oxynitrides with the general formula SrTi 1-x Nb x (O,N) 3 (x=0.05, 0.10, 0.20, 0.50, 0.80, 0.90, 0.95) have been investigated. Oxide samples were prepared by a polymerized complex synthesis route and post-treated under ammonia at 850 o C for 24 h to substitute nitrogen for oxygen. Synchrotron X-ray powder diffraction (XRD) evidenced that the mixed oxide phases were all transformed into oxynitrides with perovskite-type structure during a thermal ammonolysis. SrTi 1-x Nb x (O,N) 3 with compositions x≤0.80 crystallized in a cubic and samples with x≥0.90 in a tetragonal structure. The Rietveld refinement indicated a continuous enlargement of the lattice parameters towards higher niobium content of the samples. Thermogravimetric analysis (TGA) and hotgas extraction revealed the dependence of the nitrogen incorporation upon the degree of niobium substitution. It showed that more nitrogen was detected in the samples with higher niobium content. Furthermore, TGA disclosed stability for all oxynitrides at T≤400 o C. Diffuse reflectance spectroscopy indicated a continuous decrease of the band gap's width from 3.24 eV (SrTi 0.95 Nb 0.05 (O,N) 3 ) to 1.82 eV (SrTi 0.05 Nb 0.95 (O,N) 3 ) caused by the increasing amount of nitrogen towards the latter composition. -- Graphical Abstract: The system SrTi 1-x Nb x (O,N) 3 is described and the changes in crystal structure, nitrogen content and width of the band gap are discussed. Display Omitted Research highlights: → Synthesis of SrTi 1-x Nb x (O,N) 3 perovskite-type oxynitrides via thermal ammonolysis. → Co-substitution of Nb 5+ enabled to adjust the amount nitrogen insertion. → Tuning of the optical band gap through nitrogen.→ Changes of crystal structure from cubic to tetragonal with increasing niobium content.

  13. Synthesis, crystal structure and redox properties of dihydropyrazole-bridged ferrocene-based derivatives

    Science.gov (United States)

    Li, Heng-Dong; Ma, Zai-He; Yang, Kun; Xie, Li-Li; Yuan, Yao-Feng

    2012-09-01

    Dihydropyrazole-bridged ferrocene-based derivatives were prepared by corresponding chalcones with hydrazine hydrate, then acylation with 3-(ethoxycarbonyl)propionyl chloride directly in high yields and purity. All of these compounds were characterized by MS, IR, 1H NMR, 13C NMR and elemental analysis. The relationship between the structure and redox properties was investigated based on the results of single crystal X-ray structure determinations and cyclic voltammetry. The mechanism of the electron transfer for representative compound 4b was verified by density functional theory (DFT) calculations.

  14. Synthesis and crystal structure of the γ-modifications of US2 and USe2

    International Nuclear Information System (INIS)

    Kohlmann, H.; Beck, H.P.

    1997-01-01

    We report on γ-US 2 and γ-USe 2 which may be synthesized by a presumably topotactic reaction from the corresponding U 3 X 5 compounds and elementary chalcogen. γ-USe 2 can also be prepared by a high pressure transformation of α-USe 2 at 4 GPa and 773 K. The structure of the γ phases could be determined and refined by a Rietveld procedure from powder date. They crystallize in an anti-Fe 2 P-type arrangement. Unusual features of these structures and a possible reaction mechanism for the formation of the compounds are discussed. (orig.)

  15. Synthesis and crystal structure of the coordination compound of pyridoxine with manganese sulfate

    Energy Technology Data Exchange (ETDEWEB)

    Furmanova, N. G., E-mail: furm@ns.crys.ras.ru; Verin, I. A. [Russian Academy of Sciences, Shubnikov Institute of Crystallography (Russian Federation); Shyityeva, N.; Sulaimankulov, K. S.; Berdalieva, Zh.; Resnyanskii, V. F. [National Academy of Sciences of Kyrgyzstan, Institute of Chemistry and Chemical Technology (Kyrgyzstan); Duishenbaeva, A. T. [Kyrgyz National University (Kyrgyzstan)

    2011-11-15

    The reaction of pyridoxine with manganese sulfate in an aqueous solution gave the coordination compound MnSO{sub 4} {center_dot} 2C{sub 8}H{sub 11}O{sub 3}N {center_dot} 2H{sub 2}O (I). The structure of I was determined from single-crystal X-ray diffraction data. In the centrosymmetric complex (sp. gr. P1-bar, Z = 1), the Mn atom is coordinated by two pyridoxine molecules and two water molecules, thus adopting an octahedral coordination. The sulfate anion is also at a center of symmetry and, consequently, is disordered. The pyridoxine molecules are coordinated to the metal atom through the oxygen atoms of the deprotonated hydroxyl group and the CH{sub 2}OH group that retains the hydrogen atom. The nitrogen atom is protonated in such a way that the heterocycle assumes a pyridinium character. The crystal structure also contains six water molecules of crystallization. A thermogravimetric study showed that the decomposition of I occurs in several successive steps, such as dehydration, the combustion of organic ligands, and the formation of an inorganic residue.

  16. Crystal structure and prediction.

    Science.gov (United States)

    Thakur, Tejender S; Dubey, Ritesh; Desiraju, Gautam R

    2015-04-01

    The notion of structure is central to the subject of chemistry. This review traces the development of the idea of crystal structure since the time when a crystal structure could be determined from a three-dimensional diffraction pattern and assesses the feasibility of computationally predicting an unknown crystal structure of a given molecule. Crystal structure prediction is of considerable fundamental and applied importance, and its successful execution is by no means a solved problem. The ease of crystal structure determination today has resulted in the availability of large numbers of crystal structures of higher-energy polymorphs and pseudopolymorphs. These structural libraries lead to the concept of a crystal structure landscape. A crystal structure of a compound may accordingly be taken as a data point in such a landscape.

  17. Synthesis, crystal structure, and spectral studies of 10-(2-Benzothiazolylazo)-9-phenanthrol

    Science.gov (United States)

    Davydov, V. V.; Sokol, V. I.; Polyanskaya, N. A.; Linko, R. V.; Ryabov, M. A.; Sergienko, V. S.

    2012-03-01

    10-(2-Benzothiazolylazo)-9-phenanthrol ( L) is prepared by a reaction of 2-hydrazinobenzothiazol with 9,10-phenanthrenequinone. The crystal and molecular structure of the L·CHCl3 solvate is determined by X-ray diffraction. The data of the X-ray diffraction study, as well as IR, 1H NMR, and electronic absorption spectra, indicate that in the crystal state and solutions the L molecule exists in the form of a quinohydrazone tautomer ( b) ( s-trans, cis) stabilized by the intramolecular N2-HN2…O1 hydrogen bond. The "mobile" H atom is located at the N2 atom of the azo group. The benzothiazolyl and phenanthrenequinone fragments are nearly coplanar. Spectroscopic criteria for the state of L in various media are determined based on the data of IR, 1H NMR, and electronic absorption spectroscopy and the results of the Pariser-Parr-Pople quantum-chemical calculations.

  18. Synthesis and crystal structure of novel fluorescent 1,3,4-oxadiazole-containing carboxylate ligands

    Science.gov (United States)

    Mikhailov, Igor E.; Popov, Leonid D.; Tkachev, Valery V.; Aldoshin, Sergey M.; Dushenko, Galina A.; Revinskii, Yurii V.; Minkin, Vladimir I.

    2018-04-01

    Novel chelating ligands, 3-(5-aryl-1,3,4-oxadiazol-2-yl)acrylic acids and their zinc complexes were synthesized and their spectral and luminescent properties studied. The compounds intensively (quantum efficiencies φ = 0.18-0.76) luminesce in nonpolar solvents in the blue-green region (λmaxPL = 458-504 nm) of the spectrum. Molecular and crystal structures of 3-[5-(4-dimethylaminophenyl)-1,3,4-oxadiazol-2-yl]acrylic acid were established using X-ray crystallography. In crystal, the infinite chains of the molecules lie in the parallel planes and are arranged by the "head to tail" type to provide for strong π-π stacking interactions between the layers facilitating appearance of high electron transport properties and formation of excimers.

  19. Synthesis, crystal structure, and spectral studies of 10-(2-Benzothiazolylazo)-9-phenanthrol

    International Nuclear Information System (INIS)

    Davydov, V. V.; Sokol, V. I.; Polyanskaya, N. A.; Linko, R. V.; Ryabov, M. A.; Sergienko, V. S.

    2012-01-01

    10-(2-Benzothiazolylazo)-9-phenanthrol (L) is prepared by a reaction of 2-hydrazinobenzothiazol with 9,10-phenanthrenequinone. The crystal and molecular structure of the L·CHCl 3 solvate is determined by X-ray diffraction. The data of the X-ray diffraction study, as well as IR, 1 H NMR, and electronic absorption spectra, indicate that in the crystal state and solutions the L molecule exists in the form of a quinohydrazone tautomer (b) (s-trans, cis) stabilized by the intramolecular N 2 -HN 2 …O1 hydrogen bond. The “mobile” H atom is located at the N2 atom of the azo group. The benzothiazolyl and phenanthrenequinone fragments are nearly coplanar. Spectroscopic criteria for the state of L in various media are determined based on the data of IR, 1 H NMR, and electronic absorption spectroscopy and the results of the Pariser-Parr-Pople quantum-chemical calculations.

  20. SYNTHESIS, THERMAL STUDIES AND CRYSTAL STRUCTURE OF 4-AMINOPYRIDINIUM SEMI-OXALATE HEMIHYDRATE

    Directory of Open Access Journals (Sweden)

    CECILIA CHACÓN

    2017-06-01

    Full Text Available The title compound has been synthesized by grinding in an agate mortar. Its structure was characterized by TGA-DSC studies and single-crystal X-ray diffraction. This compound crystallize in the monoclinic system with space group C2/c, Z = 4, and unit cell parameters a = 16.109(2 Å, b = 5.748(7 Å, c = 20.580(3 Å, β = 107.36(1°. The salt, C2HO4-.C5H7N+.0.5 H2O, is an ionic ensemble assisted by hydrogen bonds established between 4-aminopyridinium cations, oxalate anions and water molecules. The three components thus construct a supramolecular assembly with a three-dimensional hydrogen bonded framework.

  1. Tetraphenylphosphonium allyldithiocarbimates derived from Morita-Baylis-Hillman adducts: Synthesis, characterization, crystal structure and antifungal activity

    Science.gov (United States)

    Tavares, Eder C.; Rubinger, Mayura M. M.; Filho, Eclair V.; Oliveira, Marcelo R. L.; Piló-Veloso, Dorila; Ellena, Javier; Guilardi, Silvana; Souza, Rafael A. C.; Zambolim, Laércio

    2016-02-01

    Botrytis blight is a very destructive disease caused by Botrytis spp., infecting flowers, trees, vegetables and fruits. Twelve new compounds were prepared by the reaction of potassium N-aryl-sulfonyldithiocarbimates with Morita-Baylis-Hillman derivatives bearing phenyl and furyl groups. These are the first examples of allyldithiocarbimate anions and were isolated as tetraphenylphosphonium salts. The new compounds were characterized by HRMS, NMR and Infrared spectroscopy. Further, the structures of three allyldithiocarbimates were determined by single crystal X-ray diffraction. The compounds are isostructural and crystallize in the space group P21/c of the monoclinic system, and the allyldithiocarbimate anions present Z configuration. All the compounds were active against Botrytis cinerea. The best results were achieved with the tetraphenylphosphonium (Z)-3-(furan-2-yl)-2-(methoxycarbonyl)allyl-(4-chlorophenylsulfonyl)dithiocarbimate (IC50 38 μM).

  2. Synthesis, crystal structure, DNA binding and molecular docking studies of zinc(II) carboxylates

    Science.gov (United States)

    Muhammad, Niaz; Ikram, Muhammad; Wadood, Abdul; Rehman, Sadia; Shujah, Shaukat; Erum; Ghufran, Mehreen; Rahim, Shahnaz; Shah, Muzamil; Schulzke, Carola

    2018-02-01

    New zinc(II) carboxylate complexes [Zn(3-F-C6H4CH2COO)2]n (1), [Zn3(3-F-C6H4CH2COO)6(Phen)2] (2) and [Zn3(3-F-C6H4CH2COO)6(bipy)2] (3) were synthesized and characterized by atomic absorption, single crystal structural analysis and IR studies. Complex 1 crystallizes as a coordination polymer constituting a web of μ - η1,η1 carboxylate bridged tetrahedral zinc centers. Complexes 2 and 3 comprise trinuclear zinc centers with two terminal fivefold coordinated slightly distorted square-pyramidal and central sixfold coordinated octahedral zinc centers. The complexes were also assessed for their DNA binding ability by UV/- Vis spectroscopy and their behavior rationalized theoretically by molecular docking studies. A DNA binding study has shown groove binding interactions with the complexes.

  3. Synthesis, crystal structure, biological activity and theoretical calculations of novel isoxazole derivatives

    Science.gov (United States)

    Jin, R. Y.; Sun, X. H.; Liu, Y. F.; Long, W.; Chen, B.; Shen, S. Q.; Ma, H. X.

    2016-01-01

    Series of isoxazole derivatives were synthesized by substituted chalcones and 2-chloro-6-fluorobenzene formaldehyde oxime with 1,3-dipolar cycloaddition. The target compounds were determined by melting point, IR, 1H NMR, elemental analyses and HRMS. The crystal structure of compound 3a was detected by X-ray diffraction and it crystallizes in the triclinic space group p2(1)/c with z = 4. The molecular geometry of compound 3a was optimized using density functional theory (DFT/B3LYP) method with the 6-31G+(d,p) basis set in the ground state. From the optimized geometry of the molecule, FT-IR, FT-Raman, HOMO-LUMO and natural bond orbital (NBO) were calculated at B3LYP/6-31G+(d,p) level. Finally, the antifungal activity of the synthetic compounds were evaluated against Pythium solani, Gibberella nicotiancola, Fusarium oxysporium f.sp. niveum and Gibberella saubinetii.

  4. Divinyl BODIPY derivative: Synthesis, photophysical properties, crystal structure, photostability and bioimaging.

    Science.gov (United States)

    Yang, Liutao; Liu, Ying; Liu, Wei; Ma, Chunping; Zhang, Chun; Li, Yang

    2015-12-15

    4,4-Difluoro-3,5-bis(3,3-dimethyl-1-butenyl)-8-anthryl-4-bora-3a,4a-diaza-s-indacene (1), a symmetric fluorescent difluoroboron dipyrromethene dye, was produced in Knoevenagel reaction involving 4,4-difluoro-3,5-bis(methyl)-8-anthryl-4-bora-3a,4a-diaza-s-indacene (2) and pivaldehyde. Its crystal structure was determined by single crystal X-ray diffraction analysis, and the photophysical properties were investigated. The BODIPY 1 exhibits significant bathochromic shifts in both absorption and fluorescence spectrum compared with the BODIPY 2. In addition, the BODIPY 1 exhibited small energy gaps (2.11eV). The extensive π conjugation is responsible for their red-shifted emission. Cell imaging experiments demonstrated its potential application as a biological fluorescent probe due to its excellent imaging contrast. Copyright © 2015 Elsevier Ltd. All rights reserved.

  5. Synthesis, crystal structure, and properties of two modifications of MgB(12)C(2).

    Science.gov (United States)

    Adasch, Volker; Hess, Kai-Uwe; Ludwig, Thilo; Vojteer, Natascha; Hillebrecht, Harald

    2007-01-01

    Single crystals of two modifications of the new magnesium boride carbide MgB(12)C(2) were synthesized from the elements in a metallic melt by using tantalum ampoules. Crystals were characterized by single-crystal X-ray diffraction and electron microprobe analysis (energy-dispersive (EDX) and wavelength-dispersive (WDX) X-ray spectroscopy). Orthorhombic MgB(12)C(2) is formed in a Cu/Mg melt at 1873 K. The crystal structure of o-MgB(12)C(2) (Imma, Z=4, a=5.6133(10), b=9.828(2), c=7.9329(15) A, 574 reflections, 42 variables, R(1)(F)=0.0208, wR(2)(I)=0.0540) consists of a hexagonal primitive array of B(12) icosahedra with Mg atoms and C(2) units in trigonal-prismatic voids. Each icosahedron has six exohedral B--B and six B--C bonds. Carbon is tetrahedrally coordinated by three boron atoms and one carbon atom with a remarkably long C--C distance of 1.727 A. Monoclinic MgB(12)C(2) is formed in an Al/Mg melt at 1573 K. The structure of m-MgB(12)C(2) (C2/c, Z=4, a=7.2736(11), b=8.7768(13), c=7.2817(11) A, beta=105.33(3) degrees , 1585 reflections, 71 variables, R(1)(F)=0.0228, wR(2)(I)=0.0610) may be described as a distorted cubic close arrangement of B(12) icosahedra. Tetrahedral voids are filled by C atoms and octahedral voids are occupied by Mg atoms. The icosahedra are interconnected by four exohedral B--B bonds to linear chains and by eight interstitial C atoms to form a three-dimensional covalent network. Both compounds fulfill the electron-counting rules of Wade and Longuet-Higgins.

  6. Synthesis, crystal structure and spectroscopic properties of ethanol solvated α-Keggin heteropolymolybdate

    Science.gov (United States)

    Tümer, Ferhan; Köse, Muhammet; Tümer, Mehmet

    2017-11-01

    In this study, the ethanol solvated α-Keggin heteropolymolybdate (A) was prepared and characterized by the spectroscopic methods such as single-crystal X-ray diffraction, Uv-vis, FT-IR and photoluminescence methods. Thermal analysis of the compound (A) was performed in the 20-1000 °C range in the N2 atmosphere and electrochemical studies were carried out in the 100-1000 mV/s scan rate range. The ethanol solvated α-Keggin compound exhibits three irreversible anodic and cathodic peak potentials. The structure of the Keggin type polyoxometalate compound was solved in trigonal unit cell and R-3 space group with Rfinal value of 0.0507. The structure of the compound contains H4[SiMo12O40] molecule and three ethanol solvates. The Hirshfeld surface for H4[SiMo12O40]·3EtOH was obtained to determine the interaction sites within the crystal structure. A cyclic hydrogen bond pattern was shown by a large number of fused spots in the fingerprint plot and these hydrogen bond contacts link the other symmetry-related molecules forming a 3D hydrogen bond networks. Hydrogen bond interactions resulted in the formation of honey comb structure.

  7. Synthesis, crystal structure and magnetic properties of a novel copper(II) complex with sulfoisophthalic acid

    Science.gov (United States)

    Kurc, Teresa; Videnova-Adrabinska, Veneta; Turowska-Tyrk, Ilona; Duczmal, Marek; Jerzykiewicz, Maria

    2013-12-01

    A new Cu(II) complex, [Cu2(μ2-OH2)2(HSIP)2(H2O)6] (H3SIP = 5-sulfoisophthalic acid), has been synthesized and characterized by single crystal X-ray diffraction, EPR spectroscopy (X- (9.5 GHz) and Q-band (35 GHz)) and magnetic measurements. The solid state structure of the complex consists of coordination dimers [Cu2(μ2-OH2)2(HSIP)2(H2O)6] which are hydrogen bonded into 3D network. The neighbouring metal ions form a rare example of centrosymetric dinuclear core [Cu2(μ2-OH2)2] with equatorial - axial positions of the bridging ligands. The coordination dimers are organized into inorganic monolayers via water-sulfonate hydrogen bond intractions, and further linked in 3D structure via carboxylic-carboxylic hydrogen bond intractions. The magnetic properties and EPR spectra are discussed in terms of crystal structure features. The X- and Q-band EPR spectra exhibit fine structure signals due to S = 1 and the simulated parameters indicate small zero field splitting parameter Dexp (-0.035 cm-1) dominated by Ddip (-0.031 cm-1). A usually forbidden ΔMs = 2 line of lower intensity is observed in the half field region at about 150 mT. The susceptibility data have been analyzed using a spin-ladder model with both ferromagnetic (rungs) and antiferromagnetic (legs) coupling.

  8. Synthesis, Crystal Structure and Anti-Fatigue Effects of Some Benzamide Derivatives

    Directory of Open Access Journals (Sweden)

    Xianglong Wu

    2014-01-01

    Full Text Available A series of benzamide derivatives such as 1-(1,3-benzodioxol-5-ylcarbonyl piperidine (1-BCP were synthesized by the reaction of substituted benzoic acids with piperidine, morpholine or pyrrolidine using a novel method. The crystals of these benzamide derivatives were obtained by recrystallization. Structures of target and intermediate compounds were determined via FT-IR, 1H-NMR and elemental analysis and X-ray crystallography of select examples. The crystal structures of these compounds have potential applications to identify the binding site for allosteric modulators of the α-amino-3-hydroxy-5-methylisoxazole-4-propionic acid (AMPA receptor. The anti-fatigue effects of the benzamide derivatives in weight-loaded forced swimming mice were investigated in a swimming endurance capacity test used as an indicator of fatigue. The swimming times to exhaustion were longer in the b3, d3, and e3 groups than in the caffeine group (p < 0.05. In conclusion, b3, d3 and e3 enhanced the forced swimming capacity of mice. The mechanism of the anti-fatigue effects will be studied in the future.

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

    Science.gov (United States)

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

    2018-04-01

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

  10. Hydrothermal synthesis and crystal structure of CsFe23(HPO4)2(PO4)(H2O)

    International Nuclear Information System (INIS)

    Anisimova, N.Yu.; Ilyukhin, A.B.; Chudinova, N.N.; Serafin, M.

    2001-01-01

    The double acid iron-cesium orthophosphate CsFe 2 3 (HPO 4 ) 2 (PO 4 )(H 2 O) was prepared by hydrothermal synthesis (from the Fe 2 O 3 , Cs 2 CO 3 and H 3 PO 4 mixture at 290 Deg C during 1 h following by cooling to 25 Deg C). Its crystal structure (a = 5.021(3), b = 15.80(1), c = 13.646(8), β 94.49(4) Deg, sp. gr. P2 1 /n, Z = 4) was analyzed by X-ray diffraction. The structure is formed by the orthophosphate tetrahedrons and the FeO 6 octahedrons, the water molecule is coordinated by the iron atom [ru

  11. Synthesis and crystal structure of Pb(Bipy)2B12H12

    International Nuclear Information System (INIS)

    Lagun, V.L.; Orlova, A.M.; Katser, S.B.; Solntsev, K.A.; Kuznetsov, N.T.

    1994-01-01

    Lead complex with B 12 H 12 2- anion and 2,2' bipyridine-lead(2) dodecahydro-closo-dodecaborate di(2,2' bipyridine) is synthesized and characterized by IF, UV and NMR spectrography methods. According to roentgen-structural analysis the crystals belong to monoclinic syngony, sp.gr. C2/m,a=17.872(4), b=18.672(5), c=9.228(7)A, β=109.11(4), V=2910(2)A 3 , Z=4. The structure consists of Pb 2 (Bipy) 4 (B 12 H 12 ) 2 dimeric units. The Pb-B distances are within the limits of 3.313-3.514A. 11 refs.; 2 figs.; 2 tabs

  12. Synthesis, crystal and supramolecular structure of rac-N-acetyl-2- thiohydantoin-asparagine

    Directory of Open Access Journals (Sweden)

    Gerzon E. Delgado

    2014-05-01

    Full Text Available The title compound, C7H9N3O3S, also known as rac-N-acetyl-5-propionamide-2-thioxo-imidazolidin-4-one, crystallize in the monoclinic system with space group P21/n (Nº14, Z=4, and unit cell parameters a= 9.338 (7 Å, b= 7.545 (5 Å, c= 13.212 (10 Å, E= 97.10 (2°, V= 932.8 (12 Å3. The acetyl group and the mean plane of the ureido group form an angle of 81.0 (2°. In the supramolecular structure, the molecules are joined by N--H···O hydrogen bonds into cyclic structures with graph-set R2 2(14 and R2 2(16, forming a three-dimensional network.

  13. STUDY ON SYNTHESIS AND CRYSTAL STRUCTURE OF TETRAKIS-(μ2-ACETATO-DIHYDRATE-DICOPPER(II

    Directory of Open Access Journals (Sweden)

    LI-HUA WANG

    2015-10-01

    Full Text Available A new binuclear Cu(II complex, tetrakis-(μ2-acetato-dihydrate-dicopper (II, has been prepared by the reaction of Cu(OAc2·H2O with 2-formyl-benzenesulfonate-hydrazine in the CH3CH2OH/H2O (v : v = 1 : 1. It was characterized by elemental analysis, IR and X-ray single crystal diffraction analysis. The crystal of the Cu(II complex belongs to monoclinic, space group C2/c with a = 13.162(3 Å, b = 8.5572(17 Å, c = 13.860(3 Å, β = 117.06(3 º, V = 1390.1(5 Å3, Z = 4, Dc = 1.889 μg·m-3, μ = 3.103 mm-1, F(000 = 792, and final R1 = 0.0548, wR2 = 0.1410. Two Cu(II centers are bridged by oxygen atoms of carboxylato groups. Each Cu(II center is five-coordinated with four O donor atoms of acetate and a O donor of coordinated water molecule. The molecules form three dimensional network structures by the inaction of π-π stacking and hydrogen bonds.

  14. Synthesis, fluorescence, TGA and crystal structure of thiazolyl-pyrazolines derived from chalcones

    Science.gov (United States)

    Suwunwong, T.; Chantrapromma, S.; Fun, H.-K.

    2015-04-01

    Thiazolyl-pyrazolines 3a-3d were synthesized in a three step procedure using chalcones as starting materials and characterized by FT-IR, UV-Vis, and 1H NMR techniques. The crystal structure of compound 3a was also determined by X-ray diffraction analysis. Compound 3a crystallized out in the orthorhombic P212121 space group with the unit cell dimensions: a = 5.2106(2) Å, b = 12.4341(5) Å, c = 33.3254(13) Å, α = β = γ = 90°, V = 2159.12(15) Å3, Z = 4, D cald = 1.372 M gm-3 and F(000) = 928. Fluorescence of 3a-3d were studied in solid state and acetonitrile solution. It was found that, these compounds exhibit the green fluorescence light (506-508 nm) in both solid and solution states. The pH stability on fluorescence property and the thermal gravimetric analysis of compound 3a were specifically carried out. It was revealed that 3a shows high thermal stability up to around 250°C and presenting high stability in various pH ranges in the acetonitrilewater matrix.

  15. Synthesis, crystal and molecular structure of two biologically active aromatic sulfonamides and their hydrochloride salts

    Science.gov (United States)

    Remko, Milan; Kožíšek, Jozef; Semanová, Jana; Gregáň, Fridrich

    2010-06-01

    4-Sulfamoyl-N-(3-morpholinopropyl) benzamide (P10), N-(3-morpholinopropyl)benzene-1,4-disulfonamide (P20) and their hydrochloride salts (P11 and P22) were prepared. The X-ray molecular structure of these compounds was determined. The gas-phase structure of these drugs was computed using Becke3LYP/6-31G(d) and Becke3LYP/6-311 + G(d,p) model chemistries. The conformational behavior of these systems in water was examined using the solvation CPCM model. In the solid state, gas phase and in solution the conformations of the basic compounds P10 and P20 possess a characteristic L-shaped structure stabilized via an intramolecular hydrogen bonding system of the N sbnd H⋯N type. This hydrogen bond is not present in P11 and P22. A network of intermolecular hydrogen bonds mediated by the Cl atoms and crystal-packing forces in P11 and P22 stabilize a more extended structure in the solid state.

  16. A White-Light-Emitting Small Molecule: Synthesis, Crystal Structure, and Optical Properties

    Directory of Open Access Journals (Sweden)

    Sin-Kai Fang

    2014-01-01

    Full Text Available A white-light-emitting small molecule (1 was synthesized and characterized by single-crystal X-ray diffraction. Compound 1 undergoes an excited-state intramolecular proton transfer (ESIPT reaction, resulting in a tautomer that is in equilibrium with the normal species and exhibiting a dual emission that covers almost all of the visible spectrum, and consequently generates white light. Furthermore, the geometric structures, the frontier molecular orbitals (MOs, and the potential energy curves for 1 in the ground and the first singlet excited state were fully rationalized by density functional theory (DFT and time-dependent DFT calculations. The results show that the forward ESIPT and backward ESIPT may happen on the same timescale, enabling the excited-state equilibrium to be established.

  17. The synthesis, and crystal and magnetic structure of the iron selenide BaFe2Se3 with possible superconductivity at Tc = 11 K.

    Science.gov (United States)

    Krzton-Maziopa, A; Pomjakushina, E; Pomjakushin, V; Sheptyakov, D; Chernyshov, D; Svitlyk, V; Conder, K

    2011-10-12

    We report on the synthesis of single crystals of BaFe(2)Se(3) and study their crystal and magnetic structures by means of synchrotron single-crystal x-ray and neutron powder diffraction. The crystal structure has orthorhombic symmetry and consists of double chains of FeSe(4) edge connected tetrahedra intercalated with barium. Below 240 K, long range spin-block checkerboard antiferromagnetic order is developed. The magnetic structure is similar to one observed in A(0.8)Fe(1.6)Se(2) (A = K, Rb or Cs) superconductors. The crystals exhibit a transition to the diamagnetic state with an onset transition temperature of T(c) ∼ 11 K. Though we observe FeSe as an impurity phase (superconductor, which has T(c) ≈ 8.5 K.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-12-13

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

  19. Synthesis and crystal structure of new K and Rb selenido/tellurido ferrate cluster compounds

    Energy Technology Data Exchange (ETDEWEB)

    Stueble, Pirmin; Berroth, Angela; Roehr, Caroline [Freiburg Univ. (Germany). Inst. fuer Anorganische und Analytische Chemie

    2016-08-01

    In the course of a systematic study of alkali iron chalcogenido salts containing clusters [Fe{sub 4}Q{sub 8}] a series of new mixed-valent potassium and rubidium selenido and tellurido ferrates(II/III) was synthesized by carefully heating the pure elements enclosed in sample tubes under an argon atmosphere up to maximum temperatures of 800-900 C. Their crystal structures have been determined by means of single crystal X-ray diffraction. The mixed-valent Fe{sup II/III} tellurido ferrates A{sub 7}[Fe{sub 4}Te{sub 8}] form three different structure types. All structures contain tetramers of four edge sharing [FeTe{sub 4}] tetrahedra, which are connected by common edges to form only slightly distorted tetrahedral [Fe{sub 4}Te{sub 8}]{sup 7-} anions ('stella quadrangula') with a [Fe{sub 4}Te{sub 4}] cubane core. In all cases, these anions are surrounded by 26 alkali cations, which are located at the eight corners and the midpoints of the six faces and 12 edges of a cube. The three crystal structures can thus be described by three different packings of cuboid moieties: The monoclinic rubidium compound Rb{sub 7}[Fe{sub 4}Te{sub 8}] (space group C2/c, a = 2000.16(7), b = 897.79(3), c = 1768.12(6) pm, β = 117.4995(10) , Z = 4, R1 = 0.0296) is isotypic to the known cesium tellurido and sulfido ferrates Cs{sub 7}[Fe{sub 4}(S/Te){sub 8}]. Depending on the temperature, K{sub 7}[Fe{sub 4}Te{sub 8}] forms two different but closely related new structure types: The tetragonal r.t. modification (space group P4{sub 2}/nmc, a = 1222.25(14), c = 872.1(2) pm, Z = 2, R1 = 0.0583) crystallizes in a supergroup of the orthorhombic l.t. (100 K) form (space group Pbcn, a = 1715.5, b = 866.76(3), c = 1715.50(7) pm, Z = 4, R1 = 0.0160). In all structures, the cluster centered cubes are stacked to form columns along the short (∼ 870 pm) axis. These columns are themselves densely packed with 4 (both K compounds) and 6 (A = Rb) adjacent face-sharing columns. According to these

  20. Synthesis, crystal structure of and DFT calculations on bisglycinato-bis[p-(hydroxymethylpyridine]nickel(II

    Directory of Open Access Journals (Sweden)

    FANG FANG JIAN

    2010-09-01

    Full Text Available The main aim of this study was to investigate the relationship between mIn tA new Ni(II complex of bisglycinato-bis[p-(hydroxylmethylpy-ridine] was synthesized and characterized by elemental analysis, IR, UV–Vis spectroscopy and X-ray single crystal diffraction analysis. The thermal stability of the title complex was also determined. The complex adopts a distorted octahedral geometry and possesses inversion symmetry with the Ni(II ion as the center of inversion. Density function theory (DFT calculations of the structure, electronic absorption spectra, electron structure and natural population analysis (NPA at the B3LYP/LANL2DZ level of theory were performed. The predicted geometric parameters and electronic spectra were compared with the experimental values and they supported each other. The NPA results indicate that the electronic transitions were mainly derived from the contribution of an intra-ligand (IL transition, a ligand-to-metal charge transfer (LMCT transition and a d-d transition. The electron structure calculations suggest that the central Ni(II ion uses its 4s and 3d orbitals to form covalent bonds with coordinated N and O atoms. The calculated bond orders are also consistent with the thermal decomposition results. Based on vibrational analysis, the thermodynamic properties of the title complex were predicted and the correlative equations between these thermodynamic properties and temperature are also reported.

  1. Synthesis, crystal structure, and optical properties of the noncentrosymmetric sulfide Ce8Sb2S15

    Science.gov (United States)

    Zhao, Hua-Jun; Zhong, Xiao-Ai

    2017-07-01

    The new noncentrosymmetric sulfide Ce8Sb2S15 has been prepared at 1223 K in an evacuated silica tube. It crystallizes in the RE8Sb2S15 (RE=La, Pr, Nd) structure type with a=15.7871(6) Å, c=19.7992(16) Å, V=4934.6(5) Å3. The structure contains the discrete [SbS3]3- trigonal pyramids, which are packed in a noncentrosymmetric pseudolayer motif perpendicular to the c direction and lead to a polar structure. The Ce3+ cations and S2- anions located between them. It exhibits a weak SHG response in the IR region. UV/Vis diffuse reflectance spectroscopy study indicates that the optical gap of Ce8Sb2S15 is about 1.99 eV, showing a red shift with respect to the corresponding ternary sulfides: La8Sb2S15, which was attributed to the allowed electronic transfer from the narrow Ce 4 f level to the conduction band, mainly built from the empty Ce 5d orbitals.

  2. Alkali metal ion templated transition metal formate framework materials: synthesis, crystal structures, ion migration, and magnetism.

    Science.gov (United States)

    Eikeland, Espen; Lock, Nina; Filsø, Mette; Stingaciu, Marian; Shen, Yanbin; Overgaard, Jacob; Iversen, Bo Brummerstedt

    2014-10-06

    Four transition metal formate coordination polymers with anionic frameworks, namely, Na[Mn(HCOO)3], K[Mn(HCOO)3], Na2[Cu3(HCOO)8], and K2[Cu5(HCOO)12], were synthesized using a mild solution chemistry approach. Multitemperature single-crystal (100-300 K) and powder X-ray diffraction studies of the compounds reveal structures of large diversity ranging from cubic chiral Na-Mn formate to triclinic Na-Cu formate. The structural variety is caused by the nature of the transition metals, the alkali metal ion templation, and the versatility of the formate group, which offers metal-metal coordination through three different O-C-O bridging modes (syn-syn, syn-anti, anti-anti) in addition to metal-metal bridging via a single oxygen atom. The two manganese(II) compounds contain mononuclear, octahedrally coordinated moieties, but the three-dimensional connectivity between the manganese octahedra is very different in the two structures. The two copper frameworks, in contrast, consist of binuclear and mononuclear moieties (Na-Cu formate) and trinuclear and mononuclear moieties (K-Cu formate), respectively. Procrystal electron density analysis of the compounds indicates one-dimensional K(+)-ion conductivity in K-Mn and K-Cu, and the nature of the proposed potassium ion migration is compared with results from similar analysis on known Na(+) and K(+) ion conductors. K-Mn and Na-Mn were tested as cathode materials, but this resulted in poor reversibility due to low conductivity or structural collapse. The magnetic properties of the compounds were studied by vibrating sample magnetometric measurements, and their thermal stabilities were determined by thermogravimetric analysis and differential thermal analysis. Despite structural differences, the metal formates that contain the same transition metal have similar magnetic properties and thermal decomposition pathways, that is, the nature of the transition metal controls the compound properties.

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

    Directory of Open Access Journals (Sweden)

    Arjunsinh Rana

    2011-01-01

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

  4. Mechanochemical Synthesis and Crystal Structure of the Lidocaine-Phloroglucinol Hydrate 1:1:1 Complex

    Directory of Open Access Journals (Sweden)

    Nancy Evelyn Magaña-Vergara

    2018-03-01

    Full Text Available Molecular complexation is a strategy used to modify the physicochemical or biopharmaceutical properties of an active pharmaceutical ingredient. Solvent assisted grinding is a common method used to obtain solid complexes in the form of cocrystals. Lidocaine is a drug used as an anesthetic and for the treatment of chronic pain, which bears in its chemical structure an amide functional group able to form hydrogen bonds. Polyphenols are used as cocrystal coformers due to their ability to form O–H···X (X = O, N hydrogen bond interactions. The objective of this study was to exploit the ability of phloroglucinol to form molecular complexes with lidocaine by liquid assisted grinding. The formation of the complex was confirmed by the shift of the O–H and C=O stretching bands in the IR spectra of the polycrystalline ground powders, suggesting the formation of O–H···O=C hydrogen bonds. Hydration of the complexes also was confirmed by IR spectroscopy and by powder X-ray diffraction. The molecular structure was determined by single crystal X-ray diffraction.

  5. SYNTHESIS AND CRYSTAL STRUCTURE OF A Mg(II COMPLEX WITH 2,6-PYRIDINEDICARBOXYLIC ACID

    Directory of Open Access Journals (Sweden)

    XI-SHI TAI

    2015-05-01

    Full Text Available A Mg(II complex, [MgL·(H2O3]·2H2O (H2L = 2,6-pyridinedicarboxylic acid, has been synthesized and characterized by elemental analysis, IR and X-ray single crystal diffraction analysis. The Mg(II complex belongs to monoclinic, space group P21/n with a = 8.9318(18 Å, b = 10.002(2 Å, c = 13.290(3 Å, β = 96.86(3º, V= 1178.8(4 Å3, Z = 4, Dc = 1.575 mg·m-3, μ = 0.192 mm-1, F(000 = 584, and final R1 = 0.0349, ωR2 = 0.1212. Structural analysis shows that the Mg(II center is six-coordination with a NO5 distorted octahedral coordination environment. The Mg(II complex forms 1D chain structure by the interaction of hydrogen bonds and π-π stacking.

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

    Indian Academy of Sciences (India)

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

  7. Synthesis, crystal structure and photo luminescent property of a 3D ...

    Indian Academy of Sciences (India)

    Then the reaction mixture was placed in Teflon- lined stainless steel vessel, heated to 130. ◦. C for 2 days and then slowly cooled to room temperature over 24 h. After cooling, light yellow crystal was obtained. The crystal was filtered off and washed several times with water (yield 43%). Anal. Calc. for C20H16N2O12Cd3: C.

  8. A New 1D Chained Coordination Polymer: Synthesis, Crystal Structure, Antitumor Activity and Luminescent Property

    Directory of Open Access Journals (Sweden)

    Xi-Shi Tai

    2015-11-01

    Full Text Available A new 1D chained coordination polymer of Zn(II, {[Zn(L2(4,4′-bipy]·(H2O}n(1 (HL = N-acetyl-l-phenylalanine; 4,4′-bipy = 4,4′-bipyridine has been synthesized and characterized by elemental analysis, IR and X-ray single crystal diffraction analysis. Theresults show that each asymmetric unit of Zn(II complex belongs to monoclinic, space group P21 with a = 11.421(2 Å, b = 9.2213(17 Å, c = 15.188(3 Å,β = 106.112(3°, V = 1536.7(5 Å3, Z = 2, Dc = 1.444 g·cm−3, µ = 0.857 mm−1, F(000 = 696, and final R1 = 0.0439, ωR2 = 0.1013. The molecules form one-dimensional chained structure by its the bridging 4,4′-bipyridine ligands. The antitumor activities and luminescent properties of Zn(II coordination polymer have also been investigated.

  9. Microwave-assisted stereospecific synthesis of novel tetrahydropyran adenine isonucleosides and crystal structures determination

    Science.gov (United States)

    Silva, Fábio P. L.; Cirqueira, Marilia L.; Martins, Felipe T.; Vasconcellos, Mário L. A. A.

    2013-11-01

    We describe in this article stereospecific syntheses for new isonucleosides analogs of adenine 5-7 from tosyl derivatives 2-4 accessing by microwave irradiations (50-80%). The adenine reacts entirely at the N(9) position. Compounds 2-4 were prepared in two steps from the corresponding alcohols 1, 8 and 9 (81-92%). These tetrahydropyrans alcohols 1, 8 and 9 are achiral (Meso compounds) and were prepared in two steps with complete control of 2,4,6-cis relative configuration by Prins cyclization reaction (60-63%) preceded by the Barbier reaction between allyl bromide with benzaldehyde, 4-fluorobenzaldehyde and 2-naphthaldehyde respectively under Lewis acid conditions (96-98%). The configurations and preferential conformations of 5-7 were determined by crystal structure of 6. These novel isonucleosides 5-7 present in silico potentiality to act as GPCR ligand, kinase inhibitor and enzyme inhibitor, evaluated by Molinspiration program, consistent with the expected antiviral and anticancer bioactivities.

  10. Hydrothermal synthesis and crystal structure of a new lanthanum(III coordination polymer with fumaric acid

    Directory of Open Access Journals (Sweden)

    Hayet Anana

    2015-05-01

    Full Text Available The title compound, poly[diaquatris(μ4-but-2-enedioato(μ2-but-2-enedioic aciddilanthanum(III], [La2(C4H2O43(C4H4O4(H2O2]n, was synthesized by the reaction of lanthanum chloride pentahydrate with fumaric acid under hydrothermal conditions. The asymmetric unit comprises an LaIII cation, one and a half fumarate dianions (L2−, one a half-molecule of fumaric acid (H2L and one coordinated water molecule. Each LaIII cation has the same nine-coordinate environment and is surrounded by eight O atoms from seven distinct fumarate moieties, including one protonated fumarate unit and one water molecule in a distorted tricapped trigonal–prismatic environment. The LaO8(H2O polyhedra centres are edge-shared through three carboxylate bridges of the fumarate ligand, forming chains in three dimensions to construct the MOF. The crystal structure is stabilized by O—H...O hydrogen-bond interactions between the coordinated water molecule and the carboxylate O atoms, and also between oxygen atoms of fumaric acid

  11. 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.

  12. A new zinc(II supramolecular square: Synthesis, crystal structure, thermal behavior and luminescence

    Directory of Open Access Journals (Sweden)

    Wang Xiu-Yan

    2015-01-01

    Full Text Available A new square-shaped Zn(II complex, namely, [Zn4(L4(phen4]•6H2O (1 (L = 2-hydroxynicotinate and phen = 1,10- phenanthroline, has been synthesized under hydrothermal condition. The crystal of 1 belongs to triclinic, space group P -1 with a = 10.773(2 Å, b = 12.641(3 Å, c = 13.573(3 Å, α = 107.44(3º, β = 102.66(3º, γ = 93.89(3°, C72H56N12O18Zn4, Mr = 1638.77, V = 1702.8(6 Å3 , Z = 1, Dc = 1.598 g/cm3 , S = 1.045, μ(MoKα = 1.475 mm-1 , F(000 = 836, R = 0.0472 and wR = 0.0919. In 1, four L ligands bridge four Zn(II atoms to form a square-shaped structure, where four phen ligands are respectively located on four corners of the square. The π-π stacking interactions extend the adjacent squares into a 1D supramolecular chain. The thermal behavior of 1 has been characterized. Moreover, its solid state luminescence property has been studied at room temperature.

  13. Synthesis and Crystal Structure of Diaqua(1,10-Phenanthroline-N,N')(Thiosulfato-O,S)Manganese(II). Biological Properties.

    Science.gov (United States)

    Brezeanu, M; Badea, M; Morgant, G; Viossat, B; Bouttier, S; Fourniat, J; Marinescu, D; Huy, D N

    1998-01-01

    The synthesis of diaqua(1,10-phenanthroline-N,N')(thiosulfato-O,S)manganese(ll) [Mn(phen)(S(2)O(3))(H(2)O)(2)] was investigated. Its structure was determined by single crystal X-ray diffraction from 2418 reflections (I > 3 sigma(I)) to a final value of R = 0.047 and Rw = 0.054. Crystal data are as follows : space group P(2) (1); a = 10.356(3), b = 7.097(3), c = 20.316(2) A, beta = 94.29(2) degrees , V = 1489.1(8) , A(3), Z = 2. There are two independent title compounds in the asymetric unit. Each manganese atom has a distorted octahedral Mn(SO)N(2)O(2) geometry with the S and O atoms (from two neighbouring thiosulfate ligands) mutually trans, two N atoms from the 1,10-phenanthroline ligand and two water oxygen. The thiosulfate group behaves as a bridging ligand, connecting, through sulfur and oxygen, Mn atoms related by the binary b translation, thus forming infinite chains running parallel to this axis. Infrared and electronic spectra are reported.

  14. Synthesis and Crystal Structure of Diaqua(1,10-Phenanthroline-N,N′)(Thiosulfato-O,S)Manganese(II). Biological Properties.

    Science.gov (United States)

    Brezeanu, Maria; Badea, Mikaela; Morgant, Georges; Viossat, Bernard; Bouttier, Sylvie; Fourniat, Jacky; Marinescu, Dana

    1998-01-01

    The synthesis of diaqua(1,10-phenanthroline-N,N′)(thiosulfato-O,S)manganese(ll) [Mn(phen)(S2O3)(H2O)2] was investigated. Its structure was determined by single crystal X-ray diffraction from 2418 reflections (I > 3 σ(I)) to a final value of R = 0.047 and Rw = 0.054. Crystal data are as follows : space group P21; a = 10.356(3), b = 7.097(3), c = 20.316(2) Å, β = 94.29(2)°, V = 1489.1(8) , Å3, Z = 2. There are two independent title compounds in the asymetric unit. Each manganese atom has a distorted octahedral Mn(SO)N2O2 geometry with the S and O atoms (from two neighbouring thiosulfate ligands) mutually trans, two N atoms from the 1,10-phenanthroline ligand and two water oxygen. The thiosulfate group behaves as a bridging ligand, connecting, through sulfur and oxygen, Mn atoms related by the binary b translation, thus forming infinite chains running parallel to this axis. Infrared and electronic spectra are reported. PMID:18475862

  15. Synthesis and crystal structures of gold nanowires with Gemini surfactants as directing agents.

    Science.gov (United States)

    Xu, Feng; Hou, Hao; Gao, Zhinong

    2014-12-15

    The preparation of crystalline gold nanowires (NWs) by using gemini surfactants as directing agents through a three-step seed-mediated method is reported. Unlike the nanorods with relatively low aspect ratios (typically below 20) obtained by using cetyltrimethylammonium bromide as a directing agent, the NWs obtained in this investigation can reach up to 4.4 μm, and the largest aspect ratio is calculated to be 210. For this, each of seven different gemini surfactants are utilized as directing agents, and the length and/or aspect ratio of the NWs can be tuned by varying the hydrocarbon chain lengths of the gemini surfactants. Both single and twinned crystalline structures are elucidated by selected-area electron diffraction and high-resolution transmission electron microscopy studies. The use of gemini surfactants not only advances the synthesis of gold nanostructures, but improves the understanding of the growth mechanism for seed-mediated growth. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-11-15

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

  17. Synthesis and Crystal Structures of Two Novel O, N-Containing Spiro Compounds

    Directory of Open Access Journals (Sweden)

    Wulan Zeng

    2016-06-01

    Full Text Available Two novel O, N-containing spiro compounds, C16H16ClNO4 (1 and C16H16N2O6 (2, were prepared by reactions of monosubstituted benzenamine (substituent = –NO2, –Cl and 1,5-dioxaspiro[5.5]undecane-2,4-dione in ethanol solution of trimethoxymethane. Their structures were characterized by elemental analysis, IR, UV-Vis and single-crystal X-ray diffraction. Compound 1 is triclinic with space group P-1 and cell constants: a = 5.9448(12, b = 9.782(2, c = 13.480(3 Å, α = 100.28(3°, β = 100.66(3°, γ = 97.83(3°, Mr = 321.75, V = 746.3(3 Å3, Z = 2, Dc = 1.432 g/cm3, F(000 = 336, μ(MoKa = 0.274 mm−1, the final R = 0.0544 and wR = 0.1538. Compound 2 is monoclinic with space group P21/c and cell constants: a = 12.472(3, b = 11.856(2, c = 10.643(2 Å, β = 99.83(3°, Mr = 332.31, V = 1550.7(5 Å3, Z = 4, Dc = 1.423 g/cm3, F(000 = 696, μ(MoKa = 0.110 mm−1, the final R = 0.0444 and wR = 0.1187. In 1, there exist some intra- and inter-molecular hydrogen bonds and C–H···π supramolecular interactions, while there are still π···π stacking interactions except for some intra- and intermolecular hydrogen bonds in 2. Two compounds both form a three-dimensional network structure via above intermolecular interactions.

  18. Synthesis, X-ray crystal structure, DNA binding and Nuclease activity ...

    Indian Academy of Sciences (India)

    BPAH)₂(NO₃)(H₂O)₂] 2NO₃.H₂O (where, BPAH = 2-benzoylpyridine acetyl hydrazone), were synthesized and characterized by elemental analysis, molar conductance, IR spectroscopy and single crystal X-ray diffraction and Hirschfeld ...

  19. Synthesis, growth, structural, optical, thermal, electrical and mechanical properties of hydrogen bonded organic salt crystal: Triethylammonium-3, 5-dinitrosalicylate

    Science.gov (United States)

    Rajkumar, Madhu; Chandramohan, Angannan

    2017-04-01

    Triethylammonium-3, 5-dinitrosalicylate, an organic salt was synthesized and single crystals grown by slow solvent evaporation solution growth technique using methanol as a solvent. The presence of various functional groups and mode of vibrations has been confirmed by FT-IR spectroscopic technique. The UV-vis-NIR Spectrum was recorded in the range 200-1200 nm to find optical transmittance window and lower cut off wavelength of the title crystal. The formation of the salt and the molecular structure was confirmed by NMR spectroscopic technique. Crystal system, crystalline nature, cell parameters and hydrogen bonding interactions of the grown crystal were determined by single crystal x-ray diffraction analysis. The thermal characteristics of grown crystal were analyzed by thermo gravimetric and differential thermal analyses. Dielectric studies were carried out to study the distribution of charges within the crystal. The mechanical properties of the title crystal were studied by Vicker's microhardness technique.

  20. Synthesis and Crystal Structures of Ni(II)/(III) and Zn(II) Complexes with Schiff Base Ligands

    International Nuclear Information System (INIS)

    Koo, Bon Kweon

    2013-01-01

    Coordination polymers are of great interest due to their intriguing structural motifs and potential applications in optical, electronic, magnetic, and porous materials. The most commonly used strategy for designing such materials relies on the utilization of multidentate N- or Odonor ligands which have the capacity to bridge between metal centers to form polymeric structures. The Schiff bases with N,O,S donor atoms are an useful source as they are readily available and easily form stable complexes with most transition metal ions. Schiff bases are also important intermediates in synthesis of some bioactive compounds and are potent anti-bacterial, anti-fungal, anticancer and antiviral compounds. In this work, the Schiff bases, Hapb and Hbpb, derived from 2-acetylpyridene or 2-benzoylpyridine and benzhydrazide were taken as trifunctional (N,N,O) monobasic ligand (Scheme 1). This ligand is of important because the π-delocalization of charge and the configurational flexibility of their molecular chain can give rise to a great variety of coordination modes. Although many metal.Schiff base complexes have been reported, the 1D, 2D, and 3D networks of coordination polymers linked through the bridging of ligands such as dicyanamide, N(CN) 2 - as coligand have been little published. In the process of working to extend the dimensionality of the metal-Schiff base complexes using benzilic acid as a bridging ligand, we obtained three simple metal (II)/(III) complexes of acetylpyridine/2-benzoyl pyridine based benzhydrazide ligand. Therefore, we report here the synthesis and crystal structures of the complexes

  1. Synthesis and Crystal Structures of Ni(II)/(III) and Zn(II) Complexes with Schiff Base Ligands

    Energy Technology Data Exchange (ETDEWEB)

    Koo, Bon Kweon [Catholic Univ., of Daegu, Daegu (Korea, Republic of)

    2013-12-15

    Coordination polymers are of great interest due to their intriguing structural motifs and potential applications in optical, electronic, magnetic, and porous materials. The most commonly used strategy for designing such materials relies on the utilization of multidentate N- or Odonor ligands which have the capacity to bridge between metal centers to form polymeric structures. The Schiff bases with N,O,S donor atoms are an useful source as they are readily available and easily form stable complexes with most transition metal ions. Schiff bases are also important intermediates in synthesis of some bioactive compounds and are potent anti-bacterial, anti-fungal, anticancer and antiviral compounds. In this work, the Schiff bases, Hapb and Hbpb, derived from 2-acetylpyridene or 2-benzoylpyridine and benzhydrazide were taken as trifunctional (N,N,O) monobasic ligand (Scheme 1). This ligand is of important because the π-delocalization of charge and the configurational flexibility of their molecular chain can give rise to a great variety of coordination modes. Although many metal.Schiff base complexes have been reported, the 1D, 2D, and 3D networks of coordination polymers linked through the bridging of ligands such as dicyanamide, N(CN){sub 2}{sup -} as coligand have been little published. In the process of working to extend the dimensionality of the metal-Schiff base complexes using benzilic acid as a bridging ligand, we obtained three simple metal (II)/(III) complexes of acetylpyridine/2-benzoyl pyridine based benzhydrazide ligand. Therefore, we report here the synthesis and crystal structures of the complexes.

  2. Halide/pseudohalide complexes of cadmium(II) with benzimidazole: Synthesis, crystal structures and fluorescence properties

    Science.gov (United States)

    Zhao, Hai-Yan; Yang, Fu-Li; Li, Na; Wang, Xiao-Jing

    2017-11-01

    Two new dinuclear Cd(II) complexes, [CdL1Cl2]2·H2O (1) and [CdL1(N3)2]2·CH3OH (2) and one dicyanamide bridged one-dimensional polynuclear network [CdL1(μ1,5-dca)dca]n (3) of the potentially tridentate NNN-donor Schiff base 2-((1H-benzimidazol-2-yl-ethylimino)-methyl)pyridine (L1) and another dinucler Cd(II) complex [CdL2Cl(dca)]2 (4) of a similar NNN-donor Schiff base ligand 2-((1H-benzimidazol-2-yl-propylimino)-methyl)pyridine (L2), have been synthesized and characterized by elemental analyses, IR and single crystal X-ray crystallography. The ligands L1 and L2 are [1 + 1] condensation products of pyridine-2-carbaldehyde with 2-aminoethyl-1H-benzimidazole and 2-aminopropyl-1H-benzimidazole, respectively. In the complexes 1 and 4 the two Cd(II) centers are held together by the bridged chloride ligands, while in 2 the two Cd(II) centers are bridged by μ1,1-azide ions. Complex 3 has a one-dimensional infinite chain structure in which Cd(II) ions are bridged by single dicyanamide groups in end-to-end fashion. All the metal centers have a distorted octahedral geometry and H-bonding or π⋯π interactions are operative to bind the complex units in the solid state. Furthermore, these complexes have been investigated by thermogravimetric analyses and fluorescence spectra.

  3. New strategies for the synthesis of naphthoquinones employing Cu(II) complexes: Crystal structures and cytotoxicity

    Science.gov (United States)

    Azeredo, Nathália F. B.; Souza, Fabrícia P.; Demidoff, Felipe C.; Netto, Chaquip D.; Resende, Jackson A. L. C.; Franco, Roberto W. A.; Colepicolo, Pio; Ferreira, Ana M. C.; Fernandes, Christiane

    2018-01-01

    The syntheses, physico-chemical characterization and cytotoxicity toward three human cell lines (standard and resistant sarcoma cells, and fibroblast) of a new copper(II) complex [Cu(HBPA)(L1)Cl]·3H2O 2 are reported. Complex 2 was obtained through the reaction between the ligand stilbene-quinone (HL1) and Cu[HBPA]Cl21, where HBPA = 2-hydroxybenzyl-2pyridylmethylamine. The synthesis of HL1 was performed in high yield through Heck reaction on PEG-400. X-ray diffraction and solution studies (UV-Vis, EPR, ESI(+)-MS and ESI(+)-MS/MS) were performed for complex 2, in which the copper(II) center is coordinated to the quinone in its deprotonated form, to the ligand HBPA and to a chloro ligand. Similar reaction employing CuCl2·2H2O, instead of Cu[HBPA]Cl21 and HL1, has resulted in the obtainment of a furano-o-naphtoquinone (L2) with 99% selectivity, suggesting a new methodology to cyclize the ligand HL1. In order to obtain the analogous para-isomer (L3), and to evaluate the isomerism influence on cytotoxicity activity, a cyclization reaction of HL1 with NBS (N-bromosuccinimide) was also performed, which resulted in the obtainment of L2 (8%) and L3 (13%). X-ray diffraction studies were performed for L2 and complex 2, and the description of their structure elucidated. Results from MTT assay revealed that complex 2 is more active against sarcoma cell lines (MES-SA/Dx5 and MES-SA) than both the free ligand HL1 and complex 1, reducing cell viability to less than 50 μmol L-1. L2 was the most active in the series, presenting cytotoxicity against resistant MES-SA/Dx5 and its standard MES-SA cell line, respectively, three and ten times higher than the current drug doxorubicin.

  4. Synthesis, spectral, crystal structure, thermal behavior, antimicrobial and DNA cleavage potential of two octahedral cadmium complexes: A supramolecular structure

    Science.gov (United States)

    Montazerozohori, M.; Musavi, S. A.; Masoudiasl, A.; Naghiha, A.; Dusek, M.; Kucerakova, M.

    2015-02-01

    Two new cadmium(II) complexes with the formula of CdL2(NCS)2 and CdL2(N3)2 (in which L is 2,2-dimethyl-N,N‧-bis-(3-phenyl-allylidene)-propane-1,3-diamine) have been synthesized and characterized by elemental analysis, molar conductivity measurements, FT/IR, UV-Visible, 1H and 13C NMR spectra and X-ray studies. The crystal structure analysis of CdL2(NCS)2 indicated that it crystallizes in orthorhombic system with space group of Pbca. Two Schiff base ligands are bonded to cadmium(II) ion as N2-donor chelate. Coordination geometry around the cadmium ion was found to be partially distorted octahedron. The Cd-Nimine bond distances are found in the range of 2.363(2)-2.427(2) Å while the Cd-Nisothiocyanate bond distances are 2.287(2) Å and 2.310(2) Å. The existence of C-H⋯π and C-H⋯S interactions in the CdL2(NCS)2 crystal leads to a supramolecular structure in its network. Then cadmium complexes were screened in vitro for their antibacterial and antifungal activities against two Gram-negative and two Gram-positive bacteria and also against Candida albicans as a fungus. Moreover, the compounds were subjected for DNA-cleavage potential by gel electrophoresis method. Finally thermo-gravimetric analysis of the complexes was applied for thermal behavior studies and then some thermo-kinetics activation parameters were evaluated.

  5. Synthesis and crystal structure of Sr(2)AlH(7): a new structural type of alkaline earth aluminum hydride.

    Science.gov (United States)

    Zhang, Qing-An; Nakamura, Yumiko; Oikawa, Ken-ich; Kamiyama, Takashi; Akiba, Etsuo

    2002-12-16

    The title hydride and its deuteride were successfully synthesized. The heavy atom structure and hydrogen positions were determined respectively by X-ray powder diffraction and time-of-flight neutron powder diffraction. They crystallize with a new monoclinic structure in space group I2 (No. 5); cell parameters: a = 12.575(1) A, b = 9.799(1) A, c = 7.9911(8) A, beta = 100.270(4) degrees (hydride), a = 12.552(1) A, b = 9.7826(8) A, c = 7.9816(7) A, beta = 100.286(4) degrees (deuteride), Z = 8. Sr(2)AlH(7) is the first example that consists of isolated [AlH(6)] units and infinite one-dimensional twisted chains of edge-sharing [HSr(4)] tetrahedra along the crystallographic c axis.

  6. The RMgSn{sub 2} series of compounds (R = rare earth metal). Synthesis, crystal structure, and magnetic measurements

    Energy Technology Data Exchange (ETDEWEB)

    Solokha, Pavlo; Minetti, Riccardo; De Negri, Serena; Saccone, Adriana [Dipartimento di Chimica e Chimica Industriale, Universita di Genova (Italy); Pereira, Laura Cristina J.; Goncalves, Antonio P. [Centro de Ciencias e Tecnologias Nucleares, Instituto Superior Tecnico, EN 10, Universidade de Lisboa, Bobadela (Portugal)

    2017-06-30

    The novel isostructural series of phases RMgSn{sub 2} (R = Y, La-Nd, Sm, Gd-Tm, Lu) is presented. They were prepared by direct synthesis in an induction furnace and subsequently annealed at 500 C. Their crystal structures were determined through single-crystal X-ray diffraction analysis of the Ce representative [I anti 42m, tI32-LaMgSn{sub 2}, Z = 8, a = 0.82863(3) nm, c = 1.23129(5) nm] and confirmed by powder X-ray diffraction analysis of the other members of the series. Rietveld refinements were also performed on the homologues with R = Pr, Tm, and Y. The title phases show a unique space distribution of atoms, characterized by the presence of a Sn-Sn dumbbell distanced at around 0.29 nm. Their structures are related to those of a few binary AeTt{sub 3} (Ae = alkaline earth; Tt = Si, Ge; I4/mmm, tI32-YbSi{sub 3}) compounds that are stable at high pressure, characterized by a more complex 3D covalently bonded Tt network. Compounds CeMgSn{sub 2} and TbMgSn{sub 2} were magnetically characterized; they show paramagnetic behavior with the presence of ferromagnetic interactions, more pronounced in the case of TbMgSn{sub 2}, as suggested by the Curie-Weiss temperatures, determined in the high-temperature range, of 0.96 and 27.6 K for CeMgSn{sub 2} and TbMgSn{sub 2}, respectively. (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  7. Corrigendum to "Synthesis, crystal structure and electrochemical and DNA binding studies of oxygen bridged-copper(II) carboxylate" [J. Mol. Struct. 1093 (2015) 135-143

    Science.gov (United States)

    Iqbal, Muhammad; Ali, Saqib; Tahir, Muhammad Nawaz; Muhammad, Niaz; Shah, Naseer Ali; Sohail, Manzar; Pandarinathan, Vedapriya

    2017-04-01

    The authors regret to inform that Scheme 1 in the article titled 'Synthesis, crystal structure and electrochemical and DNA binding studies of oxygen bridged-copper(II) carboxylate' in vol. 1093 of the Journal of Molecular Structure is incorrect. The corrected scheme is as shown in this correction. This is purely a copy error. The error does not affect the conclusion in paper. The authors would like to apologize for any inconvenience caused.

  8. Nanometric solid solutions of the fluorite and perovskite type crystal structures: Synthesis and properties

    Directory of Open Access Journals (Sweden)

    Snežana Bošković

    2012-09-01

    Full Text Available In this paper a short review of our results on the synthesis of nanosized CeO2, CaMnO3 and BaCeO3 solid solutions are presented. The nanopowders were prepared by two innovative methods: self propagating room temperature synthesis (SPRT and modified glycine/nitrate procedure (MGNP. Different types of solid solutions with rare earth dopants in concentrations ranging from 0–0.25 mol% were synthesized. The reactions forming solid solutions were studied. In addition, the characteristics of prepared nanopowders, phenomena during sintering and the properties of sintered samples are discussed.

  9. Synthesis, growth, structural, optical, thermal, dielectric and mechanical studies of an organic guanidinium p-nitrophenolate crystal

    Science.gov (United States)

    Dhavamurthy, M.; Peramaiyan, G.; Mohan, R.

    2014-08-01

    Guanidinium p-nitrophenolate (GUNP), a novel organic compound, was synthesized and crystals were grown from methanol solution by a slow evaporation solution growth technique. A single crystal X-ray diffraction study elucidated the crystal structure of GUNP belonging to the orthorhombic crystal system with space group Pnma. Thermal studies revealed that the GUNP crystal is thermally stable up to 192 °C. The lower cut-off wavelength of GUNP was found to be 505 nm by UV-vis-NIR spectral studies. The luminescence properties of the GUNP crystal were investigated. The three independent tensor coefficients ε11, ε22 and ε33 of the dielectric permittivity were calculated. The mechanical properties of the grown crystal were studied by Vickers' microhardness hardness technique.

  10. 1,2,4-triazole: Synthesis, Crystal Structure, Theoretical Study, The

    Indian Academy of Sciences (India)

    71073 Å) on a Rigaku Saturn. 724. +. CCD diffractometer. A well-selected 0.22 × 0.20 ×. 0.18 mm3 yellow block crystal was used for the single crys- tal X-ray diffraction experiments. The SMART and SAINT program packages were used for data collection and inte- gration, respectively. The collected data were also corrected.

  11. Synthesis, crystal structure and magnetic properties of [Cu(mal)(abpt ...

    African Journals Online (AJOL)

    Complex 1 consist of a neutral mononuclear [Cu(mal)(abpt)(H2O)] unit and water molecule of crystallization in a distorted square pyramidal coordination sphere, while complex 2 is viewed as being made up of [Cu(sq)(abpt)2] units with the squarato ligand bridging the two copper(II) cations. Variable temperature magnetic ...

  12. Synthesis and structural characterization of Na2MnP2O7 crystal

    Indian Academy of Sciences (India)

    Unknown

    C and 50–60 bars. The starting mixture consists of manganese oxide, 85% orthophos- phoric acid and 2⋅5–5 M NaOH solution which acts as a mineralizer. Na2MnP2O7 crystals could be synthesized under the following molar ratio.

  13. SHORT COMMUNICATION SYNTHESIS AND CRYSTAL ...

    African Journals Online (AJOL)

    Preferred Customer

    -2-cyano-3-methylthioacrylyl)- N'-(substituted phenyl)ureas. Their NMR analysis, mass spectrum analysis and crystal structure have been investigated. RESULTS AND DISCUSSION. The preparation route of target compounds is shown in ...

  14. Synthesis, structural characterization, crystal structure and theoretical study of a Pd(II)-salen complex with propylene linkage

    Science.gov (United States)

    Azam, Mohammad; Al-Resayes, Saud I.; Soliman, Saied M.; Kruszynska, Agata Trzesowska; Kruszynski, Rafal

    2017-06-01

    A Pd(II)-salen complex derived from salen ligand is reported. The reported complex is investigated by microanalyses (C, H, N), ESI-MS spectrometry, FT-IR, 1H and 13C NMR and UV/Vis spectroscopic studies. In addition, crystal structure measurement study has also been carried out in order to confirm the structure of Pd(II)-salen complex. In order to explore the insights into the structural bonding of the studied complex, computational measurements has been carried out. Combined topology and NBO studies were made to explore the nature of Pdsbnd O and Pdsbnd N bonding in the complex. The natural charges showed that the transfers of the negative charge from the ligand to palladium atom is at 1.4157-1.4312 e. Atom in a molecule (AIM) analysis showed the electron density (ρ(r) > 0.1) and its Laplacian (∇2 ρ(r) > 0). These topological parameters showed that covalent bonding interactions are dominant in Pdsbnd N and Pdsbnd O bonds. However, Pdsbnd N bonds have more covalent characters than Pdsbnd O bonds, which is further confirmed by the ratio of local electron potential energy density to the local electron kinetic energy density (|V(r)|/G(r)) found to be higher for Pdsbnd N bonds (1.1683-1.1993) as compared to Pdsbnd O bonds (1.0689-1.0926). AIM and NBO reveal that shorter Pdsbnd N and Pdsbnd O bonds have higher interaction energies (Eint) and hence higher bond covalence.

  15. 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.

  16. Synthesis, crystal structure and antitumor activities of water soluble protonated salt of 20(S)-camptothecin

    Science.gov (United States)

    Lu, Wen; Wang, Yong; Wang, Luna; Zhao, Fengyi; Yang, Shilong; Xi, Chengjie; Yang, Yu; Xu, Li; Chi, Xingwei

    2018-03-01

    A water soluble camptothecin protonated salt has been synthesized; single crystals were grown by slow evaporation solution growth technique at room temperature and characterized by single crystal X-ray diffraction, FT-IR and 1H NMR. The CPT was protonated as (CPT+H+) cations, the cationic protonation occurred on the N position at pyridine group, which fromed a cation-anion compound with perchlorate ion that determined by X-Ray diffraction. Its activities against Hela (cervix), MCF-7 (breast), A549 (lung), HepG2 (liver) and HUVEC (umbilical vein, normal cell) were investigated. The toxicity of the protonated salt was slightly lower than camptothecin. IC50 values of 7.01 μM against HepG-2 cell, 8.61 μM against A549 cell, 17.82 μM against McF-7 cell, all of them are lower than the IC50 values of CPT against these cells except Hela cell.

  17. Synthesis, crystal structure and characterization of novel open framework CHA-type aluminophosphate involving a chiral diamine.

    Science.gov (United States)

    Komura, Kenichi; Horibe, Yukiko; Yajima, Hiroaki; Hiyoshi, Norihito; Ikeda, Takuji

    2016-09-27

    A highly crystalline new precursor of CHA-type zeolite AlPO 4 -34 was obtained by using an aluminophosphate gel with a chiral diamine [(S)-(+)-1-(2-pyrrolidinylmethyl)pyrrolidine; C 9 H 18 N 2 ] as an organic structure directing agent under hydrothermal synthesis conditions. This precursor (called GAM-1) was changed into the zeolite AlPO 4 -34 which had a high porosity (the Brunauer-Emmett-Teller (BET) surface area is approximately 700 m 3 g -1 ) using calcination. The GAM-1 obtained was characterized by various measurements, e.g., powder X-ray diffraction, scanning electron microscopy, and solid-state nuclear magnetic resonance spectroscopy, and so on. Structure determination from powder diffraction data revealed that the new precursor GAM-1 has triclinic symmetry [space group P1[combining macron], a = 9.16535(11) Å, b = 9.23042(11) Å, c = 9.29228(11) Å, α = 79.8243(7)°, β = 87.4593(7)°, γ = 86.5365(7)°] and the chemical formula was estimated to be: |Al 6 P 6 O 24 H 2 F 2 |(C 9 H 18 N 2 )·2.5(H 2 O). It also revealed that a two edge sharing AlO 4 F 2 octahedron with an [triple bond, length as m-dash]Al-F-Al[triple bond, length as m-dash] bridge was included in the framework. GAM-1 was transformed into AlPO 4 -34 with rhombohedral symmetry (R3[combining macron]) by elevating temperature to over 400 °C. At high temperatures, AlO 4 F 2 octahedron connectivity was changed into an AlO 4 tetrahedron. The crystal structure of the dehydrated AlPO 4 -34 changed back to a triclinic symmetry (P1) model again after rehydration in the atmosphere.

  18. Synthesis, Crystal Structure, Spectroscopic Properties and Potential Biological Activities of Salicylate‒Neocuproine Ternary Copper(II Complexes

    Directory of Open Access Journals (Sweden)

    Lenka Kucková

    2015-01-01

    Full Text Available Mixed ligand copper(II complexes containing derivatives of salicylic acid and heterocyclic ligands with nitrogen donor atoms have been the subject of various studies and reviews. In this paper, synthesis and characterization of the ternary copper(II complexes of neocuproine (2,9-dimethyl-1,10-phenanthroline, Neo and salicylate ligands (Sal are reported. In addition, the crystal structures of ([Cu(H2O(5-Cl-Sal(Neo] (1, [Cu(μ-Sal(Neo]2 (2, Cu2(μ-5-Cl-Sal(5-Cl-HSal2(Neo2]·EtOH (3 were determined. In order to compare structural and biological properties of the prepared complexes, spectroscopic and biological studies were performed. Results of X-ray diffraction show that prepared complexes form three types of crystal structures in a given system: monomeric, dimeric and dinuclear complex. The preliminary study on the DNA cleavage activity has shown that the complexes under study behave as the chemical nucleases in the presence of added hydrogen peroxide with slight differences in the activity (1 > 2 > 3. The complexes 1 and 2 exhibited nuclease activity itself indicating the interaction of complexes with the DNA. It has been proposed that the enhanced destructive effect of the complexes 1 and 2 on the DNA is a result of two possible mechanisms of action: (i the conversion of closed circular DNA (form I to the nicked DNA (form II caused by the copper complex itself and (ii damage of DNA by Reactive Oxygen Species (ROS—products of the interaction of copper with hydrogen peroxide by means of Fenton reaction (hydroxyl radicals. Thus the biological activity of the prepared Cu(II complexes containing derivatives of salicylic acid and phenanthroline molecules is substantiated by two independent mechanisms. While derivatives of salicylic acids in the coordination sphere of copper complexes are responsible for radical-scavenging activity (predominantly towards superoxide radical anion, the presence of chelating ligand 2,9-dimethyl-1,10-phenanthroline

  19. 2.2.2. Synthesis, crystal structure and biological activity of triphenyltin 4-acetylphenolate

    Directory of Open Access Journals (Sweden)

    Zhikun Liua, Yunsai Donga, Xiaoliang Zhengb, You Yua, Laijin Tiana,*

    2015-03-01

    Full Text Available Abs t ract : Tr i ph en yl t in 4-a cet yl ph en ol at e, 4- CH3COC6H4OSnPh3 (1, has been synthesized and characterized by elemental analysis, IR, NMR (1H, 13C and 119Sn spectra, and X-ray single crystal diffraction. Compound  1 possesses a trans-C3SnO2 trigonal bipyramidal geometry with the axial positions occupied by the phenolate oxygen and carbonyl oxygen of an adjacent molecule and form an one-dimensional infinite chain. Bioassay results have shown that the compound has good in vitro anti-bacterial and anti-tumor activities. Supporting information: X-Ray (CIF file

  20. Synthesis, crystal structure and thermodynamic properties of a new praseodymium Schiff-base complex

    Energy Technology Data Exchange (ETDEWEB)

    Li, Chuan-Hua, E-mail: lichuanhua0526@126.com [School of Chemistry and Chemical Engineering, Central South University, Changsha 410083, Hunan (China); Hunan Provincial Key Laboratory of Xiangnan Rare-Precious Metals Compounds and Applications, Department of Chemistry and Life Science, Xiangnan University, Chenzhou 423000, Hunan (China); Song, Xiang-Zhi, E-mail: xzsong@csu.edu.cn [School of Chemistry and Chemical Engineering, Central South University, Changsha 410083, Hunan (China); Jiang, Jian-Hong [Hunan Provincial Key Laboratory of Xiangnan Rare-Precious Metals Compounds and Applications, Department of Chemistry and Life Science, Xiangnan University, Chenzhou 423000, Hunan (China); Gu, Hui-Wen [State Key Laboratory of Chemo/Biosensing and Chemometrics, College of Chemistry and Chemical Engineering, Hunan University, Changsha 410082, Hunan (China); Tao, Li-Ming; Yang, Ping; Li, Xu; Xiao, Sheng-Xiong; Yao, Fei-Hong; Liu, Wen-Qi; Xie, Jin-Qi; Peng, Meng-Na; Pan, Lan; Wu, Xi-Bin; Jiang, Chao; Wang, Song; Xu, Man-Fen [Hunan Provincial Key Laboratory of Xiangnan Rare-Precious Metals Compounds and Applications, Department of Chemistry and Life Science, Xiangnan University, Chenzhou 423000, Hunan (China); Li, Qiang-Guo, E-mail: liqiangguo@163.com [Hunan Provincial Key Laboratory of Xiangnan Rare-Precious Metals Compounds and Applications, Department of Chemistry and Life Science, Xiangnan University, Chenzhou 423000, Hunan (China)

    2014-04-01

    Highlights: • A new mononuclear Schiff base praseodymium complex was synthesized. • Based on Hess's law, thermochemical cycles of two reactions were designed. • The dissolution enthalpies were measured by a solution–reaction calorimeter. • The standard molar enthalpy of formation of the complex was calculated. - Abstract: The title complex [Pr(H{sub 2}vanen)(NO{sub 3}){sub 2}(H{sub 2}O){sub 2}·NO{sub 3}] was synthesized reacting of Valen Schiff-base ligand [H{sub 2}vanen = N,N′-ethylene-bis(3-methoxysalicylideneimine)] and Pr(NO{sub 3}){sub 3}·6H{sub 2}O in ethanol at 60 °C. The complex was crystallized in the monoclinic crystal system with space group P21/c. The coordination polyhedron of Pr(III) ion was consisted of two bidentate nitrate ions, two molecules of water and one ligand which coordinated through oxygen atoms of the two phenolic and methoxy groups. After designing two reasonable thermochemical cycles according to Hess's law, the calorimetric experiments were conducted using isoperibol solution–reaction calorimeter at a constant temperature of 298.15 K. The standard molar enthalpy changes of two reactions were determined to be Δ{sub r}H{sub m}{sup θ}(1a)=−(51.94±1.26) kJ mol{sup −1} and Δ{sub r}H{sub m}{sup θ}(1b)=−(8.62±1.34) kJ mol{sup −1}. Then the standard molar enthalpies of formation of the ligand and the title complex were calculated to be Δ{sub f}H{sub m}{sup θ} [H{sub 2}vanen(s), 298.15 K] = −(517.75 ± 2.36) kJ mol{sup −1} and Δ{sub f}H{sub m}{sup θ} [Pr(H{sub 2}vanen)(NO{sub 3}){sub 2}(H{sub 2}O){sub 2}·NO{sub 3} (s), 298.15 K] = −(2454.8 ± 2.7) kJ mol{sup −1}, respectively. The rationality of two thermochemical cycles was verified by UV spectra and refractive indexes.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-08-03

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

  2. Synthesis, crystal structure, characterization and antifungal activity of pyrazolo[1,5-a]pyrimidines derivatives

    Science.gov (United States)

    Zhang, Jin; Peng, Ju-Fang; Wang, Tao; Wang, Ping; Zhang, Zun-Ting

    2016-09-01

    Under microwave radiation, isomers 2-(pyrazolo[1,5-a]pyrimidin-5-yl)phenols (3) and 2-(pyrazolo[1,5-a]pyrimidin-7-yl)phenols (4) were simultaneously obtained by the condensation of chromones and 3-aminopyrazoles. These two isomers were fully characterized by IR, 1H NMR, 13C NMR and HRMS. In addition, a representative product 5-chloro-2-(2-methyl-pyrazolo[1,5-a] pyrimidin-5-yl)phenol (3e) was further conformed by the single crystal X-ray diffraction. The antifungal abilities of the obtained products 3 and 4 were evaluated against five phytopathogenic fungi (Cytospora sp., Colletotrichum gloeosporioides, Botrytis cinerea, Alternaria solani and Fusarium solani). The results revealed that 2-(pyrazolo[1,5-a]pyrimidin-5-yl)phenol (3a) and 4-chloro-2-(2-methylpyrazolo[1,5-a]pyrimidin-7-yl)phenol (4e) exhibited good antifungal abilities against Colletotrichum gloeosporioides with the IC50 values of 24.90 and 28.28 μg/mL, respectively.

  3. Synthesis, crystal structure and adsorption properties of a novel Mn(II) coordination polymer

    Science.gov (United States)

    Cui, Lian-Sheng; Gan, Yong-Le; Li, Yuan-Cheng; Meng, Jun-Rong

    2017-11-01

    A novel Mn(II) coordination polymer based on a "V"-shaped 1,3-di(4‧-carboxyl-phenyl)benzene acid (H2dpb, dpb = 1,3-di(4‧-carboxyl-phenyl)benzene), namely {[Mn(dpb)(4,4‧-bibp)]·H2O}n (4,4‧-bibp = 4,4‧-bis(imidazol-1-yl)biphenyl) has been hydrothermally synthesized and characterized by single-crystal X-ray diffraction and further characterized by elemental analysis, IR spectra, and thermogravimetric analysis (TGA). Furthermore, CO2 and SO2 adsorption properties of the complex were tested by high-pressure adsorption instrument under different pressure. The results show that the adsorption performance of CO2 is far superior to SO2 on the same conditions. The adsorption capacity increases with temperature rising. Very interestingly, the saturated adsorption amount (5.5 mmol/g) at 100 °C is less than the one at 80 °C (7.20 mmol/g). This phenomenon is caused by the escape of water vapor.

  4. Synthesis, crystal structure and photoluminescence property of Eu/Tb MOFs with mixed polycarboxylate ligands

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Lu; Zhang, Sheng; Qu, Xiaoni; Yang, Qi [Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of Ministry of Education, College of Chemistry and Materials Science, Northwest University, Xi’an 710127 (China); Liu, Xiangyu [Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of Ministry of Education, College of Chemistry and Materials Science, Northwest University, Xi’an 710127 (China); School of Chemistry and Chemical Engineering, Ningxia University, Yinchuan 750021 (China); Wei, Qing; Xie, Gang [Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of Ministry of Education, College of Chemistry and Materials Science, Northwest University, Xi’an 710127 (China); Chen, Sanping, E-mail: sanpingchen@126.com [Key Laboratory of Synthetic and Natural Functional Molecule Chemistry of Ministry of Education, College of Chemistry and Materials Science, Northwest University, Xi’an 710127 (China)

    2015-11-15

    Lanthanide MOFs, [Eu(TCA)(NDC)·H{sub 2}O]{sub n} (1) and [Tb(TCA)(NDC)·H{sub 2}O]{sub n} (2), have been prepared with the mixed aromatic carboxylate ligands, namely, 4,4′,4″-tricarboxytriphenylamine (H{sub 3}TCA) and 1,4-naphthalenedicarboxylate (H{sub 2}NDC). Single-crystal X-ray diffraction analysis reveals that isomorphic 1 and 2 present pillar-layered 3D framework that Eu/Tb(III) bond with carboxylate in various coordination fashions. Optical investigation indicates that the as-prepared compounds feature characteristic luminescence emission bands of Eu/Tb ions in the visible regions at room temperature. Moreover, compound 2 shows a relatively longer luminescence lifetime (τ=0.342 ms) and significantly enhanced quantum yield (Φ{sub overall}=11%) comparing with those of 1 (τ=0.335 ms, Φ{sub overall}=0.06%). - Graphical abstract: Synoptic: Two Ln-MOFs (Ln=Eu{sup III}, Tb{sup III}) with mixed polycarboxylate ligands present different luminescent properties. - Highlights: • Two Eu/Tb-MOFs with H{sub 3}TCA and H{sub 2}NDC ligands have been obtained. • The ancillary ligand is employed to decrease water molecule coordinate numbers. • 2displays superior quantum yield and lifetime than those of 1.

  5. A porous cadmium(II) framework. Synthesis, crystal structure, gas adsorption, and fluorescence sensing properties

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Pingping [College of Sciences, Agricultural University of Hebei, Baoding (China)

    2017-05-18

    The Cd{sup II} compound, namely [Cd(Tppa)(SO{sub 4})(H{sub 2}O)]{sub n} (1) [Tppa = tris(4-(pyridyl)phenyl) amine], was synthesized by the reaction of CdSO{sub 4}.8H{sub 2}O and Tppa under solvothermal conditions. Single crystal X-ray diffraction analysis revealed that compound 1 features a 3D porous framework based on 1D inorganic -[Cd-SO{sub 4}-Cd]{sub n}- chains. Topological analysis reveals that compound 1 represents a trinodal (3,4,6)-connected topological network with the point symbol of {6.7"2}{sub 2}{6"4.7.10}{6"4.7"5.8"4.10"2}. Gas adsorption properties investigations indicate that compound 1 exhibits moderate adsorption capacities for light hydrocarbons at room temperature. Luminescence property studies revealed that this Cd{sup II} compound exhibits high fluorescence sensitivity for sensing of CS{sub 2} molecule. (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  6. Molybdenum Nitride Films: Crystal Structures, Synthesis, Mechanical, Electrical and Some Other Properties

    Directory of Open Access Journals (Sweden)

    Isabelle Jauberteau

    2015-10-01

    Full Text Available Among transition metal nitrides, molybdenum nitrides have been much less studied even though their mechanical properties as well as their electrical and catalytic properties make them very attractive for many applications. The δ-MoN phase of hexagonal structure is a potential candidate for an ultra-incompressible and hard material and can be compared with c-BN and diamond. The predicted superconducting temperature of the metastable MoN phase of NaCl-B1-type cubic structure is the highest of all refractory carbides and nitrides. The composition of molybdenum nitride films as well as the structures and properties depend on the parameters of the process used to deposit the films. They are also strongly correlated to the electronic structure and chemical bonding. An unusual mixture of metallic, covalent and ionic bonding is found in the stoichiometric compounds.

  7. Synthesis, crystal structure and electrochemical and DNA binding studies of oxygen bridged-copper(II) carboxylate

    Science.gov (United States)

    Iqbal, Muhammad; Ali, Saqib; Tahir, Muhammad Nawaz; Muhammad, Niaz; Shah, Naseer Ali; Sohail, Manzar; Pandarinathan, Vedapriya

    2015-08-01

    A new binuclear O-bridged Cu(II) complex with 4-chlorophenyl acetate and 2,2‧-bipyridine has been synthesized and characterized using FT-IR, powder and single crystal XRD and electrochemical solution studies. The results revealed that the two penta-coordinated Cu(II) centers are linked by two carboxylate ligands in end-on bonding fashion. The coordination geometry is slightly distorted square pyramidal (SP) with bridging oxygen atoms occupying the apical position and other ligands lying in the equatorial plane. The striking difference in Cu-O bond distance of the bridging oxygen atom in the complex may be responsible for the SP geometry of Cu(II) ion. The complex gave rise to metal centered irreversible electro-activity where one electron Cu(II)/Cu(III) oxidation process and a single step two electron Cu(II)/Cu(0) reduction process was observed. The redox processes were found predominantly adsorption controlled. The values of diffusion coefficient and heterogeneous rate constant for oxidation process were 6.98 × 10-7 cm2 s-1 and 4.60 × 10-5 cm s-1 while the corresponding values for reduction were 5.30 × 10-8 cm2 s-1 and 5.41 × 10-6 cm s-1, respectively. The formal potential and charge transfer coefficient were also calculated. The DNA-binding ability was explored through cyclic voltammetry and UV-Visible spectroscopy. Diminution in the value of Do for oxidation indicated the binding of the complex with DNA corresponding to Kb = 8.58 × 104 M-1. UV-Visible spectroscopy yielded ε = 49 L mol-1 cm-1 and Kb = 2.96 × 104 M-1. The data of both techniques support each other. The self-induced redox activation of the complex, as indicated by cyclic voltammetry heralds its potential applications in redox catalysis and anticancer activity.

  8. Luminescent lanthanide complexes with 4-acetamidobenzoate: Synthesis, supramolecular assembly via hydrogen bonds, crystal structures and photoluminescence

    International Nuclear Information System (INIS)

    Yin Xia; Fan Jun; Wang Zhihong; Zheng Shengrun; Tan Jingbo; Zhang Weiguang

    2011-01-01

    Four new luminescent complexes, namely, [Eu(aba) 2 (NO 3 )(C 2 H 5 OH) 2 ] (1), [Eu(aba) 3 (H 2 O) 2 ].0.5 (4, 4'-bpy).2H 2 O (2), [Eu 2 (aba) 4 (2, 2'-bpy) 2 (NO 3 ) 2 ].4H 2 O (3) and [Tb 2 (aba) 4 (phen) 2 (NO 3 ) 2 ].2C 2 H 5 OH (4) were obtained by treating Ln(NO 3 ) 3 .6H 2 O and 4-acetamidobenzoic acid (Haba) with different coligands (4, 4'-bpy=4, 4'-bipyridine, 2, 2'-bpy=2, 2'-bipyridine, and phen=1, 10-phenanthroline). They exhibit 1D chains (1-2) and dimeric structures (3-4), respectively. This structural variation is mainly attributed to the change of coligands and various coordination modes of aba molecules. Moreover, the coordination units are further connected via hydrogen bonds to form 2D even 3D supramolecular networks. These complexes show characteristic emissions in the visible region at room temperature. In addition, thermal behaviors of four complexes have been investigated under air atmosphere. The relationship between the structures and physical properties has been discussed. - Graphical abstract: Structure variation of four complexes is attributed to the change of coligands and various coordination modes of aba molecules. Moreover, they show characteristic emissions in the visible region. Highlights: → Auxiliary ligands have played the crucial roles on the structures of the resulting complexes. → Isolated structure units are further assembled via H-bonds to form supramolecular networks. → These solid-state complexes exhibit strong, characteristic emissions in the visible region.

  9. Synthesis and crystal structure of N-(3-benzylamino-2- cyano-3 ...

    African Journals Online (AJOL)

    Phenylurea groups were introduced into the frame of traditional cyanoacrylate and a series of N-(3-benzylamino-2-cyano-3-methylthioacrylyl)-N'-(substituted phenyl)ureas were synthesized. All compounds are new and their structures were confirmed by 1H NMR, 13C NMR and mass spectral analyses. KEY WORDS: ...

  10. Synthesis and crystal structure of trans-[Ni(pyzdcH)M 2 (H 2 O) 2 ...

    African Journals Online (AJOL)

    The determined structure of the title compound C24H20Ni2N8O20 consists of the mononuclear trans-[Ni(pyzdc)2(H2O)2], (pyzdc = pyrazine-2,3- dicarboxylate). The Ni(II) atom is hexa-coordinated by two (pyzdcH)- groups and two water molecules. The coordinated water molecules are in trans-diaxial positions and the ...

  11. Synthesis and crystal structure determination of YCo1−xFexO3 (x ...

    Indian Academy of Sciences (India)

    state (t4. 2ge2 g), or it could exist in mixed spin state.5,9. It should also be pointed out that the obtained struc- tural phase and particle size of perovskites depend on ... study, different synthetic routes and detailed structural investigation of new complex perovskites of general formula YCo1−x. FexO3 (x = 0, 0.33, 0.5, 0.67 and.

  12. Synthesis, growth, structure, mechanical and optical properties of a new semi-organic 2-methyl imidazolium dihydrogen phosphate single crystal

    Energy Technology Data Exchange (ETDEWEB)

    Nagapandiselvi, P., E-mail: nagapandiselvip@ssn.edu.in [Department of Physics, SSN College of Engineering, Kalavakkam (India); Baby, C. [Sophisticated Analytical Instrument Facility, Indian Institute of Technology Madras, Chennai (India); Gopalakrishnan, R. [Crystal Research Lab, Department of Physics, Anna University, Chennai (India)

    2016-09-15

    Highlights: • 2MIDP crystals were grown by slow evaporation solution growth technique. • Single crystal XRD revealed self-assembled supramolecular framework. • Z scan technique is employed for third order nonlinear optical susceptibility. • Structure-property correlation is established. - Abstract: A new semi-organic compound, 2-methyl imidazolium dihydrogen phosphate (2MIDP), was prepared and good quality single crystals of 2MIDP were grown by slow evaporation solution growth technique. Crystal structure elucidated using Single crystal XRD showed that 2MIDP crystallizes in monoclinic system with P2{sub 1}/c space group. FT-IR, UV-Vis-NIR, Fluorescence and FT-NMR spectra confirm the molecular structure of 2MIDP. The UV-Vis-NIR spectra established the suitability of the compound for NLO applications. TG-DSC showed that 2MIDP is thermally stable up to 200 °C. Mechanical characteristics like hardness number (H{sub v}), stiffness constant (C{sub 11}), yield strength (σ{sub v}), fracture toughness (K{sub c}) and brittleness index (B{sub i}) were assessed using Vicker’s microhardness tester. Third order nonlinear optical properties determined from Z-scan measurement using femto and picosecond lasers showed two photon reverse saturable absorption. The enhancement of nonlinear optical properties in femto second laser, revealed the suitability of 2MIDP for optical limiting applications.

  13. Luminescent lanthanide complexes with 4-acetamidobenzoate: Synthesis, supramolecular assembly via hydrogen bonds, crystal structures and photoluminescence

    Science.gov (United States)

    Yin, Xia; Fan, Jun; Wang, Zhi Hong; Zheng, Sheng Run; Tan, Jing Bo; Zhang, Wei Guang

    2011-07-01

    Four new luminescent complexes, namely, [Eu(aba) 2(NO 3)(C 2H 5OH) 2] ( 1), [Eu(aba) 3(H 2O) 2]·0.5 (4, 4'-bpy)·2H 2O ( 2), [Eu 2(aba) 4(2, 2'-bpy) 2(NO 3) 2]·4H 2O ( 3) and [Tb 2(aba) 4(phen) 2(NO 3) 2]·2C 2H 5OH ( 4) were obtained by treating Ln(NO 3) 3·6H 2O and 4-acetamidobenzoic acid (Haba) with different coligands (4, 4'-bpy=4, 4'-bipyridine, 2, 2'-bpy=2, 2'-bipyridine, and phen=1, 10-phenanthroline). They exhibit 1D chains ( 1- 2) and dimeric structures ( 3- 4), respectively. This structural variation is mainly attributed to the change of coligands and various coordination modes of aba molecules. Moreover, the coordination units are further connected via hydrogen bonds to form 2D even 3D supramolecular networks. These complexes show characteristic emissions in the visible region at room temperature. In addition, thermal behaviors of four complexes have been investigated under air atmosphere. The relationship between the structures and physical properties has been discussed.

  14. Synthesis, properties, and crystal structure of complex Cp2Yb(DAD)

    International Nuclear Information System (INIS)

    Trifonov, A.A.; Kirillov, E.N.; Bochkarev, M.N.; Shumani, G.; Myule, S.

    1999-01-01

    Diazadiene complex of trivalent ytterbium Cp 2 Yb(DAD) (1) (DAD = Bu 1 -N CH-CH = N-Bu 1 ) was obtained by three routes: the oxidation of Cp 2 Yb(THF) 2 by diazadiene in tetrahydrofuran (THF), the reaction of Cp 2 YbCl with DAD 2- Na 2 + (2:1), and the reaction of Cp 2 YbCl(THF) with DAD - K + in the 1:1 ratio. Complex 1 was characterized by microanalysis, IR spectroscopy, magnetochemistry, and X-ray structural analysis [ru

  15. Synthesis and crystal structure of Pb(Bipy)(DMFA)B12H12

    International Nuclear Information System (INIS)

    Lagun, V.L.; Solntsev, K.A.; Katser, S.B.; Orlova, A.M.; Kuznetsov, N.T.

    1994-01-01

    Lead complex with B 12 H 12 2- anion and neutral ligands -2,2' -bipyridine (Bipy) and dimethylformamide (DMFA) has been prepared by Pb(Bipy) B 12 H 12 recrystallization from mixed solvent DMFA - benzene (1:1). The complex prepared has been studied by the methods of IR spectroscopy, element and X-ray diffraction analyses. Parameters of monoclinic cell are as follows: 1 = 9.583(2), b = 16.958 (4), c = 18.685 (3) A; β = 105.65 (2), V = 2924 (1) A 3 , Z =4; sp.gr. P2 1 /c. The structure consists of dimer units. Pb-B distance is within 3.23-3.71 (3) A. 5 refs.; 2 figs.; 2 tabs

  16. Complexes of uranyl nitrate with 2,6-pyridinedicarboxamides: synthesis, crystal structure, and DFT study

    Energy Technology Data Exchange (ETDEWEB)

    Alyapyshev, Mikhail; Babain, Vasiliy [ITMO University, 49, Kronverksky pr., 197101, St. Petersburg (Russian Federation); ThreeArc Mining Ltd., 5, Stary Tolmachevskiy per., 115184, Moscow (Russian Federation); Tkachenko, Lyudmila; Lumpov, Alexander [Khlopin Radium Institute, 28, 2nd Murinskiy pr., 194021, St. Petersburg (Russian Federation); Gurzhiy, Vladislav; Zolotarev, Andrey; Dar' in, Dmitriy [St. Petersburg State University, 7-9, Universitetskaya nab., 199034, St. Petersburg (Russian Federation); Ustynyuk, Yuriy; Gloriozov, Igor [M.V. Lomonosov Moscow State University, 119991, Moscow (Russian Federation); Paulenova, Alena [Department of Nuclear Engineering, Oregon State University, Corvallis, OR (United States)

    2017-05-04

    Two complexes of uranyl nitrate with N,N,N',N'-tetrabutyl-2,6-pyridinedicarboxamide (TBuDPA) and N,N'-diethyl-N,N'-diphenyl-2,6-pyridinedicarboxamide (EtPhDPA) were synthesized and studied. The complex of tetraalkyl-2,6-pyridinedicarboxamide with metal nitrate was synthesized for the first time. XRD analysis revealed the different type of complexation: a 1:1 metal:ligand complex for EtPhDPA and complex with polymeric structure for TBuDPA. The quantum chemical calculations (DFT) confirm that both ligands form the most stable complexes that match the minimal values pre-organization energy of the ligands. (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

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

    Directory of Open Access Journals (Sweden)

    Imtiaz Khan

    2012-07-01

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

  18. Synthesis, crystal structure and computational chemistry research of a Zinc(II complex: [Zn(Pt(Biim2

    Directory of Open Access Journals (Sweden)

    Teng Fei

    2012-01-01

    Full Text Available The title metal-organic coordination complex [Zn(pt(Biim2] (pt=phthalic acid, benzene-1,2-dicarboxylate, Biim=2,2'-biimidazole 1 has been obtained by using hydrothermal synthesis and characterized by single-crystal X-ray diffraction. The complex crystallizes in monoclinic, space group P21/n with a = 8.5466(15 Å, b = 11.760(2 Å, c = 20.829(4 Å, β = 95.56(2º, V = 2083.5(6 Å3, Mr =497.78, Dc = 1.587 g/cm3, μ(MoKα = 1.226 mm−1, F(000 = 1016, Z = 4, the final R = 0.0564 and wR = 0.1851 for 3656 observed reflections (I > 2σ(I. The elemental analysis, IR, TG and the theoretical calculation were also investigated.

  19. Investigation on synthesis, growth, structure and physical properties of AgGa0.5In0.5S2 single crystals for Mid-IR application

    Science.gov (United States)

    Karunagaran, N.; Ramasamy, P.

    2018-02-01

    Silver Gallium Indium Sulfide (AgGa0.5In0.5S2) belongs to the family of AIBIIIC2VI ternary compound semiconductors which crystallize in the chalcopyrite structure. Synthesis of the polycrystalline material from the starting elements is achieved using melt temperature oscillation method. The AgGa0.5In0.5S2 single crystals have been grown by the vertical Bridgman technique. The synthesized AgGa0.5In0.5S2 polycrystalline charge was confirmed by powder XRD. The peak positions are in good agreement with the powder diffraction file. Thermal property was analyzed using differential scanning calorimetry (DSC) technique. The melting point of the crystal is 896 °C and freezing point is 862 °C. The unit cell parameters were confirmed by single crystal X-ray. The transmittance of the grown crystal is 55% in the NIR region and 60% in the mid-IR region. The optical band gap was found to be 2.0 eV. The stoichiometric composition of AgGa0.5In0.5S2 was measured using energy dispersive spectrometry (EDS). The photoluminescence behavior of AgGa0.5In0.5S2 has been analyzed. The resistivity of the grown single crystal has been measured.

  20. Synthesis, crystal structure, vibrational spectroscopy and photoluminescence of new hybrid compound containing chlorate anions of stanate (II)

    Science.gov (United States)

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

    2017-08-01

    The present work aimed at studying a new organic-inorganic bis (4-amino quinolinium) hexachloro stanate (II) dihydrate compound. It was prepared and characterized by single crystal X-ray diffraction, X-ray powder, Hirshfeld surface, Spectroscopy measurement, thermal study and photoluminescence properties. It was found to crystallize in the monoclinic system (P21/c space group) with the following lattice parameters: a = 7.2558(6) Å, b = 13.4876(5) Å, c = 17.2107(13) Å, β = 102.028 (12)°. Its crystal structure was determined and refined down to an R value of 0.06 and a wR value of 0.087. The structure consisted of two different alternating organic-inorganic layers. The crystal packing was stabilized by Nsbnd H⋯Cl and Osbnd H⋯Cl hydrogen bonds and π-π interactions. Hirshfeld surface analysis was used to investigate intermolecular interactions, as well 2D finger plots were conducted to reveal the contribution of these interactions in the crystal structure quantitatively. The X-ray powder is in agreement with the X-ray structure. Scanning electronic microscopy (SEM) was carried out. Furthermore, the room temperature Infra Red (IR) spectrum of the title compound was analyzed on the basis of data found in the literature. Solid state 13C NMR spectrum shows ten signals, confirming the solid state structure determined by X-ray diffraction. Thermal analysis shows two anomalies at 380 and 610 °C. The optical properties of the crystal were studied using optical absorption UV-visible and photoluminescence (PL) spectroscopy, which were investigated at room temperature.

  1. Zintl Salts Ba2P7X (X = Cl, Br, and I: Synthesis, Crystal, and Electronic Structures

    Directory of Open Access Journals (Sweden)

    Juli-Anna Dolyniuk

    2013-08-01

    Full Text Available Two barium phosphide halides, Ba2P7Br and Ba2P7I, were synthesized and structurally characterized by single crystal X-ray diffraction. Both compounds crystallize in the monoclinic space group P21/m (No. 11 and are isostructural to Ba2P7Cl. The crystal structures of Ba2P7X (X = Cl, Br, I feature the presence of heptaphosphanortricyclane P73− clusters along with halogen anions and barium cations. According to the Zintl concept, Ba2P7X compounds are electron-balanced semiconductors. Quantum-chemical calculations together with UV-Visible spectroscopy confirm the title compounds are wide bandgap semiconductors. The bonding in the P73− clusters was analyzed by means of electron localization function. The elemental compositions were confirmed using energy dispersive X-ray spectroscopy.

  2. Synthesis, crystal structures, spectral, thermal and antimicrobial properties of new Zn(II) 5-iodo- and 5-bromosalicylates

    Science.gov (United States)

    Košická, Petra; Győryová, Katarína; Smolko, Lukáš; Gyepes, Róbert; Hudecová, Daniela

    2018-03-01

    Two new analogous zinc(II) complexes containing 5-iodo- and 5-bromosalicylate ligands, respectively, were prepared in single-crystal form and characterized by IR spectroscopy, thermal analysis and elemental analysis. The solid-state structures of prepared complexes were determined by single crystal X-ray crystallography. Both complexes are isostructural and their crystal structures composed of neutral molecules [Zn(5-Xsal)2(H2O)2] (where X = Br, I, sal = salicylato). Central Zn(II) atom is in both complexes coordinated by six oxygen atoms, four of which are from two chelate bonded 5-halosalicylates and remaining two from coordinated water molecules. The found chelate binding mode is in line with the Δ values calculated from IR spectral data. Antimicrobial activity of prepared complexes was studied against selected bacteria, yeast and filamentous fungi. Obtained results indicate that 5-iodosalicylate complex is more antimicrobially active than its 5-bromo substituted analogue.

  3. Diiodo{N,N´-bis(2,3,4-trimethoxybenzaldehyde)-ethylenediimine}mercury(II): synthesis and crystal structure

    Czech Academy of Sciences Publication Activity Database

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

    2013-01-01

    Roč. 39, č. 1 (2013), s. 68-71 ISSN 1070-3284 Institutional support: RVO:68378271 Keywords : mercury (II) * Schiff base * single crystal * structure analysis Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.629, year: 2013

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

    Czech Academy of Sciences Publication Activity Database

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

    2015-01-01

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

  5. Synthesis, characterization, crystal structure determination, thermal study and catalytic activity of a new oxidovanadium Schiff base complex

    Czech Academy of Sciences Publication Activity Database

    Grivani, G.; Ghavami, A.; Kučeráková, Monika; Dušek, Michal; Khalaji, A.D.

    2014-01-01

    Roč. 1076, Nov (2014), s. 326-332 ISSN 0022-2860 R&D Projects: GA ČR(CZ) GA14-03276S Institutional support: RVO:68378271 Keywords : oxidovanadium(IV) * Schiff base * crystal structure * V 2 O 5 nano-particle * oxidation Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.602, year: 2014

  6. 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

  7. Synthesis, crystal structure, and spectra of 3,3- dimethyl-1-N-(1'-phenyl-2',3'-dimethyl-5'-oxo-3'- pyrazolin-4'-yl)imino-1,2,3,4-tetrahydroisoquinoline

    International Nuclear Information System (INIS)

    Sokol, V.I.; Ryabov, M.A.; Merkur'eva, N.Yu.; Davydov, V.V.; Zaitsev, B.E.; Shklyaev, Yu.V.; Sergienko, V.S.; Zaitsev, B.E.

    1996-01-01

    The synthesis and the crystal and molecular structure of 3,3-dimethyl-1-N-(1'-phenyl-2',3'- dimethyl-5'-oxo-3'-pyrazolin-4'-yl)imino-1,2,3,4-tetrahydroisoquinoline are reported. As is evidenced by the 1H NMR, IR, and electron spectra, the tautomeric form of the compounds observed in the crystal is also retained in solutions

  8. SYNTHESIS, STRUCTURE AND PHOTOLUMINESCENCE OF ...

    African Journals Online (AJOL)

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    dimensional supramolecular framework. ... The growing interest in the field of the crystal engineering of inorganic-organic hybrid materials .... Synthesis, structure and photoluminescence of (HgCl3)n(C6NO2H6)n(C6NO2H5)n nH2O. Bull. Chem.

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

    Science.gov (United States)

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

    2016-04-01

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

  10. LiB12PC, the first boron-rich metal boride with phosphorus--synthesis, crystal structure, hardness, spectroscopic investigations.

    Science.gov (United States)

    Vojteer, Natascha; Sagawe, Vanessa; Stauffer, Julia; Schroeder, Melanie; Hillebrecht, Harald

    2011-03-07

    We present synthesis, crystal structure, hardness, and IR/Raman and UV/Vis spectra of a new compound with the mean composition LiB(12)PC. Transparent single crystals were synthesised from Ga, Li, B, red phosphorus and C at 1500 °C in boron nitride crucibles welded in Ta ampoules. Depending on the type of boron used for the synthesis we obtained colourless, brown and red single crystals with slightly different P/C ratios. Colourless LiB(12)PC crystallizes orthorhombic in the space group Imma (No. 74) with a=10.188(2) Å, b=5.7689(11) Å, c=8.127(2) Å and Z=4. Brown LiB(12)P(0.89)C(1.11) is very similar, but with a lower P content. Red single crystals of LiB(12)P(1.13)C(0.87) have a larger unit cell with a=10.4097(18) Å, b=5.9029(7) Å, c=8.2044(12) Å. EDX measurements confirm that the red crystals contain more phosphorus than the other ones. The crystal structure is characterized by a covalent network of B(12) icosahedra connected by exohedral B-B bonds and P-P, P-C or C-C units. Li atoms are located in interstitials. The structure is closely related to MgB(7), LiB(13)C(2) and ScB(13)C. LiB(12)PC fulfils the electron counting rules of Wade and also Longuet-Higgins. Measurements of Vickers micro-hardness (H(V)=27 GPa) revealed that LiB(12)PC is a hard material. The optical band gaps obtained from UV/Vis spectra match the colours of the crystals. Furthermore we report on the IR and Raman spectra. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    International Nuclear Information System (INIS)

    Mustaffa Shamsuddin; Md Abu Affan; Ramli Atan

    1998-01-01

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

  12. Synthesis, crystal and electronic structures and optical properties of (HIm)2Hg3Cl8 and (HIm)HgI3 (HIm = imidazolium)

    Science.gov (United States)

    Nhalil, Hariharan; Whiteside, Vincent R.; Sellers, Ian R.; Ming, Wenmei; Du, Mao-Hua; Saparov, Bayrammurad

    2018-02-01

    We report synthesis, crystal and electronic structures, and optical properties of two new Hg-based zero-dimensional hybrid organic-inorganic halides (HIm)2Hg3Cl8 and (HIm)HgI3 (HIm = imidazolium). (HIm)2Hg3Cl8 crystallizes in the triclinic P-1 space group with a pseudo-layered structure made of organic imidazolium cation layers and anionic inorganic layers containing [Hg2Cl6]2- units and linear [HgCl2]0 molecules. (HIm)HgI3 crystallizes in the monoclinic P21/c space group featuring anionic [HgI3]- units that are surrounded by imidazolium cations. Based on density functional theory calculations, (HIm)2Hg3Cl8 has an indirect band gap, whereas (HIm)HgI3 has a direct band gap with the measured onsets of optical absorption at 3.43 and 2.63 eV, respectively. (HIm)2Hg3Cl8 and (HIm)HgI3 are broadband light emitters with broad photoluminescence peaks centered at 548 nm (2.26 eV) and 582 nm (2.13 eV), respectively. Following the crystal and electronic structure considerations, the PL peaks are assigned to self-trapped excitons.

  13. Synthesis and X-Ray Crystal Structure of the First Pure and Air-Stable Salt of Peroxymonosulphuric Acid: (Ph4PHSO5

    Directory of Open Access Journals (Sweden)

    Marco Crisma

    2000-06-01

    Full Text Available In this paper we describe the synthesis of tetraphenylphosphonium peroxymonosulphate, its crystal structure and packing mode. The asymmetric unit accomodates two independent molecules of the monopersulphate anion, which are held together by hydrogen bonds. In the packing mode, rows of such dimers are surrounded by four rows of tetraphenyl cations. The consequence is that the highly water sensitive HSO5¯ anions are segregated inside hydrophobic channels composed by the lipophilic cations. This circumstance presumably accounts for the exceptional stability of the title compound.

  14. Synthesis and X-Ray Crystal Structures of Mononuclear Complexes of 1,3-Bis(8-quinolyloxy)propane

    International Nuclear Information System (INIS)

    Al-Mandhary, M.R.; Steel, P.

    2002-01-01

    The preparations and X-ray crystal structures of the first transition metal complexes of 1,3-bis(8-quinolyloxy)propane are described. The ligand acts as a trans-chelating N,N'-bidentate ligand in the three-coordinate silver nitrate complex and four-coordinate copper chloride complex, but as an N,O,O',N'-tetradentate ligand in the octahedral nickel chloride complex. Copyright (2002) CSIRO Australia

  15. Two Organic Cation Salts Containing Tetra(isothiocyanatecobaltate(II: Synthesis, Crystal Structures, Spectroscopic, Optical and Magnetic Properties

    Directory of Open Access Journals (Sweden)

    Zheng Zhang

    2017-03-01

    Full Text Available Single crystals of two hybrid organic-inorganic molecular solids, benzyl pyridinium tetra(isothiocyanatecobalt ([BzPy]2[Co(NCS4] (1 and benzyl quinolinium tetra(isothiocyanatecobalt ([BzQl]2[Co(NCS4] (2, were grown using a slow evaporation growth technique at room temperature and their IR, UV-Vis, X-ray crystal structures, luminescence, and magnetism were reported. The crystal structural analysis revealed that two molecular solids crystallize in the monoclinic space group P21/c of 1 and P21/n of 2. The cations form a dimer through weak C–H···π/π···π interactions in 1 and 2, and the adjacent cation (containing N(6 atom in 2 forms a columnar structure through π···π weak interactions between the quinoline and benzene rings, while the anions in 1 form a layer structure via short S···Co interactions. The anions (A and cations (C are arranged alternatively into a column in the sequence of ···A–CC–A–CC–A··· for 1, while the two anions and cationic dimer in 2 form an alliance by the C–H···π, C–H···S and C–H···N hydrogen bonds. A weak S···π interaction was found in 1 and 2. The two molecular solids show a broad fluorescence emission around 400 nm in the solid state at room temperature, and weak antiferromagnetic coupling behavior when the temperature is lowered.

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

    Science.gov (United States)

    Amani, Vahid

    2018-03-01

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

  17. Crystal engineering: structure, property and beyond

    OpenAIRE

    Desiraju, Gautam R.

    2017-01-01

    Crystal engineering, which was considered to be crystal structure engineering, is now transforming into crystal property engineering. The same or similar crystal structures could have different properties while different crystal structures could have similar properties.

  18. Synthesis, crystal structure and biological activity of n-(5-(o-tolyl)-1, 3, 4-thiadiazol-2-yl)cyclopropanecarboxamide

    International Nuclear Information System (INIS)

    Tong, J.Y.; Sun, N.B.; Wu, H.K.

    2013-01-01

    A new 1, 3, 4-thiadiazole compound, N-(5-(o-tolyl)-1,3,4-thiadiazol-2-yl) cyclopropanecarboxamide, was synthesized and its structure was confirmed by 1H NMR, MS and HRMS. The single crystal structure of the title compound was determined by X-ray diffraction. The preliminary biological test showed that the synthesized compound has moderate herbicidal activity against Brassica campestris and fungicidal activities against Sclerotinia sclerotiorum(Lib.) de Bary, Rhizoctonia solanii, Fusarium oxysporum, Corynespora cassiicola, and Botrytis cinerea. (author)

  19. Synthesis, spectral, crystal structure, thermal behavior, antimicrobial and DNA cleavage potential of two octahedral cadmium complexes: A supramolecular structure

    Czech Academy of Sciences Publication Activity Database

    Montazerozohori, M.; Musavi, S.A.; Masoudiasl, A.; Naghiha, A.; Dušek, Michal; Kučeráková, Monika

    2015-01-01

    Roč. 137, FEB (2015), s. 389-396 ISSN 1386-1425 R&D Projects: GA ČR(CZ) GA14-03276S Institutional support: RVO:68378271 Keywords : Schiff base * Cd(II) * DNA cleavage * TG/DTG analysis * X-ray structure analysis Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 2.653, year: 2015

  20. High-pressure synthesis and crystal structures of beta- M NX (M = Zr, Hf; X = Cl, Br, I)

    CERN Document Server

    Chen, X; Yamanaka, S

    2002-01-01

    The single crystals of six kinds of metal nitride halide, beta- M NX (M = Zr, Hf; X = Cl, Br, I), were grown in sealed Au (or Pt) tubes by the reaction of M N or M NX powders with NH sub 4 X as fluxes under high-temperature and high-pressure conditions such as 3-5 GPa at 900-1200 sup o C. The x-ray structure analysis revealed that all six kinds of compound crystallize in a rhombohedral space group R3-bar m, Z = 6. beta-ZrNCl, beta-ZrNBr, and beta-HfNCl are isotypic with SmSI, and the others isostructural with YOF.

  1. Synthesis, crystal structure, vibrational spectra and theoretical calculations of quantum chemistry of a potential antimicrobial Meldrum's acid derivative

    Science.gov (United States)

    Campelo, M. J. M.; Freire, P. T. C.; Mendes Filho, J.; de Toledo, T. A.; Teixeira, A. M. R.; da Silva, L. E.; Bento, R. R. F.; Faria, J. L. B.; Pizani, P. S.; Gusmão, G. O. M.; Coutinho, H. D. M.; Oliveira, M. T. A.

    2017-10-01

    A new derivative of Meldrum's acid 5-((5-chloropyridin-2-ylamino)methylene)-2,2-dimethyl-1,3-dioxane-4,6-dione (CYMM) of molecular formula C12H11ClN2O4 was synthesized and structurally characterized using single crystal X-ray diffraction technique. The vibrational properties of the crystal were studied by Fourier Transform infrared (FT-IR), Fourier Transform Raman (FT-Raman) techniques and theoretical calculations of quantum chemistry using Density functional theory (DFT) and Density functional perturbation theory (DFPT). A comparison with experimental spectra allowed the assignment of all the normal modes. The descriptions of the normal modes were carried by means of potential energy distribution (PED). Additionally, analysis of the antimicrobial activity and antibiotic resistance modulatory activity was carried out to evaluate the antibacterial potential of the CYMM.

  2. Hydrothermal synthesis and crystal structure of a new lithium copper bismuth oxide, LiCuBiO{sub 4}

    Energy Technology Data Exchange (ETDEWEB)

    Kumada, Nobuhiro, E-mail: kumada@yamanashi.ac.jp [Center for Crystal Science and Technology, University of Yamanashi, Miyamae-cho 7-32, Kofu 400-8511 (Japan); Nakamura, Ayumi [Center for Crystal Science and Technology, University of Yamanashi, Miyamae-cho 7-32, Kofu 400-8511 (Japan); Miura, Akira [Center for Crystal Science and Technology, University of Yamanashi, Miyamae-cho 7-32, Kofu 400-8511 (Japan); Faculty of Engineering, Hokkaido University, Kita 13, Nishi 8, Kita-ku, Sapporo 060-8628 (Japan); Takei, Takahiro [Center for Crystal Science and Technology, University of Yamanashi, Miyamae-cho 7-32, Kofu 400-8511 (Japan); Azuma, Masaki; Yamamoto, Hajime [Laboratory for Materials and Structures, Tokyo Institute of Technology, 4259 Nagatsuta, Midori-ku Yokohama, Kanagawa 226-8503 (Japan); Magome, Eisuke; Moriyoshi, Chikako; Kuroiwa, Yoshihiro [Department of Physical Science, Hiroshima University, 1-3-1 Kagamiyama, Higashihiroshima, Hiroshima 739-8526 (Japan)

    2017-01-15

    A new lithium copper bismuth oxide, LiCuBiO{sub 4} was prepared by hydrothermal reaction using NaBiO{sub 3}0.1*4H{sub 2}O. The crystal structural model of this compound was refined by using synchrotron X-ray powder diffraction data. This bismuthate has the LiCuSbO{sub 4} related structure with the orthorhombic cell (Space group: Pnma) of a=10.9096(9), b=5.8113(5) and c=5.0073(4) Å, and the final R-factors were R{sub wp}=4.84 and R{sub p}=3.58%. This compound is the first example of a lithium copper bismuthate containing Bi{sup 5+}. An antiferromagnetic ordering of Cu{sup 2+} moment was observed at 6 K. - Graphical abstract: In the crystal structure of LiCuBiO{sub 4} all metal atoms are coordinated octahedrally by six O atoms and LiO{sub 6} and CuO{sub 6} octahedra form the one-dimensional chains by edge-sharing along the b-axis. The LiO{sub 6} and CuO{sub 6} chains form the layer by face-sharing in the bc plane. The Bi atoms are placed in that interlayer and BiO{sub 6} octahedra are edge-sharing with LiO{sub 6} and CuO{sub 6} octahedra. - Highlights: • A new lithium copper bismuth oxide, LiCuBiO{sub 4} is prepared by hydrothermal reaction. • The crystal structure of LiCuBiO{sub 4} is closely related with that of LiCuSbO{sub 4}. • This new compound exhibits an antiferromagnetic ordering of Cu{sup 2+} moment at 6 K.

  3. Synthesis, crystal structure and electrical properties of the new organic-inorganic hybrid compound bis(1-chlorido-4-aminopyridinium) octachlorodiantimoinate

    Science.gov (United States)

    Fersi, Mohamed Amine; Hajji, Rachid; Chaabane, Iskandar; Gargouri, Mohamed

    2017-10-01

    Bis(1-chlorido-4-aminopyridinium) octachlorodiantimoinate has been synthesized and characterized by a single-crystal X-ray diffraction at 296 K and impedance spectroscopy. At room temperature, the title compound is crystallized in the triclinic system (P 1 ̅ space group) with Z = 2 and the following unit cell dimensions: a = 7.919 (1) Å, b = 9.624 (1) Å, c = 17.692 (3) Å, α = 101.81 (1)°, β = 95.12 (1)°and γ = 112.48 (1)°. The crystal structure of the [C10H12Cl2N4]Sb2Cl8 compound is built of two un-equivalent monoprotonated cations [C5H6N2Cl] + and two un-equivalent tetrachloroantimonate (III) anions noted which are [Sb(1)Cl4]- and [Sb(2)Cl4]-. The arrangement of this compound can be described by an alternation of organic and inorganic layers stacked along [010] direction. The cohesion of compound entities is ensured by hydrogen bonding (N-H…. Cl) and Van Der Waals interaction (C-H…. Cl). The temperature dependence of the σdc conductivity exhibits an Arrhenius type behavior described by the following expression σdc T = Aexp(-Ea/kβT). The Ac conductivity and the dielectric loss suggest that the correlated barrier hopping is the appropriate model for the conduction mechanism.

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

    Science.gov (United States)

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

    2017-08-01

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

  5. Synthesis, crystal structure, and properties of a perovskite-related bismuth phase, (NH43Bi2I9

    Directory of Open Access Journals (Sweden)

    Shijing Sun

    2016-03-01

    Full Text Available Organic-inorganic halide perovskites, especially methylammonium lead halide, have recently led to remarkable advances in photovoltaic devices. However, due to environmental and stability concerns around the use of lead, research into lead-free perovskite structures has been attracting increasing attention. In this study, a layered perovskite-like architecture, (NH43Bi2I9, is prepared from solution and the structure solved by single crystal X-ray diffraction. The band gap, which is estimated to be 2.04 eV using UV-visible spectroscopy, is lower than that of CH3NH3PbBr3. The energy-minimized structure obtained from first principles calculations is in excellent agreement with the X-ray results and establishes the locations of the hydrogen atoms. The calculations also point to a significant lone pair effect on the bismuth ion. Single crystal and powder conductivity measurements are performed to examine the potential application of (NH43Bi2I9 as an alternative to the lead containing perovskites.

  6. Synthesis, crystal structure, and properties of a perovskite-related bismuth phase, (NH4)3Bi2I9

    Science.gov (United States)

    Sun, Shijing; Tominaka, Satoshi; Lee, Jung-Hoon; Xie, Fei; Bristowe, Paul D.; Cheetham, Anthony K.

    2016-03-01

    Organic-inorganic halide perovskites, especially methylammonium lead halide, have recently led to remarkable advances in photovoltaic devices. However, due to environmental and stability concerns around the use of lead, research into lead-free perovskite structures has been attracting increasing attention. In this study, a layered perovskite-like architecture, (NH4)3Bi2I9, is prepared from solution and the structure solved by single crystal X-ray diffraction. The band gap, which is estimated to be 2.04 eV using UV-visible spectroscopy, is lower than that of CH3NH3PbBr3. The energy-minimized structure obtained from first principles calculations is in excellent agreement with the X-ray results and establishes the locations of the hydrogen atoms. The calculations also point to a significant lone pair effect on the bismuth ion. Single crystal and powder conductivity measurements are performed to examine the potential application of (NH4)3Bi2I9 as an alternative to the lead containing perovskites.

  7. Synthesis, crystal structure and magnetic properties of two oxalato-bridged dimetallic trinuclear complexes combined with a polar cation.

    Science.gov (United States)

    Pardo, Emilio; Train, Cyrille; Lescouëzec, Rodrigue; Boubekeur, Kamal; Ruiz, Eliseo; Lloret, Francesc; Verdaguer, Michel

    2010-05-28

    Two isostructural heterometallic trinuclear oxalato-bridged complexes of formula C(4)[MCr(2)(ox)(6)(H(2)O)(2)]·nH(2)O (C(+) = 4-aminopyridinium; ox(2-) = oxalate dianion; M(2+) = Mn(2+), n = 3, 1; M(2+) = Co(2+), n = 3.25, 2) have been synthesized by using direct self-assembly methods combining C(3)[Cr(ox)(3)] and the chloride salts of the corresponding metal ion. The crystal structures of both compounds have been resolved by single-crystal X-ray diffraction. They crystallize in the C2/c space group [a = 11.5113(15) Å, b = 20.250(3) Å, c = 21.810(4) Å, beta = 100.447(10) degrees, V = 5161.6(3) Å(3), and Z = 4 for 1, and a = 11.4334(16) Å, b = 20.243(2) Å, c = 21.805(3) Å, beta = 101.113(9) degrees, V = 4951.9(11) Å(3), and Z = 4 for 2]. The structures of 1 and 2 consist of discrete linear [MCr(2)(ox)(6)](4-) bimetallic trinuclear units, pyridinium cations and crystallization water molecules. The linear trinuclear unit is built from a central trans-diaquametal(II), linked to two Cr(ox)(3)](3-) entities by oxalate bridges. One of the oxalate ions is coordinated to the central metal ion whereas the other two oxalate ligands are non-bridging. In the crystal, intermolecular hydrogen bonds involving oxalate ligands, water molecules and pyridinium cations, build a complex three-dimensional network. Variable-temperature magnetic susceptibility measurements for 1 and 2 indicate a weak ferromagnetic interaction (J = +1.16 and +2.62/+2.70 cm(-1) for 1 and 2, respectively) between the two terminal Cr(III) (S(Cr) = 3/2) and the central high-spin Mn(II) (S(Mn) = 5/2) and Co(II) (S(Co) = 3/2) ions. The nature and the amplitude of the exchange interaction are rationalized using DFT calculations and orbital interpretations.

  8. Six-coordinate oxo-vanadium(V) dimer complex with methoxy bridging: synthesis, crystal structure, biological activity and molecular docking

    Czech Academy of Sciences Publication Activity Database

    Heidari, F.; Fatemi, S.J.A.; Yousef Ebrahimipour, S.; Ebrahimnejad, H.; Castro, J.; Dušek, Michal; Eigner, Václav

    2017-01-01

    Roč. 76, Feb (2017), s. 1-4 ISSN 1387-7003 R&D Projects: GA MŠk(CZ) LO1603; GA ČR(CZ) GA14-03276S EU Projects: European Commission(XE) CZ.2.16/3.1.00/24510 Institutional support: RVO:68378271 Keywords : oxo-vanadium(V) * Schiff base complex * antimicrobial activity * X-ray crystal structure Subject RIV: CA - Inorganic Chemistry OBOR OECD: Inorganic and nuclear chemistry Impact factor: 1.640, year: 2016

  9. Synthesis, spectral and luminescence study, crystal structure determination and DFT calculation of binuclear palladium(II) complexes

    Science.gov (United States)

    Seyfi, S.; Alizadeh, R.; Darvish Ganji, M.; Amani, V.

    2018-02-01

    Binuclear palladium(II) complexes with metal-metal (d8-d8) bonding interaction were synthesized by reactions of the 1-methyl-1H-1,2,3,4-tetrazole-5-thiol (Hmtzt) or a mixture of Hmtzt and 1,3-propanediamine (1,3-pda) ligands. Complex [Pd2(μ-mtzt)4]·2CH3CN (1) was synthesized by the reaction of Pd(OAc)2 with Hmtzt dissolved in acetonitrile and complex [Pd2(μ-mtzt)2(mtzt)2(1,3-pda)] (2) was synthesized by reaction of a mixture of Hmtzt and 1,3-propanediamine (dissolved in methanol) with PdCl2 (dissolved in acetonitrile) and were identified through elemental analysis, IR, UV-Vis, 1H NMR, luminescence spectroscopy as well as single-crystal X-ray diffraction method. A single-crystal of complex 1 shows that two Pd(II) centers are linked together by four bridging tetrazole ligands providing a paddle wheel-like arrangement. Also a crystal structure of complex 2 shows that this complex possesses a symmetric structure in which one Pd atom is tetra-coordinated by four sulfur atoms to forms PdS4 and other Pd atom is tetra-coordinated by four nitrogen to forms PdN4 coordination sphere. Density functional theory (DFT) was performed in this study for the Hmtzt ligand and binuclear palladium(II) complexes (1) and (2). The DFT calculation shows PdII-PdII bond lengths of 2.831 and 3.086 Å in complex 1 and 2, respectively which are close to the observed bond lengths of 2.802(11) and 3.0911(17) Å from single-crystal X-ray structure. The optimized geometry of the complexes is shown good agreement by X-ray data. Structural properties and molecular descriptors including bond lengths, bond angles, chemical hardness, dipole moment, HOMO-LUMO energy levels, electron transfer were analyzed. The IR spectroscopy was performed using VEDA4 software and UV-Vis spectra were analyzed using time-dependent density functional theory (TD-DFT) method. The theoretical and experimental data were also compared with each other.

  10. Synthesis and crystal structure of a homoleptic diruthenium complex containing tetra-2-pyridyl-1,4-pyrazine (tppz)

    Energy Technology Data Exchange (ETDEWEB)

    Graf, Marion; Mayer, Peter; Boettcher, Hans-Christian [Muenchen Univ. (Germany). Dept. Chemie

    2017-07-01

    Treatment of hydrated ruthenium(III) chloride with tetra-2-pyridyl-1,4-pyrazine (tppz) in refluxing ethoxyethanol afforded the homoleptic dinuclear complex [(tppz)Ru(μ-tppz)Ru(tppz)]{sup 4+} (1) besides small amounts of the species [Ru(tppz){sub 2}]{sup 2+}. The title complex 1 was obtained as purple crystals and characterized as its hexafluoridophosphate salt by NMR spectroscopy, mass spectrometry and microanalyses. The molecular structure of 1(PF{sub 6}){sub 4} has been established by X-ray crystallography.

  11. Synthesis of NaCl Single Crystals with Defined Morphologies as Templates for Fabricating Hollow Nano/micro-structures

    DEFF Research Database (Denmark)

    Wang, B.B.; Jin, P.; Yue, Yuanzheng

    2015-01-01

    Hollow nanostructures have a wide range of applications in nanotechnology. To accurately fabricate such nanostructures, the first and common key step is to synthesize high quality templates with controlled symmetry and geometry, ideally through a green, efficient, and economical approach. However....... These naturally abundant NaCl single crystal templates are water-soluble, environmentally-friendly and uniform in both geometry and size, and hence are ideal for preparing high quality hollow nano/micro structures. The new approach may have the potential to replace the conventional hard or soft template...

  12. Synthesis, spectral and luminescence study, crystal structure determination and DFT calculation of binuclear palladium(II) complexes.

    Science.gov (United States)

    Seyfi, S; Alizadeh, R; Darvish Ganji, M; Amani, V

    2018-02-05

    Binuclear palladium(II) complexes with metal-metal (d 8 -d 8 ) bonding interaction were synthesized by reactions of the 1-methyl-1H-1,2,3,4-tetrazole-5-thiol (Hmtzt) or a mixture of Hmtzt and 1,3-propanediamine (1,3-pda) ligands. Complex [Pd 2 (μ-mtzt) 4 ]·2CH 3 CN (1) was synthesized by the reaction of Pd(OAc) 2 with Hmtzt dissolved in acetonitrile and complex [Pd 2 (μ-mtzt) 2 (mtzt) 2 (1,3-pda)] (2) was synthesized by reaction of a mixture of Hmtzt and 1,3-propanediamine (dissolved in methanol) with PdCl 2 (dissolved in acetonitrile) and were identified through elemental analysis, IR, UV-Vis, 1 H NMR, luminescence spectroscopy as well as single-crystal X-ray diffraction method. A single-crystal of complex 1 shows that two Pd(II) centers are linked together by four bridging tetrazole ligands providing a paddle wheel-like arrangement. Also a crystal structure of complex 2 shows that this complex possesses a symmetric structure in which one Pd atom is tetra-coordinated by four sulfur atoms to forms PdS 4 and other Pd atom is tetra-coordinated by four nitrogen to forms PdN 4 coordination sphere. Density functional theory (DFT) was performed in this study for the Hmtzt ligand and binuclear palladium(II) complexes (1) and (2). The DFT calculation shows Pd II -Pd II bond lengths of 2.831 and 3.086Å in complex 1 and 2, respectively which are close to the observed bond lengths of 2.802(11) and 3.0911(17)Å from single-crystal X-ray structure. The optimized geometry of the complexes is shown good agreement by X-ray data. Structural properties and molecular descriptors including bond lengths, bond angles, chemical hardness, dipole moment, HOMO-LUMO energy levels, electron transfer were analyzed. The IR spectroscopy was performed using VEDA4 software and UV-Vis spectra were analyzed using time-dependent density functional theory (TD-DFT) method. The theoretical and experimental data were also compared with each other. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Synthesis and crystal structure of 4-(2-ammonioethylmorpholin-4-ium dichloridodiiodidocadmate/chloridotriiodidocadmate (0.90/0.10

    Directory of Open Access Journals (Sweden)

    Najla Mahbouli Rhouma

    2016-10-01

    Full Text Available The crystal structure of the title compound, (C6H16N2O[CdCl1.90I2.10], a new organic–inorganic hybrid salt synthesized in the form of single crystals, consists of discrete statistically distributed dichloridodiiodidocadmate/chloridotriiodidocadmate anions (occupancy ratio 0.90:0.10 and 4-(2-ammonioethylmorpholin-4-ium cations, [NH3(CH22NH(CH24O]2+. The cations are linked by intermolecular N—H...O hydrogen bonds, forming corrugated chains extending parallel to the c axis. The [CdCl1.90I2.10]2− tetrahalidocadmate anions lie between the chains to maximize the electrostatic interactions and are connected with the organic cations via N—H...Cl and C—H...Cl(I hydrogen bonds developing in the ab plane and leading to the formation of a three-dimensional network structure. The tetracoordinate CdII atom has a distorted tetrahedral conformation, with a τ4 index of 0.87.

  14. Hydrothermal synthesis and crystal Structure of a new coordination polymer: [Zn1(deta(btec(H2O2]n

    Directory of Open Access Journals (Sweden)

    Manel Halouani

    2013-05-01

    Full Text Available A new metal–organic compound [Zn1(deta(btec(H2O2]n where (deta= Diethylenetriamine and (btec= benzenetetracarboxylic acid (I was hydrothermally synthesized from an aqueous solution of Zn(NO32 6H2O, (deta and (btec. Compound I crystallizes in the monoclinic system with the P21/c space group. The unit cell parameters are a= 9.6716(5Å, b= 14.3776(8Å, c= 13.5306(8Å, β= 105.311(3°, Z= 4, V= 1814.71(18 Å3 and Dx= 1.657 g/cm3. The refinement converged into R= 0.045, Rw= 0.048. The structure, determined by single crystal X-ray diffraction, consists of a network of ZnO4 centers, tetrahedrally coordinated by pyromellitate anions giving rise to a two-dimensional sheet structure. The connectivity resembles a 4-connected network in which each Zn atom is connected to four btec anions and each btec anion is linked to four Zn2+ ions.

  15. Synthesis, crystal structure and physical properties of europium - manganese fluoride pnictides, EuMnPnF (Pn = P, As, Sb)

    Science.gov (United States)

    Plokhikh, I. V.; Charkin, D. O.; Verchenko, V. Yu.; Kuznetsov, A. N.; Tsirlin, A. A.; Kazakov, S. M.; Shevelkov, A. V.

    2018-02-01

    The quaternary compounds EuMnPnF (Pn = P, As, Sb) have been prepared via solid state route at 1173 K, and their crystal and electronic structures as well as magnetic and transport properties have been elucidated. These compounds belong to the widespread LaAgSO structure type and crystallize in tetragonal (P4/nmm) unit cells with a = 4.0292(1) Å, c = 8.9505(2) Å for EuMnPF, a = 4.1227(1) Å, c = 9.0846(2) Å for EuMnAsF, and a = 4.3120(1) Å, c = 9.4356(2) Å for EuMnSbF. At low temperatures, the magnetic response is dominated by Eu2+. Contrary to previous reports, we do not observe any magnetic transitions in EuMnPF down to 2 K, whereas its arsenide and antimonide analogs exhibit Eu2+ ordering around 3 K. According to the electrical resistivity measurements and density-functional calculations, all three compounds are narrow-gap semiconductors.

  16. Flux synthesis, modulated crystal structures, and physical properties of REMn0.5SeO (RE = La, Ce)

    International Nuclear Information System (INIS)

    Peschke, Simon; Johrendt, Dirk; Nitsche, Fabian

    2015-01-01

    The selenide oxides REMn 0.5 SeO (RE = La, Ce) were synthesized by heating RE 2 O 3 , RE, Mn, and Se in a NaI/KI flux at 800 C, and their modulated crystal structures determined by X-ray single crystal and powder diffraction {P 1 1 2/n(αβ1/2)0s, Z = 2, LaMn 0.5 SeO: a = 405.7(1), b = 405.7(1), c = 915.2(1) pm, γ = 90 , q = [1/10, -1/10, 1/2]; CeMn 0.5 SeO: a = 402.0(1), b = 401.8(1), c = 910.7(1) pm, γ = 90.000(4) , q = [0.0789(2), -0.0783(2), 1/2]}. The structures are related to the ZrCuSiAs-type structure with ordered vacancies at the manganese sites. The resulting modulations of the checkerboard pattern in the [Mn 0.5 Se] layers can be approximated by 10a x 10b x 2c and 51a x 51b x 2c supercells in LaMn 0.5 SeO and CeMn 0.5 SeO, respectively. Both compounds are insulators. The optical bandgap of LaMn 0.5 SeO was determined to 2.13 eV from the Kubelka-Munk function. Magnetic measurements indicate antiferromagnetic ordering of the Mn 2+ moments with Neel points well above room temperature, as known from related manganese compounds. (Copyright copyright 2015 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  17. Synthesis, crystal structure and properties of a new lead fluoride borate, Pb{sub 3}OBO{sub 3}F

    Energy Technology Data Exchange (ETDEWEB)

    Zhao, Wenwu [Xinjiang Key Laboratory of Electronic Information Materials and Devices, Xinjiang Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, 40-1 South Beijing Road, Urumqi 830011 (China); Graduate School of the Chinese Academy of Sciences, Beijing 100049 (China); Pan, Shilie, E-mail: slpan@ms.xjb.ac.cn [Xinjiang Key Laboratory of Electronic Information Materials and Devices, Xinjiang Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, 40-1 South Beijing Road, Urumqi 830011 (China); Dong, Xiaoyu [Xinjiang Key Laboratory of Electronic Information Materials and Devices, Xinjiang Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, 40-1 South Beijing Road, Urumqi 830011 (China); Graduate School of the Chinese Academy of Sciences, Beijing 100049 (China); Li, Junjie; Tian, Xuelin; Fan, Xiaoyun [Xinjiang Key Laboratory of Electronic Information Materials and Devices, Xinjiang Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, 40-1 South Beijing Road, Urumqi 830011 (China); Chen, Zhaohui [Xinjiang Key Laboratory of Electronic Information Materials and Devices, Xinjiang Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, 40-1 South Beijing Road, Urumqi 830011 (China); Physical and Chemical Detecting Center, Xinjiang University, Urumqi 830046 (China); Zhang, Fangfang [Xinjiang Key Laboratory of Electronic Information Materials and Devices, Xinjiang Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, 40-1 South Beijing Road, Urumqi 830011 (China)

    2012-04-15

    Graphical abstract: The structure of Pb{sub 3}OBO{sub 3}F consists of two distortional Pb-centered tetrahedra and BO{sub 3} triangles which are all symmetrical with each other respectively in the gestalt structure to the extent that the Pb{sub 3}OBO{sub 3}F compound crystallizes in the symmetrical space group. Highlights: Black-Right-Pointing-Pointer Pb{sub 3}OBO{sub 3}F has been grown from PbO-PbF{sub 2}-B{sub 2}O{sub 3} system for the first time. Black-Right-Pointing-Pointer It crystallizes in the orthorhombic system, space group Pbcm. Black-Right-Pointing-Pointer Pb{sub 3}OBO{sub 3}F consists of Pb(1)O{sub 3}F tetrahedra, Pb(2)O{sub 4} tetrahedra and BO{sub 3} triangles. -- Abstract: A new compound, Pb{sub 3}OBO{sub 3}F, has been grown by the high temperature solution method from the PbO-PbF{sub 2}-B{sub 2}O{sub 3} system. It crystallizes in the orthorhombic system, space group Pbcm with unit-cell parameters a = 7.6313(14) Angstrom-Sign , b = 6.5229(12) Angstrom-Sign , c = 11.906(2) Angstrom-Sign , Z = 4, volume = 592.66(19) Angstrom-Sign {sup 3}. The structure of the compound is solved by the direct methods and refined to R{sub 1} = 0.0528 and wR{sub 2} = 0.1400. Pb{sub 3}OBO{sub 3}F consists of Pb(1)O{sub 3}F tetrahedra, Pb(2)O{sub 4} tetrahedra and BO{sub 3} triangles which build up the symmetrical chains extended along the c-axis. The powder X-ray diffraction pattern of the Pb{sub 3}OBO{sub 3}F has been measured. Functional groups presented in the sample were identified by Fourier transform infrared spectrum.

  18. New mixed valence defect dicubane cobalt(II)/cobalt(III) complex: Synthesis, crystal structure, photoluminescence and magnetic properties

    Science.gov (United States)

    Coban, Mustafa Burak; Gungor, Elif; Kara, Hulya; Baisch, Ulrich; Acar, Yasemin

    2018-02-01

    A new defect dicubane cobalt(II)/cobalt(III), [(CoII2CoIII2L42(H2O)(CH3COO)(CH3COOH]. 4H2O complex (1) where H2L = [1-(3-hydroxypropyliminomethyl)naphthalene-2-ol], has been synthesized and characterized by element analysis, FT-IR, solid UV-Vis spectroscopy and single crystal X-ray diffraction. The crystal structure determination shows a cationic tetrameric arrangement consisting of a defect dicubane core with two missing vertexes. Each cobalt ion has a distorted octahedral geometry with six coordinate ordered CoII and CoIII ions. The solid state photoluminescence properties of complex (1) and its ligand H2L have been investigated under UV light at 349 nm in the visible region. H2L exhibits blue emission while complex (1) shows red emission at room temperature. Variable-temperature magnetic susceptibility measurements on the complex (1) in the range 2-300 K indicate an antiferromagnetic interaction.

  19. 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.

  20. Synthesis, crystal structures, molecular docking and urease inhibition studies of Ni(II) and Cu(II) Schiff base complexes

    Science.gov (United States)

    Sangeeta, S.; Ahmad, K.; Noorussabah, N.; Bharti, S.; Mishra, M. K.; Sharma, S. R.; Choudhary, M.

    2018-03-01

    [Ni(L)2] 1 and [Cu(L)2] 2 [HL = 2-((E)-(2-methoxyphenylimino)methyl)-4,6-dichlorophenol] Schiff base complexes have been successfully synthesized and were characterized by FT-IR, UV-Vis, fluorescence spectroscopy and thermogravimetric analysis. The crystal structures of the two complexes were determined through X-ray crystallography. Its inhibitory activity against Helicobacter pylori urease was evaluated in vitro and showed strong inhibitory activity against H. pylori urease compared with acetohydroxamic acid (IC50 = 42.12 μmolL-1), which is a positive reference. A docking analysis using the AutoDock 4.0 program could explain the inhibitory activity of the complex against urease.

  1. Iron(II) tris(3-bromo-1,10-phenanthroline) complex:synthesis, crystal structure and electropolymerization

    CERN Document Server

    Lee, K J; Lee, S S; Lee, B Y

    2002-01-01

    The complex of iron(II) tris(3-Br-phen)(3-Br-phen; 3-bromo-1,10-phenanthroline) was prepared as a precursor of electropolymerization and the crystal structure of [Fe(3-Br-phen) sub 3](PF sub 6) sub 2 centre dot CH sub 3 CN with a distorted octahedral geometry has been investigated. The reductive electropolymerization of [Fe(3-Br-phen) sub 3] sup 2 sup + complex onto the surface of a glassy carbon electrode and indium tin oxide (ITO) optically transparent electrode were performed in acetonitrile at room temperature. Thin film of poly-[Fe(3-Br-phen) sub 3] sup 2 sup + formed was adherent, electroactive and stably deposited on a glassy carbon disk electrode. The thin metallopolymeric film formed was also confirmed by absorption spectroscopy.

  2. Synthesis, Crystal Structure, and Antimicrobial Properties of a Novel 1-D Cobalt Coordination Polymer with Dicyanamide and 2-Aminopyridine

    Directory of Open Access Journals (Sweden)

    Amah Colette Benedicta Yuoh

    2015-01-01

    Full Text Available A novel one-dimensional coordination polymer bis(2-aminopyridine-μ-bis(dicyanamido cobaltate(II has been synthesized and characterized by elemental analyses and infrared and ultraviolet visible spectroscopies and the structure has been determined by single crystal X-ray diffraction. Co(II ion in the complex is coordinated to two axial 2-aminopyridine ligands through the pyridine N-atom and four equatorial dicyanamide ligands to give a CoN6 slightly distorted octahedral coordination environment around the metal ion. The amino N-atom forms intrachain hydrogen bonds. Antimicrobial screening of the complex against eight pathogenic microorganisms (four bacteria and four fungi isolated from humans, indicates that the complex is moderately active.

  3. Unprecedented Hexanuclear Cobalt(II Nonsymmetrical Salamo-Based Coordination Compound: Synthesis, Crystal Structure, and Photophysical Properties

    Directory of Open Access Journals (Sweden)

    Zong-Li Ren

    2018-03-01

    Full Text Available A novel hexanuclear Co(II coordination compound with a nonsymmetrical Salamo-type bisoxime ligandH4L, namely [{Co3(HL(MeO(MeOH2(OAc2}2]·2MeOH, was prepared and characterized by elemental analyses, UV–vis, IR and fluorescence spectra, and X-ray single-crystal diffraction analysis. Each Co(II is hexacoordinated, and possesses a distorted CoO6 or CoO4N2 octahedrons. The Co(II coordination compound possesses a self-assembled infinite 2D supramolecular structure with the help of the intermolecular C–H···O interactions. Meanwhile, the photophysical properties of the Co(II coordination compound were studied.

  4. Synthesis, crystal structures, fluorescence and xanthine oxidase inhibitory activity of pyrazole-based 1,3,4-oxadiazole derivatives

    Science.gov (United States)

    Qi, De-Qiang; Yu, Chuan-Ming; You, Jin-Zong; Yang, Guang-Hui; Wang, Xue-Jie; Zhang, Yi-Ping

    2015-11-01

    A series of pyrazole-based 1,3,4-oxadiazole derivatives were rationally designed and synthesized in good yields by following a convenient route. All the newly synthesized molecules were fully characterized by IR, 1H NMR and elemental analysis. Eight compounds were structurally determined by single crystal X-ray diffraction analysis. The fluorescence properties of all the compounds were investigated in dimethyl sulfoxide media. In addition, these newly synthesized compounds were evaluated for in vitro inhibitory activity against commercial enzyme xanthine oxidase (XO) by measuring the formation of uric acid from xanthine. Among the compounds synthesized and tested, 3d and 3e were found to be moderate inhibitory activity against commercial XO with IC50 = 72.4 μM and 75.6 μM. The studies gave a new insight in further optimization of pyrazole-based 1,3,4-oxadiazole derivatives with excellent fluorescence properties and XO inhibitory activity.

  5. Synthesis, spectral characterization and crystals structure of some arsane derivatives of gold (I complexes: a comparative density functional theory study.

    Directory of Open Access Journals (Sweden)

    Omar Bin Shawkataly

    Full Text Available A series of complexes of the type LAuCl where L = tris(p-tolylarsane, tris(m-tolylarsane, bis(diphenylarsanoethane, and tris(naphthylarsane have been synthesized. All of the new complexes, 1-4, have been fully characterized by means of ¹H NMR and ¹³C NMR spectroscopy and single crystal X-ray crystallography. The structures of complexes 1-4 have been determined from X-ray diffraction data. The linear molecules have an average bond distance between gold-arsenic and gold-chlorine of 2.3390Å and 2.2846Å, respectively. Aurophilic interaction was prominent in complex 1 and 3, whereas complex 2 and 4 do not show any such interaction. The intermolecular gold interaction bond length was affected by the electronegativity of the molecule. The computed values calculated at DFT level using B3LYP function are in good agreement with the experimental results.

  6. Synthesis, crystal structure, antibacterial activities, and electrochemical studies of new N,N‧-polymethylene bis-sulfonamides

    Science.gov (United States)

    Özbek, Neslihan; Alyar, Saliha; Mamaş, Serhat; Şahin, Ertan; Karacan, Nurcan

    2012-02-01

    Four disulfonamide derivatives (C2H5·SO2·NH)2(CH2)n (n = 2, 3, 4, 5) were synthesized and characterized by FTIR, 1H NMR, 13C NMR, HETCOR, LCMS and elemental analysis. Ethanesulfonamide-N,N'-pentamethylene bis was also characterized by X-ray single crystal diffraction measurement. The electrochemical characteristics of the disulfonamide derivatives were performed by cyclic voltammetry and chronoamperometry. 1H and 13C NMR chemical shifts of the compounds were calculated by using DFT/B3LYP methods with a 6-311++G (d,p) basis set. Antibacterial activity and the structural relationship of the compounds showed that activity decreases proportionately to the increasing length of the carbon chain between NH groups, log P values, hydration energy and molecular volumes. Anodic peak potentials and HOMO values do not correlate with the activity, but reduction potential and LUMO decrease weakly with increasing activity.

  7. Synthesis and crystal structure of the iridium(I) carbene complex with a pair of hydrogen wing tips

    Energy Technology Data Exchange (ETDEWEB)

    Huang, H.-Y.; Chen, Z.-M.; Wang, Y.; Wu, E.-M.; Wang, G. [Jiangsu Institute of Nuclear Medicine, Ministry of Health, Key Laboratory of Molecular Nuclear Medicine (China); Jiang, M.-J., E-mail: jmj16888@126.com [Nanjing Medical University, Affiliated Wuxi Peoples Hospital, Wuxi Institute of Translational Medicine, Department of Clinical Laboratory Science (China)

    2016-12-15

    The iridium(I) cyclooctadiene complex with two (3-tert-butylimidazol-2-ylidene) ligands [(H-Im{sup t}Bu){sub 2}Ir(COD)]{sup +}PF{sub 6}{sup −} (C{sub 22}H{sub 32}PF{sub 6}IrN{sub 4}) has been prepared, and its crystal structure is determined by X-ray diffraction. Complex exhibits slightly distorted square planar configurations around the metal atom, which is coordinated by two H-Im{sup t}Bu ligands and one cyclooctadiene group. The new iridium carbene complex has a pair of hydrogen wing tips. The Ir−C{sub carbene} bond lengths are 2.066(5) and 2.052(5) Å, and the bond angle C−Ir−C between these bonds is 95.54(19)°. The dihedral angle between two imidazol-2-ylidene rings is 86.42°.

  8. Synthesis, crystal structure and biological activity of the Schiff base organotin(IV) complexes based on salicylaldehyde-o-aminophenol

    Science.gov (United States)

    Tan, Yu-Xing; Zhang, Zhi-Jian; Liu, Yang; Yu, Jiang-Xi; Zhu, Xiao-Ming; Kuang, Dai-Zhi; Jiang, Wu-Jiu

    2017-12-01

    Schiff base organotin(IV) complexes C1 ∼ C5b have been synthesized via the reaction of the substituted salicylaldehyde-o-aminophenol Schiff base ligands (L1 ∼ L3) with the dibenzyltin dichloride, n-butyltin trichloride or dibutyltin oxide, respectively. The complexes have been characterized by IR, UV-Vis, 1H NMR, 13C NMR spectra, elemental analysis and the crystal structures have been determined by X-ray diffraction. The anticancer activity of the Schiff base ligand and complexes C1 ∼ C5b against five species of cancer cell which are Hela, MCF7, HepG2, Colo205, NCIsbnd H460 were tested respectively, the tests showed that C1 ∼ C5b exhibited significant anticancer activity for the cancer cells in comparison with the ligand, and the activity was greater than carboplatin.

  9. Cerium(III) pivalate [Ce(Piv)3(HPiv)3]2: synthesis, crystal structure, and thermal stability

    International Nuclear Information System (INIS)

    Khudyakov, M.Yu.; Kuz'mina, N.P.; Pisarevskij, A.P.; Martynenko, L.I.

    2002-01-01

    Complex [Ce(Piv) 3 (HPiv) 3 ] 2 was prepared by precipitation of cerium(III) nitrate aqueous solution with salt NH 4 (Piv) (HPiv = pivalic acid) and subsequent recrystallization from 5% HPiv solution in hexane. According to data of X-ray diffraction analysis and IR spectroscopy crystal structure of the complex is built of centrally symmetric dimers, in which cerium atoms are bound by four bridge pivalate ligands. Thermal analysis suggests that heating of the complex in nitrogen atmosphere results first in splitting off six HPiv molecules in the range of 90-190 deg C and then in thermolysis of Ce(Piv) 3 formed at 290-450 deg C. Sublimation of Ce(Piv) 3 occurs in the range of 290-350 deg C along with thermolysis during heating in vacuum (0.01 mm Hg), which permits preparing CeO 2 films by the method of chemical precipitation from gaseous phase [ru

  10. Surfactant-controlled composition and crystal structure of manganese(II sulfide nanocrystals prepared by solvothermal synthesis

    Directory of Open Access Journals (Sweden)

    Elena Capetti

    2015-12-01

    Full Text Available We investigated how the outcome of the solvothermal synthesis of manganese(II sulfide (MnS nanocrystals (NCs is affected by the type and amount of long chain surfactant present in the reaction mixture. Prompted by a previous observation that a larger than stoichiometric amount of sulfur is required [Puglisi, A.; Mondini, S.; Cenedese, S.; Ferretti, A. M.; Santo, N.; Ponti A. Chem. Mater. 2010, 22, 2804–2813], we carried out a wide set of reactions using Mn(II carboxylates and Mn2(CO10 as precursors with varying amounts of sulfur and carboxylic acid. MnS NCs were obtained provided that the S/Mn ratio was larger than the L/Mn ratio, otherwise MnO NCs were produced. Since MnS can crystallize in three distinct phases (rock salt α-MnS, zincblende β-MnS, and wurtzite γ-MnS, we also investigated whether the surfactant affected the NC polymorphism. We found that MnS polymorphism can be controlled by appropriate selection of the surfactant. γ-MnS nanocrystals formed when a 1:2 mixture of long chain carboxylic acid and amine was used, irrespective of the presence of carboxylic acid as a free surfactant or ligand in the metal precursor. When we used a single surfactant (carboxylic acid, alcohol, thiol, amine, α-MnS nanocrystals were obtained. The peculiar role of the amine seems to be related to its basicity. The nanocrystals were characterized by TEM and electron diffraction; ATR-FTIR spectroscopy provided information about the surfactants adsorbed on the NCs.

  11. Synthesis, solution and crystal structure of the coenzyme B(12) analogue Co(β)-2'-fluoro-2',5'-dideoxyadenosylcobalamin.

    Science.gov (United States)

    Hunger, Miriam; Wurst, Klaus; Kräutler, Bernhard

    2015-07-01

    Crystal structure analyses have helped to decipher the mode of binding of coenzyme B12 (AdoCbl) in the active site of AdoCbl-dependent enzymes. However, the question of how such enzymes perform their radical reactions is still incompletely answered. A pioneering study by Gruber and Kratky of AdoCbl-dependent glutamate mutase (GLM) laid out a path for the movement of the catalytically active 5'-deoxyadenosyl radical, in which H-bonds between the protein and the 2'- and 3'-OH groups of the protein bound AdoCbl would play a decisive role. Studies with correspondingly modified coenzyme B12-analogues are of interest to gain insights into cofactor binding and enzyme mechanism. Here we report the preparation of Coβ-2'-fluoro-2',5'-dideoxyadenosylcobalamin (2'FAdoCbl), which lacks the 2'-OH group critical for the interaction in enzymes. 2'FAdoCbl was prepared by alkylation of cob(I)alamin, obtained from the electrochemical reduction of aquocobalamin. Spectroscopic data and a single crystal X-ray analysis of 2'FAdoCbl established its structure, which was very similar to that one of coenzyme B12. 2'FAdoCbl is a (19)F NMR active mimic of coenzyme B12 that may help to gain insights into binding interactions of coenzyme B12 with AdoCbl-dependent enzymes, proteins of B12 transport and of AdoCbl-biosynthesis, as well as with B12-riboswitches. Copyright © 2015 Elsevier Inc. All rights reserved.

  12. Synthesis, Crystal Structure, and Biological Activity of cis/trans Amide Rotomers of (Z-N′-(2-Oxoindolin-3-ylideneformohydrazide

    Directory of Open Access Journals (Sweden)

    Hatem A. Abdel-Aziz

    2014-01-01

    Full Text Available (Z-N′-(2-Oxoindolin-3-ylideneformohydrazide (2 was synthesized by the reaction of (Z-3-hydrazonoindolin-2-one (1 with formic acid under reflux. The structure of 2 was characterized by IR, Mass, 1H NMR, and X-ray crystal structure determination. Interestingly, compound 2 appeared in DMSO-d6 as cis and trans amide rotomers in 25% and 75%, respectively. The X-ray analysis showed the Z geometrical isomer of 2 around –C=N– for cis and trans amide rotomers. The crystal of 2 belongs to monoclinic, space group P21/c, with a=4.5206 (1 Å, b=22.4747 (7 Å, c=17.3637 (5 Å, β=103.752 (1°, Z=8, V=1713.57 (8 Å3, Dc=1.467 Mg m−3, μ=0.11 mm−1, F(000=784, R=0.047, and wR=0.123 for 3798 observed reflections with I>2σ(I. Compound 2 exhibited a moderate activity in its antimicrobial evaluation against E. coli and P. aeruginosa and a good activity against S. aureus close to that of the standard drug ciprofloxacin. The in vitro anticancer activity of 2 was evaluated against two human tumor cell lines, namely, HepG2 hepatocellular carcinoma and MCF-7 breast cancer. HepG2 cancer cell line was more susceptible to compound 2 than MCF-7.

  13. Synthesis by two methods and crystal structure determination of a new pyrochlore-related compound Sm{sub 2}FeTaO{sub 7}

    Energy Technology Data Exchange (ETDEWEB)

    Torres-Martinez, Leticia M., E-mail: lettorresg@yahoo.com [Departamento de Ecomateriales y Energia, Facultad de Ingenieria Civil, Universidad Autonoma de Nuevo Leon, Cd. Universitaria, San Nicolas de los Garza, Nuevo Leon 66450 (Mexico); Ruiz-Gomez, Miguel A. [Departamento de Ecomateriales y Energia, Facultad de Ingenieria Civil, Universidad Autonoma de Nuevo Leon, Cd. Universitaria, San Nicolas de los Garza, Nuevo Leon 66450 (Mexico); Facultad de Ciencias Quimicas, Universidad Autonoma de San Luis Potosi, Av. Manuel Nava 6, San Luis Potosi, S.L.P. 78290 (Mexico); Figueroa-Torres, M.Z.; Juarez-Ramirez, Isaias [Departamento de Ecomateriales y Energia, Facultad de Ingenieria Civil, Universidad Autonoma de Nuevo Leon, Cd. Universitaria, San Nicolas de los Garza, Nuevo Leon 66450 (Mexico); Moctezuma, Edgar [Facultad de Ciencias Quimicas, Universidad Autonoma de San Luis Potosi, Av. Manuel Nava 6, San Luis Potosi, S.L.P. 78290 (Mexico); and others

    2012-04-16

    Graphical abstract: The monoclinic (space group C2/c) structure of a new compound, Sm{sub 2}FeTaO{sub 7} shows an alternating Sm-O and Fe/Ta-O layers. In the Fe/Ta-O layer, Fe/Ta1 and Fe/Ta3 cations are coordinated by six oxygen atoms, forming irregular octahedral interconnected into a hexagonal tungsten bronze (HTB) type network. The HTB layer is a fundamental framework in the pyrohlore-related structure. Highlights: Black-Right-Pointing-Pointer Pyrochlore-related compound Sm{sub 2}FeTaO{sub 7} prepared by solid state reaction and sol-gel. Black-Right-Pointing-Pointer Sm{sub 2}FeTaO{sub 7} crystallizes with a monoclinic crystal structure and space group C2/c. Black-Right-Pointing-Pointer The compound is synthesized by sol-gel at lower temperature and time than solid state. Black-Right-Pointing-Pointer Surface area of sol-gel Sm{sub 2}FeTaO{sub 7} is 10 times higher than that prepared by solid state. - Abstract: This paper reports on the synthesis of a new pyrochlore-related compound Sm{sub 2}FeTaO{sub 7} by both solid state reaction and sol-gel synthesis routes. Structural features were determined by X-ray powder diffraction and Rietveld refinement and were corroborated using Transmission Electron Microscopy (TEM). The results revealed that Sm{sub 2}FeTaO{sub 7} crystallized in the monoclinic system with space group C2/c and the following cell parameters: a = 13.1307(5) Angstrom-Sign , b = 7.5854(3) Angstrom-Sign , c = 11.6425(4) Angstrom-Sign and {beta} = 100.971(2) Degree-Sign . The monoclinic structure of Sm{sub 2}FeTaO{sub 7} showed an arrangement of alternating Sm-O and Fe/Ta-O layers and two types of irregular octahedra of Fe/Ta-O, which are interconnected into a hexagonal tungsten bronze (HTB)-type network. On the other hand, Sm{sub 2}FeTaO{sub 7} prepared by sol-gel was obtained with lower particle sizes than the solid state produced compound. The difference in particle size causes a difference of one order of magnitude in the specific surface area. In

  14. Hydrothermal synthesis, crystal structures, and luminescent properties of a series of new lanthanide oxalatophosphonates with a layer architecture.

    Science.gov (United States)

    Zhu, Yan-Yu; Sun, Zhen-Gang; Tong, Fei; Liu, Zhong-Min; Huang, Cui-Ying; Wang, Wei-Nan; Jiao, Cheng-Qi; Wang, Cheng-Lin; Li, Chao; Chen, Kai

    2011-05-28

    Eleven new lanthanide oxalatophosphonate hybrids with a 2D layered structures, namely, [Ln(H(3)L)(C(2)O(4))]·2H(2)O (Ln = La-Dy, Er and Y, H(4)L = C(6)H(5)CH(2)N(CH(2)PO(3)H(2))(2)), have been synthesized under hydrothermal conditions and structurally characterized by X-ray single-crystal diffraction, X-ray powder diffraction, infrared spectroscopy, elemental analysis and thermogravimetric analysis. Compounds 1-11 are isomorphous and they exhibit a 2D framework structure. Two {LnO(8)} polyhedra and four {CPO(3)} tetrahedra are interconnected into a unit via corner-sharing, and the so-built units are bridged by the oxalate anions into a layer. The result of connections in this manner is the formation of a 24-atom window. The thermal stabilities and guest desorption-sorption properties of compounds 1-11 have been investigated. The luminescent properties of compounds 5, 6, 8 and 9 have also been studied.

  15. Synthesis, crystal structure, cytotoxic, antileishmanial activities and docking studies on N,N‧-(ethane-1,2-diyl)bis(3-methylbenzamide)

    Science.gov (United States)

    Aziz, Hamid; Saeed, Aamer; Jabeen, Farukh; Simpson, Jim; Munawar, Amna; Qasim, Muhammad

    2018-03-01

    Amide derivatives have gained considerable attention because of their extensive range of biological activities and pharmaceutical applications. The current paper presents the synthesis of N, N‧-(ethane-1,2-diyl) bis (3-methylbenzamide), (I), its molecular and crystal structure and an evaluation of its likely biological activity, including cytotoxicity (LD50 = 37.21 μg/ml) and antileishmanial activity (IC50 = 5.77 μg/ml). Moreover, a docking simulation was used to determine the possible interaction sites of the compound (I) with TryR, an enzyme involved in the redox metabolism of the leishmania parasite. Docking computations demonstrate that the compound established prominent binding interactions with the key residues of the TryR and possess the potential to effectively inhibit the catalytic activities of the enzyme. Thus the results suggest that this compound can serve as a potential scaffold for the treatment of leishmaniasis and deserves further development.

  16. Versatile and green synthesis, spectroscopic characterizations, crystal structure and DFT calculations of 1,2,3‒triazole‒based sulfonamides

    Science.gov (United States)

    Saeidian, Hamid; Sadighian, Hamed; Abdoli, Morteza; Sahandi, Morteza

    2017-03-01

    A green, and practically reliable method for the synthesis of novel 1,2,3‒triazole-based sulfonamides via copper (I)‒catalyzed azide‒alkyne [3 + 2] cycloaddition reaction was reported. The desired products were characterized by CHN analysis, FT-IR, 1H and 13C NMR, ESI-MS spectroscopy, single crystal X-ray diffraction and density functional theory (DFT) geometry optimization and molecular orbital calculations. Mild and green reaction conditions, atom-economic and high yields (61-91%) make this protocol an attractive option for the synthesis of 1,2,3‒triazoles bearing sulfonamide moiety. Geometrical structures, vibrational frequencies, 1H and 13C chemical shift values, Mulliken charge distribution and electrophilicity index (HOMO-LUMO analysis) of the characterized structure of 3f in the ground state have been calculated with the aid of DFT studies. The calculated chemical shifts (NMR) and vibrational frequencies (FT-IR) are in compliance with the experimental findings. The aim of the DFT study was to make a reasonable assignment of vibrational bands and chemical shifts.

  17. Synthesis, Crystal Structure, and Cytotoxic Activity of a Novel Eight-Coordinated Dinuclear Ca(II-Schiff Base Complex

    Directory of Open Access Journals (Sweden)

    Xi-Shi Tai

    2016-09-01

    Full Text Available A novel eight-coordinated dinuclear Ca(II complex, [Ca2(L2(H2O10]·H2O (L = 4-formylbenzene-1,3-disulfonate-3-pyridinecarboxylic hydrazone (1, was synthesized by the reaction of 3-pyridinecarboxylic hydrazide, disodium 4-formylbenzene-1,3-disulfonate, and Ca(ClO42·4H2O in ethanol-water solution (v:v = 3:1 at 50 °C. Complex 1 was characterized by elemental analysis, IR, 1H-NMR, 13C-NMR, and X-ray single crystal diffraction analysis. Dinuclear Ca(II complex 1 belongs to triclinic, space group P-1 with a = 7.186(3 Å, b = 11.978(5 Å, c = 12.263(5 Å, α = 90.318(5°, β = 91.922(5°, γ = 96.797(5°, V = 1047.5(8 Å3, Z = 1, Dc = 1.685 mg·m−3, μ = 0.572 mm−1, F(000 = 552, and final R1 = 0.0308, ωR2 = 0.0770. Dinuclear Ca(II molecules form a 1D chained structure by π–π stacking interaction. The 1D chains form a 3D framework structure by the π–π stacking interaction and hydrogen bonds. The in vitro cytotoxic activity activity of 1 against HL-60 and MLTC-1 was also investigated.

  18. Synthesis, Crystal Structure, Luminescence and Magnetism of Three Novel Coordination Polymers Based on Flexible Multicarboxylate Zwitterionic Ligand

    Directory of Open Access Journals (Sweden)

    Yulu Ma

    2017-01-01

    Full Text Available Three novel zwitterionic coordination polymers, namely, {[Zn(HCbdcp2]·H2O} (1, {[Mn(Cbdcp]·3H2O} (2 and {[Cu2(Cbdcp(HCbdcpCl·H2O]·2H2O} (3, Cbdcp = 3,5-dicarboxy-1-(4-carboxybenzylpyridin-1-ium, have been prepared by a hydrothermal method and characterized by X-ray single crystal diffraction analysis, powder X-ray diffraction analysis, IR spectroscopy, and thermogravimetric analysis. With the changing of metal centers, these complexes show distinct structures: a mononuclear 2D 44-sql network for 1, a 3D 6,6-connected-type topology for 2 and a novel dinuclear 2D layer for 3. These diverse architectures prove that coordination geometry of metal ions, coordination modes of carboxylate groups and the rotationally flexible CH2 linker played significant roles in the construction of CPs; moreover, they also indicated that H3CbdcpCl is an ideal organic candidate for the building of novel structures. The solid-state luminescent properties of complexes 1–3 were investigated, respectively. In addition, the magnetic properties of 2 and 3 were studied and both of them exhibit antiferromagnetic behaviors.

  19. Synthesis, crystal structure and theoretical analysis of intermolecular interactions in two biologically active derivatives of 1,2,4-triazoles

    Science.gov (United States)

    Shukla, Rahul; Mohan, T. P.; Vishalakshi, B.; Chopra, Deepak

    2017-04-01

    In the present study, we have synthesized and structurally characterized two biologically active derivatives of 1,2,4 triazoles, namely 3-(4-fluoro-3-phenoxyphenyl)-1-(piperidin-1-ylmethyl)-1H-1,2,4-triazole-5(4H)-thione (TR) and 1-((3-(4-fluoro-3-phenoxyphenyl)-5-(methylthio)-1H-1,2,4-triazol-1-yl)methyl)piperidine (TR1) via single crystal X-ray diffraction. Both the structures show the presence of various intermolecular interactions in the crystalline solid such as Csbnd H…F, Csbnd H…S, Csbnd H…N, Csbnd H…O, Csbnd H … π, and π … π intermolecular interactions. The role of these interactions in molecular packing was analyzed, and the nature of these interactions was evaluated through computational procedures using PIXEL. Hirshfeld analysis further reveals that the contribution of H…F interactions was more prominent towards packing as compared to H…N/O intermolecular interactions.

  20. Synthesis, crystal structures and antitumor activities of copper(II) complexes with a 2-acetylpyrazine isonicotinoyl hydrazone ligand

    Science.gov (United States)

    Xu, Jun; Zhou, Tao; Xu, Zhou-Qing; Gu, Xin-Nan; Wu, Wei-Na; Chen, Hong; Wang, Yuan; Jia, Lei; Zhu, Tao-Feng; Chen, Ru-Hua

    2017-01-01

    Five complexes, [Cu(L)2]·4.5H2O (1), [Cu(HL)2](NO3)2·CH3OH (2) {[Cu2(L)2(NO3)(H2O)2]·(NO3)}n (3), [Cu2(HL)2(SO4)2]·2CH3OH (4) and [Cu4(L)4Cl4]·5H2O (5) based on HL (where HL = 2-acetylpyrazine isonicotinoyl hydrazone) have been synthesized and characterized by X-ray diffraction analyses. The counter anion and organic base during the synthesis procedure influence the structures of the complexes efficiently, which generate five complexes as mono-, bi-, tetra-nuclear and one-dimensional structures. The antitumor activities of the complexes 1-5 (except for complex 3 with the poor solubility) against the Patu8988 human pancreatic cancer, ECA109 human esophagus cancer and SGC7901 human gastric cancer cell lines are screened by MTT assay. The results indicate that the chelation of Cu(II) with the ligand is responsible for the observed high cytotoxicity of the copper(II) complexes and the 1:2 copper species 1 and 2 demonstrate lower antitumor activities than that of the 1:1 copper species 4 and 5. In addition, the in vitro apoptosis inducing activity of the copper(II) complex 5 against SGC7901 cell line is determined. And the results show that the complex can bring about apoptosis of the cancerous cells in vitro.

  1. Hydrothermal synthesis of cubic boron nitride crystals

    International Nuclear Information System (INIS)

    Yu Meiyan; Cui Deliang; Kai Li; Yin Yansheng; Wang Qilong; Lei Chu

    2005-01-01

    Cubic boron nitride (cBN) crystals have been successfully synthesized by in situ hydrothermal method. In order to obtain cBN pure phase crystals, two comparative experiments were carried out. The experimental results indicated that compared to one-step in situ hydrothermal method, multi-step in situ hydrothermal method was beneficial to the synthesis of cBN. It is believed that the multi-step in situ hydrothermal method is the optimal route to synthesize pure cBN bulk crystals

  2. Influence of synthesis conditions on the crystal structure of the powder formed in the ZrO2 - Ce2O3/CeO2 system

    International Nuclear Information System (INIS)

    Popov, V V; Menushenkov, A P; Khubbutdinov, R M; Sharapov, A S; Svetogorov, R D; Zubavichus, Ya V; Kurilkin, V V

    2016-01-01

    Influence of synthesis conditions (type of atmosphere, reduction and oxidation, annealing temperature) on the chemical composition and structure of the compounds formed in the “ZrO 2 - Ce 2 O 3 / CeO 2 ” system has been investigated by X-ray absorption fine structure (XAFS) spectroscopy combined with X-ray diffraction (XRD) and thermogravimetric analysis (TGA). It is revealed that isothermal annealing of precursor at temperatures less than 1000 °C in air leads to formation of Ce 0.5 Zr 0.5 O 2 powders with cubic fluorite-type structure (Fm-3m). Further increase of annealing temperatures above 1000 °C causes decomposition of formed crystal structure into two phases: cubic and tetragonal. Annealing in reduction hydrogen atmosphere causes formation of Ce 4 + 2xCe 3 + 2-2xZr 2 O 7 + x compounds with intermediate valency of cerium, where value of x depends on the reducing conditions and treatment parameters of precursor. Annealing in vacuum at 1400 °C strongly reduces the content of Ce 4 + in a powder samples and leads to formation of pyrochlore structure (space group Fd-3 m ) with practically Ce 3+ valence state. (paper)

  3. Synthesis, structural, X-ray photoelectron spectroscopy (XPS) studies and IR induced anisotropy of Tl{sub 4}HgI{sub 6} single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Parasyuk, O.V. [Department of Inorganic and Physical Chemistry, Lesya Ukrainka Eastern European National University, Voli Ave. 13, Lutsk, 43025 (Ukraine); Khyzhun, O.Y. [Frantsevych Institute for Problems of Materials Science, National Academy of Sciences of Ukraine, 3 Krzhyzhanivsky St., 03142, Kyiv (Ukraine); Piasecki, M. [Institute of Physics, J. Dlugosz University Częstochowa, Armii Krajowej 13/15, Częstochowa (Poland); Kityk, I.V., E-mail: iwank74@gmail.com [Electrical Engineering Department, Czestochowa University Technology, Armii Krajowej 17, PL-42-217, Czestochowa (Poland); Lakshminarayana, G. [Wireless and Photonic Networks Research Centre, Faculty of Engineering, Universiti Putra Malaysia, 43400, Serdang, Selangor (Malaysia); Luzhnyi, I. [Frantsevych Institute for Problems of Materials Science, National Academy of Sciences of Ukraine, 3 Krzhyzhanivsky St., 03142, Kyiv (Ukraine); Fochuk, P.M. [Yuriy Fed’kovych Chernivtsi National University, 2 Kotziubynskoho Str., 58012, Chernivtsi (Ukraine); Fedorchuk, A.O. [Department of Inorganic and Organic Chemistry, Lviv National University of Veterinary Medicine and Biotechnologies, Pekarska Street 50, 79010, Lviv (Ukraine); Levkovets, S.I.; Yurchenko, O.M.; Piskach, L.V. [Department of Inorganic and Physical Chemistry, Lesya Ukrainka Eastern European National University, Voli Ave. 13, Lutsk, 43025 (Ukraine)

    2017-02-01

    In the present work, we report on the synthesis and structural properties including X-ray protoelectron spectroscopy (XPS) analysis of Tl{sub 4}HgI{sub 6} crystals that were grown by Bridgman-Stockbarger method up to 80 mm in length and 18 mm in diameter. The existence of the ternary compound Tl{sub 4}HgI{sub 6} that melts incongruently at 641 K was confirmed. Phase equilibria and structural properties for the TlI–HgI{sub 2} system were investigated by differential thermal analysis (DTA) and X-ray diffraction (XRD) methods. X-ray photoelectron spectra were measured for both pristine and Ar{sup +} ion-bombarded Tl{sub 4}HgI{sub 6} single crystal surfaces. The data reveal that the Tl{sub 4}HgI{sub 6} single crystal is sensitive with respect to Ar{sup +} ion-bombardment as 3.0 keV Ar{sup +} irradiation over 5 min at an ion current density 14 μA/cm{sup 2} induces changes to the elemental stoichiometry of the Tl{sub 4}HgI{sub 6} surface, leading to a decrease of the mercury content in the topmost surface layers. X-ray photoelectron spectroscopy (XPS) measurements indicate very low hygroscopic nature of the Tl{sub 4}HgI{sub 6} single crystal surface. The IR coherent bicolor laser treatment at wavelengths 10.6/5.3 μm has shown an occurrence of anisotropy at wavelengths 1540 nm of Er:glass laser. This may open the applications of Tl{sub 4}HgI{sub 6} as a material for IR laser triggering. - Highlights: • Phase diagram of the HgI{sub 2}–TlI system was built. • Tl{sub 4}HgI{sub 6} single crystals were grown by Bridgman Stockbarger method. • XRD, XPS analysis was done. • Ir induced anisotropy was established. • The compounds may be proposed as Ir laser operated polarizers.

  4. 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...

  5. Demonstration of Crystal Structure.

    Science.gov (United States)

    Neville, Joseph P.

    1985-01-01

    Describes an experiment where equal parts of copper and aluminum are heated then cooled to show extremely large crystals. Suggestions are given for changing the orientation of crystals by varying cooling rates. Students are more receptive to concepts of microstructure after seeing this experiment. (DH)

  6. Synthesis, crystal structures, luminescence and catalytic properties of two d¹⁰ metal coordination polymers constructed from mixed ligands.

    Science.gov (United States)

    Wang, Xiao-xiao; Zhang, Ming-xi; Yu, Baoyi; Van Hecke, Kristof; Cui, Guang-hua

    2015-03-15

    Two new coordination polymers [Cd(bmb)(hmph)]n (1), {[Ag(bmb)]·H2btc}n (2) (bmb=1,4-bis(2-methylbenzimidazol-1-ylmethyl)benzene, H2hmph=homophthalic acid, H3btc=1,3,5-benzenetetracarboxylic acid) were synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction methods, IR spectroscopy, TGA, XRPD and elemental analysis. Complex 1 features a 3D threefold interpenetrating dia array with a 4-connected 6(6) topology. Complex 2 shows a 1D helix chain structure connected by L1 ligands, which is finally extended into a rarely 2D 4L2 supramolecular network via C-H⋯O hydrogen bond interactions. In addition, the luminescence and catalytic properties of the two complexes for the degradation of the methyl orange azo dye in a Fenton-like process were presented. The degradation efficiency of the methyl orange azo dye for 1 and 2 are 56% and 96%, respectively. Copyright © 2014 Elsevier B.V. All rights reserved.

  7. Synthesis, crystal structure, electric and magnetic properties of LaVO2.78N0.10

    International Nuclear Information System (INIS)

    Yoon, Songhak; Maegli, Alexandra E.; Karvonen, Lassi; Shkabko, Andrey; Populoh, Sascha; Sagarna, Leyre; Aguirre, Myriam H.; Pokrant, Simone; Galazka, Krzysztof; Jakes, Peter; Eichel, Ruediger A.; Ebbinghaus, Stefan G.; Weidenkaff, Anke

    2014-01-01

    Perovskite-type LaVO 2.78 N 0.10 powder was synthesized by thermal ammonolysis of the oxide precursor LaVO 4 . By X-ray, neutron, and electron diffraction an orthorhombic crystal structure with space group Pnma was identified. XANES spectra showed that the oxidation state of vanadium changes from 5+ in LaVO 4 to approximately 3+ in LaVO 2.78 N 0.10 . The temperature dependence of the electrical conductivity revealed an Arrhenius-type behavior with an activation energy of 0.103 eV in the temperature range of 119-302 K indicating that the conduction process is thermally activated band transition. Based on the positive Seebeck coefficient, holes were identified as the dominant charge carriers in the temperature range of 100-302 K. Both the Seebeck coefficient and the thermal conductivity showed an anomaly at 138 K, which is attributed to the Neel temperature for antiferromagnetic ordering according to magnetic susceptibility measurements. (Copyright copyright 2014 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  8. Synthesis, Crystal Structure, and Physical Properties of New Layered Oxychalcogenide La2O2Bi3AgS6

    Science.gov (United States)

    Hijikata, Yudai; Abe, Tomohiro; Moriyoshi, Chikako; Kuroiwa, Yoshihiro; Goto, Yosuke; Miura, Akira; Tadanaga, Kiyoharu; Wang, Yongming; Miura, Osuke; Mizuguchi, Yoshikazu

    2017-12-01

    We have synthesized a new layered oxychalcogenide La2O2Bi3AgS6. From synchrotron X-ray diffraction and Rietveld refinement, the crystal structure of La2O2Bi3AgS6 was refined using a model of the P4/nmm space group with a = 4.0644(1) Å and c = 19.412(1) Å, which is similar to the related compound LaOBiPbS3, while the interlayer bonds (M2-S1 bonds) are apparently shorter in La2O2Bi3AgS6. The tunneling electron microscopy (TEM) image confirmed the lattice constant derived from Rietveld refinement (c ˜ 20 Å). The electrical resistivity and Seebeck coefficient suggested that the electronic states of La2O2Bi3AgS6 are more metallic than those of LaOBiS2 and LaOBiPbS3. The insertion of a rock-salt-type chalcogenide into the van der Waals gap of BiS2-based layered compounds, such as LaOBiS2, will be a useful strategy for designing new layered functional materials in the layered chalcogenide family.

  9. Synthesis, characterization, X-ray crystal structures of heterocyclic Schiff base compounds and in vitro cholinesterase inhibition and anticancer activity

    Science.gov (United States)

    Arafath, Md. Azharul; Adam, Farook; Al-Suede, Fouad Saleih R.; Razali, Mohd R.; Ahamed, Mohamed B. Khadeer; Abdul Majid, Amin Malik Shah; Hassan, Mohd Zaheen; Osman, Hasnah; Abubakar, Saifullah

    2017-12-01

    Four heterocyclic embedded Schiff base derivatives (1-4) were synthesized and characterized by melting point, elemental analysis, FTIR, 1H, 13C NMR, UV-Visible spectral data. The structures of compounds 1, 2 and 4 were successfully established through single crystal X-ray diffraction analysis. In vitro cholinesterase inhibition assays showed that the cyclized derivative 1 displayed higher BuChE enzyme inhibitory activity with IC50 value of 1.45 ± 0.09 μM. The anti-proliferative efficacies of the compounds were also evaluated using human colorectal HCT 116 and breast MCF-7 adenocarcinoma cell lines. In addition, a human normal endothelial cell line (Ea.hy926) was also tested to assess the safety and selectivity of the compounds towards normal and cancer cells, respectively. Among the compounds tested, compound 2 displayed potent cytotoxic effect (IC50 = 34 μM) against HCT 116 cells with highest selectivity index of 3.1 with respect to the normal endothelial cells. Whereas, compound 4 exhibited significant anti-proliferative effect (IC50 = 21.1 μM) against MCF-7 cells with highest selectivity index of 3.3 with respect to the normal endothelial cells. The docking result of these compounds against hAChE showed potent activities with different binding modes. These compounds could be a promising pharmacological agent to treat cancer and Alzheimer's disease.

  10. Synthesis, Crystal Structures, and Photoluminescent Properties of Two Supramolecular Architectures Based on Difunctional Ligands Containing Imidazolyl and Carboxyl Groups

    Directory of Open Access Journals (Sweden)

    Mei-An Zhu

    2017-07-01

    Full Text Available Two new supramolecular architectures, namely, [Cd(L12(H2O]n (1 and [Ni(L22(H2O]n (2, were synthesized by the reaction of corresponding metal salts of CdCl2·2.5H2O and NiCl2·6H2O with 2-(1H-imidazol-4-ylbenzoic acid (HL1 and 3-(1H-imidazol-4-ylbenzoic acid (HL2 respectively, and characterized by single-crystal X-ray diffraction, IR spectroscopy, elemental analysis and powder X-ray diffraction (PXRD. Both HL1 and HL2 ligands are deprotonated to be L1- and L2- anions that coordinate with Cd(II and Ni(II atoms to form two-dimensional (2D layer structure. Topologically, complex 1 is a 2D network with (4, 4 sql topology, while 2 is a typical 63-hcb topology net. Complex 1 exhibits intense light blue emission in the solid state at room temperature.

  11. Controllable synthesis, crystal structure and magnetic properties of Monomer-Dimer Cocrystallized MnIII Salen-type composite material

    Science.gov (United States)

    Wu, Qiong; Wu, Wei; Wu, Yongmei; Li, Weili; Qiao, Yongfeng; Wang, Ying; Wang, Baoling

    2018-04-01

    By the reaction of manganese-Schiff-base complexes with penta-anionic Anderson heteropolyanion, a new supramolecular architecture [Mn2(Salen)2(H2O)2][Mn(Salen)(H2O)2]2Na[IMo6O24]·8H2O (1) (salen = N,N‧-ethylene-bis (salicylideneiminate) has been isolated. Compound 1 was characterized by the single-crystal X-ray diffraction, elemental, IR and thermal gravimetric analyses. Structural analysis reveals that the unit cell simultaneously contains MnIII-Salen dimer and monomer cation fragments, for which the Anderson-type polyanions serve as counter anions. In the packing arrangement, all the MnIII dimers are well separated by polyoxometalate units and form tertiary structure together with MnIII monomers. Interestingly, different from the previous work, in the exact same reaction conditions, we are able to template MnIII-Salen complexes into different configurations by varying the charge state of polyanions. Besides, the magnetic properties of 1 were also examined by using both dc and ac magnetic field of the superconducting quantum interference devices. Most importantly, our fitting of the experimental data to a Heisenberg-type spin model shows that there exists a ferromagnetic exchange interaction ∼5 K between the spins (S = 2) on MnIII in the dimer, while antiferromagnetic ones exist among monomers and dimer (∼2 K). This meta-magnetic state could induce a slight spin frustration at low temperature, which would in turn affect the magnetic behavior. In addition, our ac field measurement of the susceptibilities suggests a typical signature for a single-molecule magnet.

  12. Crystal structure of the human primase.

    Science.gov (United States)

    Baranovskiy, Andrey G; Zhang, Yinbo; Suwa, Yoshiaki; Babayeva, Nigar D; Gu, Jianyou; Pavlov, Youri I; Tahirov, Tahir H

    2015-02-27

    DNA replication in bacteria and eukaryotes requires the activity of DNA primase, a DNA-dependent RNA polymerase that lays short RNA primers for DNA polymerases. Eukaryotic and archaeal primases are heterodimers consisting of small catalytic and large accessory subunits, both of which are necessary for RNA primer synthesis. Understanding of RNA synthesis priming in eukaryotes is currently limited due to the lack of crystal structures of the full-length primase and its complexes with substrates in initiation and elongation states. Here we report the crystal structure of the full-length human primase, revealing the precise overall organization of the enzyme, the relative positions of its functional domains, and the mode of its interaction with modeled DNA and RNA. The structure indicates that the dramatic conformational changes in primase are necessary to accomplish the initiation and then elongation of RNA synthesis. The presence of a long linker between the N- and C-terminal domains of p58 provides the structural basis for the bulk of enzyme's conformational flexibility. Deletion of most of this linker affected the initiation and elongation steps of the primer synthesis. © 2015 by The American Society for Biochemistry and Molecular Biology, Inc.

  13. Mixed thio/oxo orthovanadates Na3[VSxO4-x] (x = 2, 3): Synthesis - crystal structures - properties

    International Nuclear Information System (INIS)

    Schnabel, S.; Roehr, C.

    2005-01-01

    Mixed sodium thio/oxo orthovanadates(V), dark red Na 3 [VS 3 O] and orange red Na 3 [VS 2 O 2 ], were synthesized via reactions in the melt starting from V, Na, Na 2 S, Na 2 O and sulfur. The structure of the low temperature phase of Na 3 [VS 3 O] (space group Pnma, a = 589.5(3), b = 962.8(5), c = 1186.6(6) pm, Z = 4, R1 = 0.0494) contains anions [VS 3 O] 3- almost identical to those known from the high temperature form, β-Na 3 [VS 3 O] (space group Cmc2 1 , a = 968.4(4), b = 1194.6(4), c = 590.5(2) pm, Z = 4, R1 = 0.0291). The second order phase transition between these two forms at 536 C was studied by temperature dependent powder diffraction and explained on the basis of a comparison of the anion packing in the two related structures. The packing of the dithiodioxovanadate anions in Na 3 [VS 2 O 2 ] (space group Pbca, a = 1162.7(2), b = 592.71(12), c = 1766.7(4) pm, Z = 8, R1 = 0.0312) is also closely related. The chemical bonding in the anions [VS 3 O] 3- and [VS 2 O 2 ] 3- of approximately ideal C 3v and C 2v symmetry is discussed on the basis of FP-LAPW band structure calculations and force constants obtained from Raman spectroscopy. The decrease of the calculated band gaps with increasing S content x in Na 3 [VS x O 4-x ] is in accordance with the optical properties showing a gradually deepening of the crystal and solution colour. Discernible trends in the chemical bonding in this series of mixed thio-oxo anions also include the amount of π bonding of the V-O and V-S bonds and the corresponding variation of force constants and V-O/V-S distances. (orig.)

  14. Synthesis and crystal structure of a chiral aromatic amine chloride salt (C8H12N)Cl

    Science.gov (United States)

    Ben Salah, A. M.; Naїli, H.; Mhiri, T.; Bataille, T.

    2015-12-01

    The new organic chloride salt incorporating an aromatic primary amine with a chiral functional group, (S)-α-methylbenzylammonium), has been synthesized by slow evaporation method at room temperature. The crystals are trigonal with non-centrosymmetric sp. gr. R3. The crystal packing is determined by N-H···Cl hydrogen bonds and C-H···π interactions between the aromatic rings of the organic moieties, resulting in supramolecular architecture.

  15. Synthesis, X-Ray Crystal Structures, Biological Evaluation, and Molecular Docking Studies of a Series of Barbiturate Derivatives

    Directory of Open Access Journals (Sweden)

    Assem Barakat

    2016-01-01

    Full Text Available A series of barbiturates derivatives synthesized and screened for different set of bioassays are described. The molecular structures of compounds 5a, 5d, and 5f were solved by single-crystal X-ray diffraction techniques. The results of bioassay show that compounds 4a, 4b, 4c, 4d, 4e, 4f, and 4g are potent antioxidants in comparison to the tested standards, butylated hydroxytoluene (BHT, and N-acetylcysteine. Compounds 4a–4e (IC50=101.8±0.8–124.4±4.4 μM and 4g (IC50=104.1±1.9 μM were more potent antioxidants than the standard (BHT, IC50=128.8±2.1 μM. The enzyme inhibition potential of these compounds was also evaluated, in vitro, against thymidine phosphorylase, α-glucosidase, and β-glucuronidase enzymes. Compounds 4c, 4h, 4o, 4p, 4q, 5f, and 5m were found to be potent α-glucosidase inhibitors and showed more activity than the standard drug acarbose, whereas compounds 4v, and 5h were found to be potent thymidine phosphorylase inhibitors, more active than the standard drug, 7-deazaxanthine. All barbiturates derivatives (4a–4x, 4z, and 5a–5m were found to be noncytotoxic against human prostate (PC-3, Henrietta Lacks cervical (HeLa and Michigan Cancer Foundation-7 breast (MCF-7 cancer cell lines, and 3T3 normal fibroblast cell line, except 4y which was cytotoxic against all the cell lines.

  16. Synthesis, Crystal Structure and Luminescent Property of Cd (II Complex with N-Benzenesulphonyl-L-leucine

    Directory of Open Access Journals (Sweden)

    Xishi Tai

    2012-09-01

    Full Text Available A new trinuclear Cd (II complex [Cd3(L6(2,2-bipyridine3] [L = N-phenylsulfonyl-L-leucinato] has been synthesized and characterized by elemental analysis, IR and X-ray single crystal diffraction analysis. The results show that the complex belongs to the orthorhombic, space group P212121 with a = 16.877(3 Å, b = 22.875(5 Å, c = 29.495(6 Å, α = β = γ = 90°, V = 11387(4 Å3, Z = 4, Dc= 1.416 μg·m−3, μ = 0.737 mm−1, F (000 = 4992, and final R1 = 0.0390, ωR2 = 0.0989. The complex comprises two seven-coordinated Cd (II atoms, with a N2O5 distorted pengonal bipyramidal coordination environment and a six-coordinated Cd (II atom, with a N2O4 distorted octahedral coordination environment. The molecules form one dimensional chain structure by the interaction of bridged carboxylato groups, hydrogen bonds and p-p interaction of 2,2-bipyridine. The luminescent properties of the Cd (II complex and N-Benzenesulphonyl-L-leucine in solid and in CH3OH solution also have been investigated.

  17. High-pressure synthesis, crystal structure and magnetic properties of double perovskite oxide Ba2CuOsO6

    International Nuclear Information System (INIS)

    Feng, Hai L.; Arai, Masao; Matsushita, Yoshitaka; Tsujimoto, Yoshihiro; Yuan, Yahua; Sathish, Clastin I.; He, Jianfeng; Tanaka, Masahiko; Yamaura, Kazunari

    2014-01-01

    A new compositional double perovskite oxide Ba 2 CuOsO 6 was synthesized under high-pressure (6 GPa) and high-temperature (1500 °C) conditions. The polycrystalline Ba 2 CuOsO 6 was characterized by synchrotron X-ray diffraction, thermogravimetric analysis, and magnetic susceptibility, isothermal magnetization, and specific heat measurements. The oxide crystallizes in a double-perovskite structure with an I4/m space group, in which Os(VI) and Cu(II) are ordered in the perovskite B-site. Ba 2 CuOsO 6 is electrically insulating with an activation energy of 0.813(2) eV and shows antiferromagnetic-like characteristics at temperatures of ∼55 K and ∼70 K. The results of the first-principle calculation suggested that the spin–orbit interaction of Os(VI) plays a substantial role in the insulating state. The Jahn–Teller distortion of CuO 6 octahedra influences the magnetic characteristics with regard to possible two-dimensional magnetic correlations. - Graphical abstract: A new compositional double perovskite oxide Ba 2 CuOsO 6 synthesized by a high-pressure (6 GPa) and high-temperature (1500 °C) method. - Highlights: • A new compositional double perovskite oxide Ba 2 CuOsO 6 was synthesized. • Ba 2 CuOsO 6 is electrically insulating and antiferromagnetic below ∼70 K. • The Jahn–Teller distortion of CuO 6 has relevance to possible magnetic anisotropy

  18. Synthesis and Crystal Structure of Binuclear and Pentanuclear Nickel(II Complexes Containing 4-(salicylaldiminatoantipyrine Schiff base

    Directory of Open Access Journals (Sweden)

    Mohamed N. EL-Kaheli

    2015-11-01

    Full Text Available The new title binuclear Ni (II compound  (1 and the novel pentanuclear Ni (II cluster {[   } (2 are formed from the reaction of an asymmetric Schiff base ligand L (L = 4-(salicylaldiminatoantipyrine with Ni .4  in the former or Ni(ClO42.6H2O in presence of malonate in the later.  Complex (1 consists of ( ]+ cation and one uncoordinated tetraphenylborate anion.  The cation adopts a distorted octahedral arrangement around each metal center.  In the binuclear unit both Ni(II ions are linked through two phenolate (µ2-O oxygen atoms of L, and two oxygen atoms of a  bridging carboxylate group. Each Ni (II coordinates to four oxygen atoms at the basal plane, two oxygen atoms from two bridging phenolate groups, one from pyrazolone ring and the last of an aqua molecule, and at the axial positions to a bridging carboxylate-O atom and an azomethine nitrogen atom.  In the pentanuclear cluster (2 consisting of [ ]+2 cation and two tetraphenylborate anions, the core of the cation is assembled by four [Ni( ] units, linked to the central Ni-ion by two bridging water molecules. The resulting coordination sphere for the external symmetry related nickel ions is a pseudo octahedron.  The central Ni-atom unusually adopts dodecahedron geometry through its coordination to eight bridging water molecules. In complex (1 each Ni-atom is coordinated to one tridentate L ligand and in complex (2 each [Ni ( ] unit is coordinated to two bidentate L ligands.  Inter-and intramolecular hydrogen bonds are present in both crystal structures.

  19. Synthesis, crystal structures and luminescence properties of new multi-component co-crystals of isostructural Co(II) and Zn(II) complexes

    Science.gov (United States)

    Tella, Adedibu C.; Owalude, Samson O.; Omotoso, Mary F.; Olatunji, Sunday J.; Ogunlaja, Adeniyi S.; Alimi, Lukman O.; Popoola, Olugbenga K.; Bourne, Susan A.

    2018-04-01

    Two novel isostructural compounds containing multi-component co-crystals [M(C6H4NO2)2(H2O)2](C9H6O6)2 (M = Co (1), Zn (2), C6H4NO2 = Picolinic acid, C9H6O6 = Trimesic acid) have been synthesized. The compounds were characterized by elemental analysis, FT-IR, UV-Visible and 1H NMR spectroscopies as well as thermal and single crystal X-ray diffraction analyses. Single crystal X-ray diffraction analysis reveals that 1 and 2 are isostructural. Compound 1 crystallizes in triclinic space group (P-1, with a = 5.154 (10) Å, b = 11.125 (2) Å, c = 14.113 (3) Å, α = 91.01 (3)°, β = 100.54 (3)°, and γ = 102.71 (3)°). In a similar fashion, compound 2 crystallizes in triclinic space group (P-1, with a = 5.1735 (3) Å, b = 11.0930 (10) Å, c = 14.1554 (8) Å, α = 91.70 (3)°, β = 100.26 (3)°, γ = 102.90 (3)°). The metal (II) cation presents distorted MN2O4 octahedral geometry with H2O molecules coordinated to the metal in equatorial position while the picolinic acid molecules are axially coordinated through the pyridine N atom. The two trimesic acid molecules are not part of the first coordination sphere. Compounds 1 and 2 constitute an example of a class of coordination compound of multicomponent crystals having trimesic acid outside the coordination sphere where it is neither protonated or deprotonated. The two compounds were investigated for luminiscence properties.

  20. Crystal structure determination of Efavirenz

    International Nuclear Information System (INIS)

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

    2015-01-01

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

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

    Czech Academy of Sciences Publication Activity Database

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

    2017-01-01

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

  2. Synthesis and X-ray crystal structure of the first tetrathiafulvalene-based acceptor-donor-acceptor sandwich

    DEFF Research Database (Denmark)

    Simonsen, Klaus B.; Thorup, Niels; Cava, Michael P.

    1998-01-01

    The synthesis and characterization of a bis-macrocyclic A-D-A sandwich produced in a simple one-pot reaction is reported. Only one acceptor unit participates in charge-transfer interactions with the TTF unit in the solid state....

  3. Synthesis, crystal structure and charge-distribution validation of β-Na4Cu(MoO43 adopting the alluadite structure-type

    Directory of Open Access Journals (Sweden)

    Wassim Dridi

    2016-08-01

    Full Text Available Single crystals of a new variety of tetrasodium copper(II tris[molybdate(VI], Na4Cu(MoO43, have been synthesized by solid-state reactions and characterized by single-crystal X-ray diffraction. This alluaudite structure-type is characterized by the presence of infinite layers of composition (Cu/Na2Mo3O14 parallel to the (100 plane, which are linked by MoO4 tetrahedra, forming a three-dimensional framework containing two types of hexagonal channels in which Na+ cations reside. The Cu2+ and Na2+ cations are located at the same general site with occupancies of 0.5. All atoms are on general positions except for one Mo, two Na (site symmetry 2 and another Na (site symmetry -1 atom. One O atom is split into two separate positions with occupancies of 0.5. The title compound is isotypic with Na5Sc(MoO44 and Na3In2As3O12. The structure model is supported by bond-valence-sum (BVS and charge-distribution CHARDI methods. β-Na4Cu(MoO43 is compared and discussed with the K4Cu(MoO43 and α-Na4Cu(MoO43 structures.

  4. 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

  5. Reverse micelles directed synthesis of TiO{sub 2}-CeO{sub 2} mixed oxides and investigation of their crystal structure and morphology

    Energy Technology Data Exchange (ETDEWEB)

    Matejova, Lenka, E-mail: matejova@icpf.cas.cz [Institute of Chemical Process Fundamentals of the ASCR, v. v. i., Department of Catalysis and Reaction Engineering, Rozvojova 135, 165 02 Prague 6 (Czech Republic); Vales, Vaclav [Charles University in Prague, Faculty of Mathematics and Physics, Department of Condensed Matter Physics, Ke Karlovu 5, 121 16 Prague 2 (Czech Republic); Fajgar, Radek [Institute of Chemical Process Fundamentals of the ASCR, v. v. i., Department of Aerosols and Laser Studies, Rozvojova 135, 165 02 Prague 6 (Czech Republic); Matej, Zdenek; Holy, Vaclav [Charles University in Prague, Faculty of Mathematics and Physics, Department of Condensed Matter Physics, Ke Karlovu 5, 121 16 Prague 2 (Czech Republic); Solcova, Olga [Institute of Chemical Process Fundamentals of the ASCR, v. v. i., Department of Catalysis and Reaction Engineering, Rozvojova 135, 165 02 Prague 6 (Czech Republic)

    2013-02-15

    The synthesis of TiO{sub 2}-CeO{sub 2} mixed oxides based on the sol-gel process controlled within reverse micelles of non-ionic surfactant Triton X-114 in cyclohexane is reported. The crystallization, phase composition, trends in nanoparticles growth and porous structure properties are studied as a function of Ti:Ce molar composition and annealing temperature by in-situ X-ray diffraction, Raman spectroscopy and physisorption. The brannerite-type CeTi{sub 2}O{sub 6} crystallizes as a single crystalline phase at Ti:Ce molar composition of 70:30 and in the mixture with cubic CeO{sub 2} and anatase TiO{sub 2} for composition 50:50. At Ti:Ce molar ratios 90:10 and 30:70 the mixtures of TiO{sub 2} anatase, rutile and cubic CeO{sub 2} appear. In these mixtures TiO{sub 2} rutile is formed at higher temperatures than conventionally. Additionally, the amount of a present amorphous phase in individual mixtures was estimated from diffraction data. The porous structure morphology depends both on molar composition and annealing temperature. This is correlated with the presence of carbon impurities of different character. - Graphical abstract: The phase composition of Ti90--Ce10 and Ti50--Ce50 oxide mixtures as a function of annealing temperature. The amount of the amorphous phase was estimated and attributed to TiO{sub 2}. Highlights: Black-Right-Pointing-Pointer Ti/Ce oxides were prepared using reverse micelles of Triton X-114. Black-Right-Pointing-Pointer Crystallization of TiO{sub 2}, CeO{sub 2} or CeTi{sub 2}O{sub 6} depends on Ti:Ce molar ratio. Black-Right-Pointing-Pointer Amorphous phase attributed to TiO{sub 2} was identified. Black-Right-Pointing-Pointer Metal oxides surface area is influenced by the character of present carbon impurities.

  6. Synthesis, Crystal Structure, DFT Studies and Evaluation of the Antioxidant Activity of 3,4-Dimethoxybenzenamine Schiff Bases

    Directory of Open Access Journals (Sweden)

    Ahmad Nazif Aziz

    2014-06-01

    Full Text Available Schiff bases of 3,4-dimethoxybenzenamine 1–25 were synthesized and evaluated for their antioxidant activity. All the synthesized compounds were characterized by various spectroscopic techniques. In addition, the characterizations of compounds 13, 15 and 16 were supported by crystal X-ray determinations and their geometrical parameters were compared with theoretical DFT calculations at the B3LYP level of theory. Furthermore, the X-ray crystal data of two non-crystalline compounds 8 and 18 were theoretically calculated and compared with the practical values of compounds 13, 15, 16 and found a good agreement. The compounds showed good DPPH scavenging activity ranging from 10.12 to 84.34 μM where compounds 1–4 and 6 showed stronger activity than the standard n-propyl gallate. For the superoxide anion radical assay, compounds 1–3 showed better activity than the standard.

  7. A new cadmium(II) complex with bridging dithiolate ligand: Synthesis, crystal structure and antifungal activity study

    Science.gov (United States)

    Singh, Mahesh Kumar; Sutradhar, Sanjit; Paul, Bijaya; Adhikari, Suman; Laskar, Folguni; Butcher, Raymond J.; Acharya, Sandeep; Das, Arijit

    2017-07-01

    A new polymeric complex of Cd(II) with 1,1-dicyanoethylene- 2,2-dithiolate [ i-MNT2- = {S2C:C(CN)2}2- ] as a bridging ligand has been synthesized and characterized on the basis of spectroscopy and single-crystal X-ray diffraction analysis. Single crystal X-ray diffraction analysis reveals that the Cadmium (II) complex is six coordinated 1D polymeric in nature. Biological screening effects in vitro of the synthesized polymeric complex has been tested against five fungi Synchitrium endobioticum, Pyricularia oryzae, Helminthosporium oryzae, Candida albicans(ATCC10231), Trichophyton mentagrophytes by the disc diffusion method. In vitro antifungal screening indicates that the complex exhibits fungistatic and fungicidal antifungal activity whereas K2i-MNT.H2O became silent on Synchitrium endobioticum, Pyricularia oryzae, Helminthosporium oryzae, Candida albicans (ATCC10231), Trichophyton mentagrophytes.

  8. Structural variability in Cu(I) and Ag(I) coordination polymers with a flexible dithione ligand: Synthesis, crystal structure, microbiological and theoretical studies

    Energy Technology Data Exchange (ETDEWEB)

    Beheshti, Azizolla, E-mail: a.beheshti@scu.ac.ir [Department of Chemistry, Faculty of Sciences, Shahid Chamran University of Ahvaz, Ahvaz (Iran, Islamic Republic of); Nozarian, Kimia; Babadi, Susan Soleymani; Noorizadeh, Siamak [Department of Chemistry, Faculty of Sciences, Shahid Chamran University of Ahvaz, Ahvaz (Iran, Islamic Republic of); Motamedi, Hossein [Department of Biology, Faculty of Sciences, Shahid Chamran University of Ahvaz, Ahvaz (Iran, Islamic Republic of); Mayer, Peter [LMU München Department Chemie, Butenandtstr 5-13, D-81377 München (Germany); Bruno, Giuseppe [Dipartimento di Chimica Inorganica, Università di Messina, Vill. S. Agata, Salita Sperone 31, 98166 Messina (Italy); Rudbari, Hadi Amiri [Faculty of Chemistry, University of Isfahan, Isfahan 81746-73441 (Iran, Islamic Republic of)

    2017-05-15

    Two new compounds namely [Cu(SCN)(µ-L)]{sub n} (1) and ([Ag (µ{sub 2}-L)](ClO{sub 4})){sub n} (2) have been synthesized at room temperature by one-pot reactions between the 1,1-(1,4-butanediyl)bis(1,3-dihydro-3-methyl-1H-imidazole- 2-thione) (L) and appropriate copper(I) and silver(I) salts. These polymers have been characterized by single crystal X-ray diffraction, XRPD, TGA, elemental analysis, infrared spectroscopy, antibacterial activity and scanning probe microscopy studies. In the crystal structure of 1, copper atoms have a distorted trigonal planar geometry with a CuS{sub 2}N coordination environment. Each of the ligands in the structure of 1 acting as a bidentate S-bridging ligand to form a 1D chain structure. Additionally, the adjacent 1D chains are interconnected by the intermolecular C-H…S interactions to create a 2D network structure. In contrast to 1, in the cationic 3D structure of 2 each of the silver atoms exhibits an AgS{sub 4} tetrahedral geometry with 4-membered Ag{sub 2}S{sub 2} rings. In the structure of 2, the flexible ligand adopts two different conformations; gauche-anti-gauche and anti-anti-anti. The antibacterial studies of these polymers showed that polymer 2 is more potent antibacterial agent than 1. Scanning probe microscopy (SPM) study of the treated bacteria was carried out to investigate the structural changes cause by the interactions between the polymers and target bacteria. Theoretical study of polymer 1 investigated by the DFT calculations indicates that observed transitions at 266 nm and 302 nm in the UV–vis spectrum could be attributed to the π→π* and MLCT transitions, respectively. - Graphical abstract: Two new Cu(I) and Ag(I) coordination polymers have been have been synthesized by one-pot reactions. Copper complex has a 2D non-covalent structure, but silver compound is a 3D coordination compound. These compounds have effective antibacterial activity. - Highlights: • Cu(I) and Ag(I) based coordination polymers

  9. New five coordinated supramolecular structured cadmium complex as precursor for CdO nanoparticles: Synthesis, crystal structure, theoretical and 3D Hirshfeld surface analyses

    Science.gov (United States)

    Ghanbari Niyaky, S.; Montazerozohori, M.; Masoudiasl, A.; White, J. M.

    2017-03-01

    In this paper, a combined experimental and theoretical study on a new CdLBr2 complex (L = N1-(2-bromobenzylidene)-N2-(2-((E)-(2-bromobenzylidene) amino)ethyl) ethane-1,2-diamine) synthesized via template method, is described. The crystal structure analysis of the complex indicates that, the Cd(II) ion is centered in a distorted square pyramidal space constructed by three iminic nitrogens of the ligand as well as two bromide anions. More analysis of crystal packing proposed a supramolecular structure stabilized by some non-covalent interactions such as Br⋯Br and Xsbnd H⋯Br (X = N and C) in solid state. Furthermore, 3D Hirshfeld surface analyses and DFT studies were applied for theoretical investigation of the complexes. Theoretical achievements were found in a good agreement with respect to the experimental data. To evaluate the nature of bonding and the strength of the intra and inter-molecular interactions a natural bond orbital (NBO) analysis on the complex structure was performed. Time dependent density functional theory (TD-DFT) was also applied to predict the electronic spectral data of the complex as compared with the experimental ones. CdLBr2 complex as nano-structure compound was also prepared under ultrasonic conditions and characterized by scanning electron microscopy (SEM) and X-ray powder diffraction (XRPD). Finally, it was found that the cadmium complex can be used as a suitable precursor for preparation of CdO nanoparticles via calcination process at 600 °C under air atmosphere.

  10. (+)-Meyeniins A-C, Novel Hexahydroimidazo[1,5-c]thiazole Derivatives from the Tubers of Lepidium meyenii: Complete Structural Elucidation by Biomimetic Synthesis and Racemic Crystallization.

    Science.gov (United States)

    Zhou, Min; Ma, Hang-Ying; Liu, Zhi-Hua; Yang, Guang-Yu; Du, Gang; Ye, Yan-Qing; Li, Gan-Peng; Hu, Qiu-Fen

    2017-03-08

    (+)-Meyeniins A-C (1-3), a novel class of sulfur-containing hexahydroimidazo[1,5-c]thiazole derivatives, were isolated from the tubers of Lepidium meyenii (maca) cultivated in Lijiang, Yunnan province, China. Guided by their biosynthetic hypothesis, a stereocontrolled biomimetic synthesis of meyeniins A-C and their individual enantiomers was efficiently accomplished by a combination of a condensation reaction and Edman degradation. The formation of high-quality crystals for X-ray crystallography occurred much more readily from a racemic mixture of (±)-meyeniin A than with the single enantiomer alone in this case. These extensive strategies, combined with circular dichroism (CD) spectra, allowed the complete structural assignments of (+)-meyeniins A-C. Among them, (+)-meyeniin A showed moderate selective cytotoxicities against the HL-60, A549 and MCF-7 human cell lines with IC 50 values of 14.41, 32.22, and 33.14 μM, respectively. To some extent, these findings support traditional applications of maca as healthy nutritional supplements or functional foods for cancer prevention.

  11. Crystal structure of pseudoguainolide

    Directory of Open Access Journals (Sweden)

    Noureddine Beghidja

    2015-03-01

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

  12. Synthesis, crystal structure and photo physical properties of isomeric fluorinated s-shaped polyaromatic dibenzo[c,l]chrysene derivatives

    Science.gov (United States)

    Moriguchi, Tetsuji; Tabuchi, Daichi; Yakeya, Daisuke; Tsuge, Akihiko; Jalli, Venkataprasad; Yoza, Kenji

    2018-01-01

    Two s-shaped fluorinated isomeric polyaromatic dibenzo[c,l]chrysene derivatives have been synthesized by a two step process using the Wittig, Heck and iodine promoted cyclization reactions. These cyclized compounds were characterized by 1H NMR and EI-MS. Further, absolute configurations of isomeric 4a and 4b were determined by X-ray diffraction analysis. Compound 4a crystallized under monoclinic system with space group P21/c and compound 4b crystallized under monoclinic system with space group Cc. They have good solubility in common organic solvents such as dichloromethane, chloroform and THF. Photophysical properties of 4a and 4b were evaluated by using UV-Visible and Fluorescence spectrophotometer. Compounds 4a and 4b showed strong absorption maximum wavelength at 317 nm. The emission spectra of 4a and 4b displayed sharp peaks in the visible region from 417 to 441 nm. The shape of the UV-Visible and Fluorescence spectra of 4a and 4b looks almost identical. But compound 4a exhibited better fluorescence intensity than compound 4b. This difference may be due to the difference in the configuration of compounds 4a and 4b.

  13. Nd(III) and Dy(III) coordination compounds based on 1H-tetrazolate-5-acetic acid ligands: Synthesis, crystal structures and catalytic properties

    Energy Technology Data Exchange (ETDEWEB)

    Li Qiaoyun; Chen Dianyu; He Minghua [Jiangsu Laboratory of Advanced Functional Materials, Department of Chemistry and Materials Engineering, Changshu Institute of Technology, Changshu 215500, Jiangsu (China); Yang Gaowen, E-mail: ygwsx@126.com [Jiangsu Laboratory of Advanced Functional Materials, Department of Chemistry and Materials Engineering, Changshu Institute of Technology, Changshu 215500, Jiangsu (China); Shen Lei; Zhai Chun; Shen Wei; Gu Kun; Zhao Jingjing [Jiangsu Laboratory of Advanced Functional Materials, Department of Chemistry and Materials Engineering, Changshu Institute of Technology, Changshu 215500, Jiangsu (China)

    2012-06-15

    Reactions of 1H-tetrazolate-5-acetic acid(H{sub 2}tza) with Nd(NO{sub 3}){sub 3}{center_dot}6H{sub 2}O or Dy(NO{sub 3}){sub 3}{center_dot}6H{sub 2}O with the presence of KOH under solvothermal conditions, produced two new coordination compounds, [M{sub 2}(tza){sub 3}(H{sub 2}O){sub 6}]{center_dot}2H{sub 2}O [M=Nd(1), Dy(2)]. Both compounds were structurally characterized by elemental analysis, IR spectroscopy and single-crystal X-ray diffraction. Compounds 1 and 2 reveal 1D structures via bridging tza as linker. Furthermore, the compounds 1 and 2 showed a specific and good catalytic behavior for the polymerization of styrene, and the polymerization showed controlled characteristics. - Graphical Abstract: Two new coordination compounds, [M{sub 2}(tza){sub 3}(H{sub 2}O){sub 6}]{center_dot}2H{sub 2}O [M=Nd(1), Dy(2)] have been synthesis. 1 and 2 reveal 1D structures via bridging tza as linker, and showed a specific and good catalytic behavior for the polymerization of styrene. Highlights: Black-Right-Pointing-Pointer we have reported two novel compounds formed by H{sub 2}tza and Nd(III) or Dy(III). Black-Right-Pointing-Pointer Compounds 1 and 2 were found to have catalysis property for the photo-polymerization of styrene. Black-Right-Pointing-Pointer The high molecular weight polymers with narrow molecular weight distributions were obtained.

  14. SHORT COMMUNICATION SYNTHESIS AND CRYSTAL ...

    African Journals Online (AJOL)

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    pyrazine dicarboxylate complexes can construct versatile structural motifs, which generate various supramolecular architectures with interesting properties. After our previous works on synthesizing coordination compounds via proton transfer mechanism [10-15] including copper, manganese, cobalt and zinc atom herein, we ...

  15. Synthesis and crystal structure of a new pyridinium bromide salt: 4-methyl-1-(3-phenoxypropylpyridinium bromide

    Directory of Open Access Journals (Sweden)

    Musa A. Said

    2017-12-01

    Full Text Available In the cation of the title molecular salt, C15H18NO+·Br−, the pyridinium and phenyl rings are inclined to one another by 11.80 (8°. In the crystal, the Br− anion is linked to the cation by a C—H...Br hydrogen bond. The cations stack along the b-axis direction and are linked by further C—H...Br interactions, and offset π–π interactions [intercentroid distances = 3.5733 (19 and 3.8457 (19 Å], forming slabs parallel to the ab plane. The effects of the C—H...X− interaction on the NMR signals of the ortho- and meta-pyridinium protons in a series of related ionic liquids, viz. 4-methyl-1-(4-phenoxybutylpyridin-1-ium salts, are reported and discussed.

  16. Synthesis, crystal structures, luminescence properties of two metal coordination polymers derived from 5-substituted isophthalate and flexible bis (triazole) ligands.

    Science.gov (United States)

    Ming, Chun-lun; Wang, Li-na; Van Hecke, Kristof; Cui, Guang-hua

    2014-08-14

    Two new metal complexes, [Ni(btx)(nip)(H2O)]n (1), {[Cd(btx)(mip)(H2O)]·H2O}n (2) (btx=1,4-bis(1,2,4-triazol-1-ylmethyl)benzene, H2nip=5-nitroisophthalic acid, H2mip=5-methyisophthalic acid) were synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction methods, IR spectroscopy, TGA and elemental analysis. Complex 1 features a 3D metal-organic framework with three-fold interpenetrating CdSO4-type topology. Complex 2 exhibits a 2D network with square grid units, which is further extended into a rare 3,5T1 three-dimensional supramolecular network via three modes of classical OH⋯O hydrogen bonds. In addition, luminescence properties of 1 and 2 have also been investigated in the solid state. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. Synthesis, Crystal Structure, and Magnetic Properties of a New Mixed Metal (Co(II, Ni(II Cubane

    Directory of Open Access Journals (Sweden)

    Ramadan Mohamed Elmehdawi

    2017-02-01

    Full Text Available The mixed Co(II/Ni(II complex, [Co2.67Ni1.33L4(CH3COO2][BPh4]2·0.75H2O where HL = 4-(salicylaldimineantipyrine, was isolated as an orange solid from the reaction of 4-(salicylaldimineantipyrine, with mixed cobalt(II acetate and nickel(II acetate in ethanol. The complex was characterized by Frustrated Total Internal Reflection (FTIR, UltraViolet Visible spectroscopy (UV-Vis, X-ray single crystal diffraction, and by elemental analysis. The complex is composed of two symmetry independent cationic units, A and B. The two units are essentially isostructural; nevertheless, small differences exist between them. The units contain four metal atoms, arranged at the corners of a distorted cubane-like core alternately with phenoxy oxygen of the Schiff base. The overall eight corners occupied by metal ions in the asymmetric unit are shared between cobalt and nickel in a 5.33:2.67 ratio. Each metal divalent cation binds three coordinated sites from the corresponding tridentate Schiff base ligand, the fourth one is bound by the acetate oxygen, the fifth and the sixth donor sites come from the phenolate oxygens of other Schiff base ligands. Intermolecular hydrogen bonds join the complexes to the water molecules present in the crystal packing. The magnetic characterization was carried out for this new complex and for its isostructural counterpart containing only cobalt ions. The magnetic measurements for the cobalt(II/nickel(II mixed compound indicate either antiferromagnetic interactions among the two cubanes or an anisotropic contribution, whereas a ferromagnetic interaction is observed within the cubane, for both the complexes, as expected by geometrical considerations. A comparison between the magnetic properties of the pure cobalt(II derivative and similar systems discussed in literature, is presented.

  18. Synthesis, growth, structural, optical and thermal properties of a new organic nonlinear optical crystal: 2-amino 5-chloropyridinium-L-tartarate

    Science.gov (United States)

    Jayanalina, T.; Rajarajan, G.; Boopathi, K.; Sreevani, K.

    2015-09-01

    A new organic nonlinear optical crystal 2-amino-5-chloropyridinium-L-tartarate [2A5CPLTA] has been synthesized and the crystals were grown by slow evaporation solution technique at room temperature using methanol as solvent. The crystal structure of the title compound has been determined by the single crystal X-ray diffraction study and it belongs to the monoclinic system with noncentrosymmetric space group P21. The presence of functional groups was ascertained by Fourier transform infrared analysis. The transmittance and lower cut off of the grown crystal was ascertained by the UV-vis-NIR spectroscopy. Thermal studies reveled that 2A5CPLTA crystal is thermally stable up to 144 °C. The dielectric measurements of the grown crystal were carried out with different frequencies and temperatures. Vickers micro hardness measurement was carried out to study the mechanical behavior of the grown crystal. The second harmonic generation of the title crystal was confirmed by the Kurtz-Perry powder test employing the Nd: YAG laser as the source.

  19. New 7-arylpiperazinylalkyl-8-morpholin-4-yl-purine-2,6-dione derivatives with anxiolytic activity - Synthesis, crystal structure and structure-activity study

    Science.gov (United States)

    Chłoń-Rzepa, Grażyna; Żmudzki, Paweł; Pawłowski, Maciej; Wesołowska, Anna; Satała, Grzegorz; Bojarski, Andrzej J.; Jabłoński, Mateusz; Kalinowska-Tłuścik, Justyna

    2014-06-01

    On the basis of our earlier studies with serotonin (5-HT) receptor ligands in the group of long-chain arylpiperazines (LCAPs), a new series of 7-arylpiperazinylalkyl-8-morpholin-4-yl-purine-2,6-dione derivatives (5-12) has been designed, synthesised and studied in vitro for their affinity for 5-HT1A, 5-HT2A, 5-HT6 and 5-HT7 receptors. The introduction of o-OCH3 and m-Cl into the phenylpiperazinyl moiety as well as the elongation of the linker between purine-2,6-dione core and arylpiperazine fragment modified the affinity for the tested 5-HT receptors. The structures of compounds 9-11 (hydrochloride salts) were confirmed by an X-ray diffraction method. All molecules adopted a different conformation in the crystal. The strongest observed type of interaction is a charge assisted hydrogen bond N+-H⋯Cl-. Additionally, the π-π interactions between 1,3-dimethyl-3,7-dihydropurine-2,6-dione cores of the neighbouring molecules were also observed. As it is observed in the presented crystal structures, the morpholine ring (a potential donor and acceptor of the hydrogen bonds) seems to be an attractive substituent, that may support binding to the non-specific sites of 5-HT receptors. Another interesting feature is the mutual orientation of rings in the arylpiperazine fragment, with plausible influence on ligand-receptor recognition. For compound 10, with strong 5-HT1A binding affinity, the mutual orientation of rings is determined by the intramolecular weak C-H⋯O hydrogen bond. This observation may contribute to a better understanding of the more selective binding of o-OCH3 arylpiperazine derivatives to the 5-HT1A receptor.

  20. Synthesis, crystal growth and characterization of nonlinear optical organic crystal: p-Toluidinium p-toluenesulphonate

    International Nuclear Information System (INIS)

    Vijayakumar, P.; Anandha Babu, G.; Ramasamy, P.

    2012-01-01

    Graphical abstract: p-Toluidinium p-toluenesulphonate (p-TTS) an organic nonlinear optical crystal has been grown from the aqueous solution by slow evaporation solution growth technique. Single crystal X-ray diffraction analysis reveals that p-TTS crystallizes in monoclinic crystal system. p-TTS single crystal belongs to negative birefringence crystal. Second harmonic conversion efficiency of p-TTS has been found to be 1.3 times higher than that of KDP. Multiple shot surface laser damage threshold is determined to be 0.30 GW/cm 2 at 1064 nm laser radiation. Highlights: ► It deals with the synthesis, growth and characterization of p-TTS an organic NLO crystal. ► Wide optical transparency window between 280 nm and 1100 nm. ► Negative birefringence crystal and dispersion of birefringence is negligibly small. ► Thermal study reveals that the grown crystal is stable up to 210 °C. ► Multiple shot surface laser damage threshold is 0.30 GW/cm 2 at 1064 nm laser radiation. -- Abstract: p-Toluidinium p-toluenesulphonate (p-TTS) an organic nonlinear optical crystal has been grown from the aqueous solution by slow evaporation solution growth technique. Single crystal X-ray diffraction analysis reveals that p-TTS crystallizes in monoclinic crystal system. The structural perfection of the grown p-TTS single crystal has been analyzed by high-resolution X-ray diffraction rocking curve measurements. Fourier transform infrared spectral studies have been performed to identify the functional groups. The optical transmittance window and the lower cutoff wavelength of the grown crystals have been identified by UV–vis–IR studies. Birefringence of p-TTS crystal has been studied using channel spectrum measurement. The laser damage threshold value was measured using Nd:YAG laser. The second harmonic conversion efficiency of p-TTS has been determined using Kurtz powder technique. Thermo gravimetric and differential thermal analyses were used to study its thermal properties

  1. Microporous crystals and synthesis schemes

    Science.gov (United States)

    Tumas, William; Ott, Kevin C.; McCleskey, T. Mark; Yates, Matthew Z.; Birnbaum, Eva R.

    2005-09-27

    Novel zeolites are produced by combining a polar solute, a silicon or phosphorous source, and a structure directing agent. Surfactants and a hydrophobic solvent are added to the previously mixed three species and shaken to disperse the surfactants. The reverse microemulsion is stirred overnight, at about room temperature and then iced for five to ten minutes. A metal source is added vigorously shaken for about two minutes. The mixture is then aged for about two hours at about room temperature. A mineralizer is added and the resultant mixture aged for about two hours at about room temperature. The mixture is heated to about 180.degree. C., for a suitable time period. The final novel product is then isolated.

  2. Microporous crystals and synthesis schemes

    Science.gov (United States)

    Tumas, William; Ott, Kevin C.; McCleskey, T. Mark; Yates, Matthew Z.; Birnbaum, Eva R.

    2008-04-22

    Novel zeolites are produced by combining a polar solute, a silicon or phosphorous source, and a structure directing agent. Surfactants and a hydrophobic solvent are added to the previously mixed three species and shaken to disperse the surfactants. The reverse microemulsion is stirred overnight, at about room temperature and then iced for five to ten minutes. A metal source is added vigorously shaken for about two minutes. The mixture is then aged for about two hours at about room temperature. A mineralizer is added and the resultant mixture aged for about two hours at about room temperature. The mixture is heated to about 180.degree. C., for a suitable time period. The final novel product is then isolated.

  3. Hydrothermal synthesis, crystal structure and properties of a novel chain coordination polymer constructed by tetrafunctional phosphonate anions and cobalt ions

    International Nuclear Information System (INIS)

    Guan, Lei; Wang, Ying

    2015-01-01

    A novel cobalt phosphonate, [Co(HL)(H 2 O) 3 ] n (1) (L=N(CH 2 PO 3 H) 3 3− ) has been synthesized by hydrothermal reaction at 150 °C and structurally characterized by X-ray diffraction, infrared spectroscopy, elemental and thermogravimetric analysis. Complex 1 features a 1D chain structure with double-channel built from CoO 6 octahedra bridged together by the phosphonate groups. Each cobalt ion is octahedrally coordinated by three phosphonate oxygen atoms and three water molecules. The coordinated water molecules can form the hydrogen bonds with the phosphonate oxygen atoms to link the 1D chains, building a 2D layered structure, further resulting in a 3D network. The luminescence spectrum indicates an emission maximum at 435 nm. The magnetic susceptibility curve exhibits a dominant antiferromagnetic behavior with a weakly ferromagnetic component at low temperatures. - Graphical abstract: The connectivity between cobalt ions and the ligands results in a chain structure with a 1D double-channel structure, which is constructed by A-type subrings and B-type subrings. - Highlights: • The tetrafunctional phosphonate ligand was used as the ligand. • A novel chain structure can be formed by A-type rings and B-type rings. • Two types of rings can form a 1D double-channel structure, along the c-axis

  4. Synthesis, Molecular and Crystal Structure Analysis of 1-(4-Methylbenzenesulfonylindole-3-carbaldehyde and DFT Investigation of Its Rotational Conformers

    Directory of Open Access Journals (Sweden)

    Julio Zukerman-Schpector

    2014-02-01

    Full Text Available Two independent molecules that differ in terms of rotation about the central S-N bond comprise the asymmetric unit of the title compound 1. The molecules have a V-shape with the dihedral angles between the fused ring system and benzene ring being 79.08(6° and 72.83(5°, respectively. The packing is mostly driven by p···p interactions occurring between the tolyl ring of one molecule and the C6 ring of the indole fused ring system of the other. DFT and IRC calculations for these and related 1-(arylsulfonylindole molecules showed that the rotational barrier about the S-N bond between conformers is within the 2.5–5.5 kcal/mol range. Crystal data for C16H13NO3S (1: Mr = 299.33, space group Pna21, a = 19.6152(4 Å, b = 11.2736(4 Å, c = 12.6334(3 Å, V = 2793.67(13 Å3, Z = 8, Z' = 2, R = 0.034.

  5. Synthesis, crystal structure, characterization and antifungal activity of 3,4-diaryl-1H-Pyrazoles derivatives

    Science.gov (United States)

    Zhang, Jin; Tan, Da-Jin; Wang, Tao; Jing, Si-Si; Kang, Yang; Zhang, Zun-Ting

    2017-12-01

    A series of 3,4-diaryl-1H-pyrazoles derivatives were designed and synthesized by the reaction of 3-heteroarylchromones and 3-phenylchromones with hydrazine hydrate in good yields. All of those compounds were characterized by 1H NMR, 13C NMR, IR, and HRMS. Moreover, 3-(2,4-dihydroxyphenyl)-4-(4-hydroxyphenyl)-1H-pyrazole and 3-(2,4-dihydroxy phenyl)-4-(4-methoxyphenyl)-1H-pyrazole were further conformed by the single crystal X-ray diffraction. In addition, the antifungal activity against five phytopathogenic fungi (Cytospora sp., Colletotrichum gloeosporioides, Botrytis cinerea, Alternaria solani and Fusarium solani) of 3,4-diaryl-1H-pyrazoles were evaluated. 3-(2-Hydroxy-4-isopropoxyphenyl)-4-phenyl-1H-pyrazole was more better and broader inhibitory effect on Cytospora sp., C. gloeosporioides, A. solani and Fusarium solani with IC50 values of 26.96, 28.84, 16.77 and 22.10 μg/mL, respectively. 4-(4-Fluorophenyl)-3-(2-hydroxy-4-methoxyphenyl)-1H-pyrazole exhibited fairly effective antifungal activity against Cytospora sp., C. gloeosporioides and A. solani with IC50 values of 11.91, 14.92 and 16.98 μg/mL, respectively.

  6. 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.

  7. Synthesis, crystal structure and cytotoxic activity of ruthenium(II) piano-stool complex with N,N-chelating ligand

    Science.gov (United States)

    Rogala, Patrycja; Jabłońska-Wawrzycka, Agnieszka; Kazimierczuk, Katarzyna; Borek, Agnieszka; Błażejczyk, Agnieszka; Wietrzyk, Joanna; Barszcz, Barbara

    2016-12-01

    A mononuclear compound of the general formula [(η6-p-cymene)RuIICl(2,2‧-PyBIm)]PF6 has been synthesized from a bidentate N,N-donor ligand, viz. 2,-(2‧-pyridyl)benzimidazole (2,2‧-PyBIm) and the corresponding chloro-complex [(η6-p-cymene)Ru(μ-Cl)Cl]2 (precursor). The isolated coordination compound was characterized by IR, UV-vis and 1H, 13C NMR spectroscopies. The single crystal X-ray analysis of the complex reveals that the asymmetric part of the unit cell consists of two symmetrically independent, [(η6-p-cymene)RuCl(2,2‧-PyBIm)]+ cationic complexes. Each cation exhibits a pseudo-octahedral three-legged piano-stool geometry, in which three "legs" are occupied by one chloride ion and two nitrogen donor atoms of the chelating ligand 2,2‧-PyBIm. The Hirshfeld surface analysis of obtained complex was determined, too. The ionic nature of the compound is identified by a strong band at around 830 cm-1 due to the νP-F stretching mode of the PF6- counter ion. The electronic spectrum of this monomeric complex displays high intensity bands in the ultraviolet region assignable to π→π*/n→π* transitions, as well as a band attributable to the metal-to-ligand charge transfer (MLCT) dπ(Ru)→π*(L) transition. Additionally, the complex has been screened for its cytotoxicity against three human cancer lines: non-small cell lung carcinoma (A549), colon adenocarcinoma (HT29) and breast adenocarcinoma (MCF-7) as well as normal mice fibroblast cells (BALB/3T3). The complex demonstrated a moderate antiproliferative activity against the cell lines tested.

  8. Synthesis and single-crystal structure of the pseudo-ternary compounds LiA[N(CN){sub 2}]{sub 2} (A = K or Rb)

    Energy Technology Data Exchange (ETDEWEB)

    Reckeweg, Olaf; DiSalvo, Francis J. [Cornell Univ., Ithaca, NY (United States). Baker Lab.

    2016-04-01

    Crystals of LiA[N(CN){sub 2}]{sub 2} were obtained from the reaction of LiCl and ACl (A = K or Rb) with Ag[N(CN){sub 2}] in water and subsequent evaporation of the filtered solution at 80 C under normal atmospheric conditions. Crystals of the title compound form thin rectangular plates that are transparent, colorless, and very fragile. Single-crystal structure analyses have shown that both compounds are isotypic and adopt the tetragonal space group I4/mcm (no. 140, Z = 4) with the cell parameters a = 701.53(12) and c = 1413.7(5) pm for LiK[N(CN){sub 2}]{sub 2} and a = 730.34(10) and c = 1414.4(4) pm for LiRb[N(CN){sub 2}]{sub 2}. The crystal structure is described and compared to that of the pseudo-binary alkali metal dicyanamides.

  9. Synthesis, crystal structure and spectral characteristics of highly fluorescent chalcone-based coumarin in solution and in polymer matrix

    Czech Academy of Sciences Publication Activity Database

    Ghouili, A.; Dušek, Michal; Petříček, Václav; Ben Ayed, T.; Ben Hassen, R.

    2014-01-01

    Roč. 75, č. 2 (2014), s. 188-193 ISSN 0022-3697 Grant - others:AV ČR(CZ) Praemium Academiae Institutional support: RVO:68378271 Keywords : coumarin chalcone * fluorescence * structure determination Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.853, year: 2014

  10. Two coordination polymers based on semicarbazone Schiff base and azide: synthesis, crystal structure, electrochemistry, magnetic properties and biological activity

    Czech Academy of Sciences Publication Activity Database

    Shaabani, B.; Khandar, A.A.; Dušek, Michal; Pojarová, Michaela; Mahmoudi, F.; Feher, A.; Kajňaková, M.

    2013-01-01

    Roč. 66, č. 5 (2013), s. 748-762 ISSN 0095-8972 Grant - others:AV ČR(CZ) AP0701 Program:Akademická prémie - Praemium Academiae Institutional support: RVO:68378271 Keywords : Schiff bases * semicarbazone * coordination polymer * structure analyses Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.224, year: 2013

  11. The first pseudo-ternary thiocyanate containing two alkali metals. Synthesis and single-crystal structure of LiK2[SCN]3

    International Nuclear Information System (INIS)

    Reckeweg, Olaf; DiSalvo, Francis J.

    2016-01-01

    A procedure was empirically developed to prepare the compound LiK 2 [SCN] 3 , which forms colorless, transparent, very fragile, and extremely hygroscopic thin rectangular plates. Its unique crystal structure was determined by single-crystal X-ray diffraction. LiK 2 [SCN] 3 adopts the orthorhombic space group Pna2 1 (no. 33, Z = 4) with the cell parameters a = 1209.32(9), b = 950.85(9), and c = 849.95(6) pm.

  12. Synthesis, Crystal Structure and Luminescent Property of A Novel Cd(II) Coordination Polymer with Bis-imidazole Ligand

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Yong Hong [Huaibei Normal Univ., Huaibei (China)

    2013-04-15

    The key to the successful design of metal-organic coordination polymers is the judicious selection of organic ligand. Recently, polydentate aromatic nitrogen heterocyclic ligands with five-membered rings have been well-studied in the construction of supramolecular structure for their N-coordinated sites apt to coordinating to transition metals. Similar to six-membered N-heterocyclic ligands, the azole-based five-membered N-heterocyclic ligands, such as imidazoles, triazoles and tetrazoles have been extensively employed in the construction of various coordination polymers with diverse topologies and interesting properties. The bis(azole) ligands in which N-donor azole rings (imidazole, triazole, or tetrazole) are separated by alkyl, (CH{sub 2}){sub n}, spacers are good choices for flexible bridging ligands. The conformational flexibility of the spacers makes the ligands adaptable to various coordination networks with one-, two-, and three dimensional structures.

  13. Synthesis, crystal structure, and TEM analysis of Sr19Li44 and Sr3Li2: a reinvestigation of the Sr-Li phase diagram.

    Science.gov (United States)

    Smetana, Volodymyr; Kienle, Lorenz; Duppel, Viola; Simon, Arndt

    2015-02-02

    Two intermetallic phases in the Sr-Li system have been synthesized and structurally characterized. According to single-crystal X-ray diffraction data, Sr(19)Li(44) and Sr(3)Li(2) crystallize with tetragonal unit cells (Sr(19)Li(44), I-42d, a = 15.9122(7) Å, c = 31.831(2) Å, Z = 4, V = 8059(2) Å(3); Sr(3)Li(2), P42/mnm, a = 9.803(1) Å, c = 8.784(2) Å, Z = 4, V = 844.2(2) Å(3)). The first compound is isostructural with the recently discovered Ba(19)Li(44). Sr in Sr(19)Li(44) can be fully replaced by Ba with no changes to the crystal structure, whereas the substitution of Sr by Ca is only possible within a limited concentration range. Sr(3)Li(2) can be assigned to the Al(2)Zr(3) structure type. The crystal structure determination of Sr(19)Li(44) was complicated by multiple twinning. As an experimental highlight, an electron microscopy investigation of the highly moisture- and electron-beam-sensitive crystals was performed, enabling high-resolution imaging of the defect structure.

  14. Synthesis, crystal structure and DFT studies of a novel dinuclear copper(I) complex with triphenylphosphine and 2-mercaptonicotinic acid

    Science.gov (United States)

    Ahmad, Tayyaba; Mahmood, Rashid; Georgieva, Ivelina; Zahariev, Tsvetan; Tahir, Muhammad Nawaz; Shaheen, Muhammad Ashraf; Gilani, Mazhar Amjad; Ahmad, Saeed

    2018-02-01

    A novel dinuclear copper(I) complex, {[Cu2(Mnt)2(PPh3)2Cl2].2H2O.CH3CN}2 (1) (Mnt = Mercaptonicotinic acid, PPh3 = triphenylphosphine) was prepared and its structure was determined by X-ray crystallography. The complex 1 consists of two dinuclear molecules and in each molecule, the two copper atoms are bridged by S atoms of N-protonated mercaptonicotinic acid forming a four-membered ring. The planar Cu2S2 core is characterized by significant cuprophilic interactions (Cusbnd Cu distance = 2.7671(8), 2.8471(8) Å). Each copper atom in 1 is coordinated by two sulfur atoms of Mnt, one phosphorus atom of PPh3 and a chloride ion adopting a tetrahedral geometry. The calculated Gibbs energies for reaction in CH3CN supported the experimental structure and predicted more favorable formation of dinuclear Cu(I) complex as compared to the mononuclear Cu(I) complex. The dinuclear complex is stabilized by 65.98 kJ mol-1 by coupling of two mononuclear Cu(I) complexes. The IR spectra of 1 and Mnt ligand were reliably interpreted and the Mnt vibrations, which are sensitive to the ligand coordination to Cu(I) ion in 1 were selected with the help of DFT/ωB97XD calculations.

  15. Triphenylphosphane Pt(II) complexes containing biologically active natural polyphenols: Synthesis, crystal structure, molecular modeling and cytotoxic studies.

    Science.gov (United States)

    Dell'Anna, Maria Michela; Censi, Valentina; Carrozzini, Benedetta; Caliandro, Rocco; Denora, Nunzio; Franco, Massimo; Veclani, Daniele; Melchior, Andrea; Tolazzi, Marilena; Mastrorilli, Piero

    2016-10-01

    Platinum complexes bearing phosphane ligands in cis configuration with deprotonated flavonoids (3-hydroxyflavone, quercetin) and deprotonated ethyl gallate were synthesized starting from cis-[PtCl 2 (PPh 3 ) 2 ]. In all cases, O,O' chelate structures were obtained. While quercetin and ethyl gallate complexes are quite stable in solution, the 3-hydroxyflavonate complex undergoes a slow aerobic photodegradation in solution with formation of salicylic and benzoic acids. The X-ray diffraction structures of quercetin and ethyl gallate complexes are reported. Cell cycle studies (in the dark) of the complexes in two human cell lines revealed that the cytotoxic activity of the complex bearing 3-hydroxyflavonate is higher than those exhibited by 3-hydroxyflavone or by cis-[PtCl 2 (PPh 3 ) 2 ] alone. Density functional theory studies on the hydrolysis pathway for the 3-hydroxyflavone and ethyl gallate complexes explained the different cytotoxic activity observed for the two compounds on the basis of the different intermediates formed during hydrolysis (relatively inert hydroxy Pt complexes for ethyl gallate and monoaqua complexes for 3-hydroxyflavone). Copyright © 2016 Elsevier Inc. All rights reserved.

  16. Synthesis, crystal structure and electrochemical properties of LiFePO4F cathode material for Li-ion batteries

    International Nuclear Information System (INIS)

    Chen, D.; Shao, G.-Q.; Li, B.; Zhao, G.-G.; Li, J.; Liu, J.-H.; Gao, Z.-S.; Zhang, H.-F.

    2014-01-01

    Highlights: • Tavorite-structured LiFePO 4 F with high purity is successfully synthesized by a two-step solid-state route. • Rietveld refinement shows that open pathways for 3D ion transport exist in LiFePO 4 F and its discharged state (Li 2 FePO 4 F). • The voltage plateaus on 2.71 / 2.86 V, in galvanostatic discharge-charge cycling, indicate a low electrode polarization of 0.15 V. • This work attained the largest initial discharge capacity at the highest rate (1 C) reported to date. • This work attained almost the same capacity retention at a tenfold higher rate (1 C) than that (0.1 C) within the maximum cycles of 100 reported to date. - Abstract: Tavorite-structured lithium-metal-fluorophosphates for Li + transition have been recognized as a good alternative to olivine-type cathodes for lithium-ion batteries. They show an exceptional ionic conductivity, excellent thermal stability and capacity retention. In this work, LiFePO 4 F with high purity is successfully synthesized by a two-step solid-state route. Rietveld refinement shows that open pathways for 3D ion transport exist in LiFePO 4 F and its discharged state (Li 2 FePO 4 F). Cyclic voltammetry data exhibit a clear indication of the Fe 3+/2+ redox couple that involves a two-phase transition. Galvanostatic discharge-charge cycling was examined at the rates 0.1 - 5 C up to 1000 cycles. The voltage plateaus on 2.71 / 2.86 V indicate a low electrode polarization of 0.15 V. This work attained the largest initial discharge capacity at the highest rate (1 C) reported to date, and almost the same capacity retention at a tenfold higher rate (1 C) than that (0.1 C) within the maximum cycles of 100 reported to date

  17. Synthesis and Crystal Structure of 1-(4-Nitrobenzyl-3-allyl-1H-benzo[d]imidazol-2(3H-one

    Directory of Open Access Journals (Sweden)

    Dounia Belaziz

    2013-01-01

    Full Text Available A functionalized benzimidazole, 1-(4-nitrobenzyl-3-allyl-1H-benzo[d]imidazol-2(3H-one, has been synthesized, and the crystal structure was determined and analyzed. This compound crystallizes in the monoclinic, space group P21/n (number 14 c with cell parameters, a=7.12148(8 Å, b=16.12035(17 Å, c=13.04169(17 Å, β=93.3043(11, V=1494.71(3 Å3, and Dcalc = 1.375 g/mm3. The solid state geometry is stabilized by intermolecular π–π interactions along with the van der Waals interactions which contribute to the stability of the crystal packing. Computational calculations have been used to properly understand the main intermolecular interactions present in the crystal.

  18. Synthesis, X-ray crystal structure and optical properties research of novel diphenyl sulfone-based bis-pyrazoline derivatives

    Energy Technology Data Exchange (ETDEWEB)

    Gong Zhongliang; Zheng Liangwen [Institute of Organic Chemistry, School of Chemistry and Chemical Engineering, Shandong University, Jinan 250100 (China); Zhao Baoxiang, E-mail: bxzhao@sdu.edu.cn [Institute of Organic Chemistry, School of Chemistry and Chemical Engineering, Shandong University, Jinan 250100 (China)

    2012-02-15

    A series of novel bis-pyrazoline derivatives were synthesized by the reaction of chalcone and (sulfonylbis(3,1-phenylene))bis(hydrazine) in 20-34% yields. The structures of the compounds were determined by IR, {sup 1}H NMR, HRMS spectra, and a representative compound 3b was confirmed based on the X-ray crystallographic analysis. Absorption and fluorescence spectra of these compounds in dichloromethane solution were investigated. The results showed that the emission maxima varied from 415 to 444 nm mainly depending on C3 substituents of pyrazoline moiety. The compounds had higher quantum yields, when C3 substituent was an electron-withdrawing p-chlorophenyl group. Moreover, absorption spectra and emission spectra exhibited a blue-shift and a red-shift with increasing the polarity of solvents, respectively. Fluorescent molecules happened to collide with each other and resulted in quench of the fluorescence when the concentration increased over to 10{sup -5} M. - Highlights: Black-Right-Pointing-Pointer A series of novel diphenyl sulfone-based bis-pyrazoline derivatives were designed and synthesized. Black-Right-Pointing-Pointer Their UV-vis absorption and fluorescence emission spectra were investigated. Black-Right-Pointing-Pointer The relationship of substituents and the optical properties were discussed. Black-Right-Pointing-Pointer With increasing the solvent polarity, fluorescence emission displayed a red-shift and fluorescence quantum yields decreased. Black-Right-Pointing-Pointer Fluorescence was quenched when the concentration increased over to 10{sup -5} M.

  19. Synthesis, X-ray crystal structure and optical properties research of novel diphenyl sulfone-based bis-pyrazoline derivatives

    International Nuclear Information System (INIS)

    Gong Zhongliang; Zheng Liangwen; Zhao Baoxiang

    2012-01-01

    A series of novel bis-pyrazoline derivatives were synthesized by the reaction of chalcone and (sulfonylbis(3,1-phenylene))bis(hydrazine) in 20–34% yields. The structures of the compounds were determined by IR, 1 H NMR, HRMS spectra, and a representative compound 3b was confirmed based on the X-ray crystallographic analysis. Absorption and fluorescence spectra of these compounds in dichloromethane solution were investigated. The results showed that the emission maxima varied from 415 to 444 nm mainly depending on C3 substituents of pyrazoline moiety. The compounds had higher quantum yields, when C3 substituent was an electron-withdrawing p-chlorophenyl group. Moreover, absorption spectra and emission spectra exhibited a blue-shift and a red-shift with increasing the polarity of solvents, respectively. Fluorescent molecules happened to collide with each other and resulted in quench of the fluorescence when the concentration increased over to 10 −5 M. - Highlights: ► A series of novel diphenyl sulfone-based bis-pyrazoline derivatives were designed and synthesized. ► Their UV–vis absorption and fluorescence emission spectra were investigated. ► The relationship of substituents and the optical properties were discussed. ► With increasing the solvent polarity, fluorescence emission displayed a red-shift and fluorescence quantum yields decreased. ► Fluorescence was quenched when the concentration increased over to 10 −5 M.

  20. Synthesis, crystal structure and anticancer activity of tetrakis(N-isopropylimidazolidine-2-selenone)platinum(II) chloride

    Science.gov (United States)

    Ahmad, Saeed; Altoum, Ali Osman S.; Vančo, Ján; Křikavová, Radka; Trávníček, Zdeněk; Dvořák, Zdeněk; Altaf, Muhammad; Sohail, Manzar; Isab, Anvarhusein A.

    2018-01-01

    A Platinum(II) complex of N-isopropylimidazolidine-2-selenone (i-PrImSe), [Pt(i-PrImSe)4]Cl2 (1) was prepared and characterized by elemental analysis, IR and NMR (1H, 13C, 77Se &195Pt) spectroscopy, and X-ray crystallography. The structure of 1 consists of [Pt(i-PrImSe)4]2+ complex ion and chloride counter ions. The platinum(II) atom adopts a distorted square planar geometry. The in vitro antitumor activity of 1 as well as cisplatin, was evaluated by MTT assay against human; ovarian carcinoma A2780 and its cisplatin-resistant subline A2780R, prostate cancer 22Rv1 and breast cancer MCF-7 cell lines. The title complex displayed the activity against the A2780 cells (IC50 = 30.8 μM) at the level comparable to cisplatin (IC50 = 26.8 μM). The interaction studies with sulfur-containing biomolecules revealed its ability to form a variety of intermediates and oxidized species with L-cysteine and reduced glutathione.

  1. Synthesis, crystal structures, and luminescent properties of two series' of new lanthanide (III) amino-carboxylate-phosphonates.

    Science.gov (United States)

    Zhou, Tian-Hua; Yi, Fei-Yan; Li, Pei-Xin; Mao, Jiang-Gao

    2010-02-01

    Hydrothermal reactions of lanthanide(III) chlorides with 4-HOOC-C(6)H(4)-CH(2)NHCH(2)PO(3)H(2) (H(3)L) at different ligand-to-metal (L/M) ratios afforded nine new lanthanide(III) carboxylate-phosphonates with two types of 3D network structures, namely, LnCl(HL)(H(2)O)(2) (Ln = Sm, 1; Eu, 2; Gd, 3; Tb, 4; Dy, 5; Er, 6) and [Ln(2)(HL)(H(2)L)(L)(H(2)O)(2)].4H(2)O (Ln = Nd, 7; Sm, 8; Eu, 9). Compounds 1-6 are isostructural and feature a 3D network in which the LnO(7)Cl polyhedra are interconnected by bridging CPO(3) tetrahedra into 2D inorganic layers parallel to the bc plane. These layers are further cross-linked by organic groups of the carboxylate-phosphonate ligands via the coordination of the carboxylate groups into a pillared-layered architecture. Compounds 7-9 are also isostructural and feature a 3D open-framework composed of 1D lanthanide(III) phosphonate inorganic slabs which are further bridged by organic groups of the carboxylate-phosphonate liagnds via the coordination of the carboxylate groups, forming large 1D tunnels along the b-axis which are filled by lattice water molecules. Luminescent measurements indicate that compounds 2, 4, and 5 show strong emission bands in red, green, and yellow light region, respectively. Magnetic properties of 2, 3, 5, and 7 have also been studied.

  2. New alkaline earth aluminum hydride with one-dimensional zigzag chains of [AlH6]: synthesis and crystal structure of BaAlH5.

    Science.gov (United States)

    Zhang, Qing-An; Nakamura, Yumiko; Oikawa, Ken-ich; Kamiyama, Takashi; Akiba, Etsuo

    2002-12-30

    The title hydride and its deuteride were successfully synthesized. The crystal structure of the deuteride was determined by time-of-flight neutron powder diffraction. BaAlD(5) crystallizes with a new orthorhombic structure in space group Pna2(1) (No. 33), cell parameters a = 9.194(1) A, b = 7.0403(9) A, and c = 5.1061(6) A, Z = 4. BaAlH(5) is the first example that contains one-dimensional zigzag chains of [AlH(6)] along the crystallographic c axis.

  3. 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.

  4. Synthesis, crystal structure and luminescent properties of lanthanide extended structure with asymmetrical dinuclear units based on 2-(methylthio)benzoic acid

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Cristiane K.; Souza, Viviane P. de; Luz, Leonis L. da [Departamento de Química Fundamental, UFPE, 50.740-560 Recife, PE (Brazil); Menezes Vicenti, Juliano R. de [Escola de Química e Alimento, FURG, 96203-900 Rio Grande, RS (Brazil); Burrow, Robert A. [Departamento de Química, UFSM, 97105-900 Santa Maria, RS (Brazil); Severino Alves; Longo, Ricardo L. [Departamento de Química Fundamental, UFPE, 50.740-560 Recife, PE (Brazil); Malvestiti, Ivani, E-mail: ivani@ufpe.br [Departamento de Química Fundamental, UFPE, 50.740-560 Recife, PE (Brazil)

    2016-02-15

    The extended structures [Ln{sub 2}(L){sub 6}(OH{sub 2}){sub 4}] with L=2-(methylthio)benzoato (2-CH{sub 3}S–C{sub 6}H{sub 4}COO{sup −}) and Ln=Tb (1), Eu (2) and Gd (3) were successfully synthesized and characterized. The single crystal structure of compound 1 was determined and showed an extended structure made up of asymmetrical dinuclear units with the formula catena-poly[{Tb(H_2O)_4}-(μ-L-1κO:2κO'){sub 2}-{Tb(L-κO,O')_2}-(μ-L-1κO:2κO'){sub 2}]. In the molecule of 1, there are two distinct metal sites. The Tb atom in site 1 is bound to four coordinated water molecules and four oxygen atoms from four different benzoate ligands, two of which bridge to site 2 Tb atoms on one side and two to site 2 Tb atoms on the other side. The site 2 Tb atom is bound to four oxygen atoms from two chelating benzoate ligands and four oxygen atoms from four different benzoate ligands, two of which bridge to site 1 Tb atoms on one side and two to site 1 Tb atoms on the other side. The bridging benzoate ligands extend the framework in one-dimension with alternating site 1/site 2 Tb atoms. The luminescent properties of these asymmetric dinuclear extended structures are quite peculiar and showed a single emitting lanthanide center. The quantum yields of 1 (ca. 50–55%) is practically independent of the excitation energy, whereas those of 2 are vanishing small (<1%) when excited at the ligand states and become sizable (ca. 10–20%) upon excitation at the intra-4f manifold. To reconcile these experimental observations in conjunction with the spectral data for compounds 1 and 3, a strong interaction between the lanthanide emitting states at sites 1 and 2 was proposed. For compound 1, the numerical solutions of the rate equations provided evidences that when the transition rates between the emitting states at both sites are larger than the highest decaying rate of these states, the system becomes an effective single emitter. This establishes, for the first time

  5. Synthesis, crystal structure and growth of a new inorganic- organic hybrid compound for nonlinear optical applications: Aquadiiodo (3-aminopropanoic acid) cadmium (II)

    Science.gov (United States)

    Boopathi, K.; Babu, S. Moorthy; Jagan, R.; Ramasamy, P.

    2017-12-01

    The new inorganic-organic hybrid material aquadiiodo (3-aminopropanoic acid) cadmium (II) [ADI (3-AP) Cd] has been successfully synthesized and good quality crystals have been grown by slow evaporation solution technique. The structure was determined by single crystal X-ray diffraction at room temperature. The compound crystallizes in monoclinic crystal system with centro symmetric space group P21/c and four molecules in the unit cell. The structure of the title compound was further confirmed by 1H and 13C nuclear magnetic resonance spectral analysis. FT-IR spectroscopy was used to confirm the presence of various functional groups in the compound. The transmittance and optical parameters of the crystal were studied by UV- Visible-NIR spectroscopy. The thermal stability of the grown crystal was evaluated using thermogravimetric and differential thermal analyses. Mechanical hardness has been identified by Vickers micro hardness study and work hardening coefficient was calculated. Dielectric measurement was carried out as a function of frequency and results are discussed. The growth mechanism of the crystal was assessed by chemical etching studies. The third-order nonlinear optical susceptibility of [ADI (3-AP) Cd] was derived using the Z-scan technique, and it was 3.24955 × 10-8 esu. The positive nonlinear refractive index 2.48505 × 10-11 m2/W, is an indication of self-defocusing optical nonlinearity of the sample. It is believed that the [ADI (3-AP) Cd] is a promising new candidate for developing efficient nonlinear optical and optical power limiting devices.

  6. SYNTHESIS, CHARACTERIZATION, AND CRYSTAL STRUCTURE ...

    African Journals Online (AJOL)

    a

    organic coordination networks based on complexes of transition metals and multifunctional bridging ligands, such as polyamine and polyacid, has proven to be a fertile field due to the intriguing network topologies and potential functions as new ...

  7. SYNTHESIS, CHARACTERIZATION, AND CRYSTAL STRUCTURE ...

    African Journals Online (AJOL)

    a

    calcd. 33.25), H 2.23 (2.37) and N 5.61 (5.54). Analytical data were consistent with the empirical formula of {[Ba2(Hpydc)2(pydc)(H2O)3].H2O.(H2pydc)}n (F.W. 1010.64). A 13C NMR signal at δ. 42 revealed that all Carbon atoms were identical.

  8. Synthesis and investigation of neptunium zirconium phosphate, a member of the NZP family: crystal structure, thermal behaviour and Mössbauer spectroscopy studies

    NARCIS (Netherlands)

    Bykov, D.; Konings, R.J.M.; Apostolidis, C.; Hen, A.; Colineau, E; Wiss, T; Raison, P.

    2017-01-01

    A new double neptunium zirconium phosphate of the type MxZr2(PO4)3 (M = Np), crystallizing in the structure type NaZr2(PO4)3 (NZP, NASICON), was synthesized by solid state reactions at high temperatures and characterized by X-ray diffraction, infrared spectroscopy and Mössbauer spectroscopy. The

  9. 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 - others: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: 1.300, year: 2015

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

    Czech Academy of Sciences Publication Activity Database

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

    2015-01-01

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

  11. Synthesis and crystal structure of tischendorfite, Pd.sub.8./sub.Hg.sub.3./sub.Se.sub.9./sub

    Czech Academy of Sciences Publication Activity Database

    Laufek, F.; Vymazalová, A.; Drábek, M.; Navrátil, J.; Drahokoupil, Jan

    2014-01-01

    Roč. 26, č. 1 (2014), s. 157-162 ISSN 0935-1221 Institutional support: RVO:68378271 Keywords : tischendorfite * crystal structure * Pd-Hg selenides Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.483, year: 2014

  12. Synthesis and X-ray crystal structure of a novel organometallic (µ(3)-oxido)(µ(3)-imido) trinuclear iridium complex

    DEFF Research Database (Denmark)

    Schau-Magnussen, Magnus; Malcho, Phillip; Herbst, Konrad

    2011-01-01

    Reaction of the organometallic aqua ion [Cp*Ir(H(2)O)(3)](2+) with tert-butyl(trimethylsilyl)amine in acetone yielded a novel trinuclear (µ(3)-oxido)(µ(3)-imido)pentamethylcyclopentadienyliridium(iii) complex, [(Cp*Ir)(3)(O)(N(t)Bu)](2+). Single crystal structure analyses show the complex can be ...

  13. Synthesis, Crystal Structures, Magnetic Properties, and Theoretical Investigation of a New Series of NiII-LnIII-WVHeterotrimetallics: Understanding the SMM Behavior of Mixed Polynuclear Complexes.

    Science.gov (United States)

    Vieru, Veacheslav; Pasatoiu, Traian D; Ungur, Liviu; Suturina, Elizaveta; Madalan, Augustin M; Duhayon, Carine; Sutter, Jean-Pascal; Andruh, Marius; Chibotaru, Liviu F

    2016-12-05

    The polynuclear compounds containing anisotropic metal ions often exhibit efficient barriers for blocking of magnetization at fairly arbitrary geometries. However, at variance with mononuclear complexes, which usually become single-molecule magnets (SMM) under the sole requirement of a highly axial crystal field at the metal ion, the factors influencing the SMM behavior in polynuclear complexes, especially, with weakly axial magnetic ions, still remain largely unrevealed. As an attempt to clarify these conditions, we present here the synthesis, crystal structures, magnetic behavior, and ab initio calculations for a new series of Ni II -Ln III -W V trimetallics, [(CN) 7 W(CN)Ni(H 2 O)(valpn)Ln(H 2 O) 4 ]·H 2 O (Ln = Y 1, Eu 2, Gd 3, Tb 4, Dy 5, Lu 6). The surprising finding is the absence of the magnetic blockage even for compounds involving strongly anisotropic Dy III and Tb III metal ions. This is well explained by ab initio calculations showing relatively large transversal components of the g-tensor in the ground exchange Kramers doublets of 1 and 4 and large intrinsic tunneling gaps in the ground exchange doublets of 3 and 5. In order to get more insight into this behavior, another series of earlier reported compounds with the same trinuclear [W V Ni II Ln III ] core structure, [(CN) 7 W(CN)Ni(dmf)(valdmpn)Ln(dmf) 4 ]·H 2 O (Ln = Gd III 7, Tb III 8a, Dy III 9, Ho III 10), [(CN) 7 W(CN)Ni(H 2 O)(valdmpn)Tb(dmf) 2.5 (H 2 O) 1.5 ]·H 2 O·0.5dmf 8b, and [(CN) 7 W(CN)Ni(H 2 O)(valdmpn)Er(dmf) 3 (H 2 O) 1 ]·H 2 O·0.5dmf 11, has been also investigated theoretically. In this series, only 8b exhibits SMM behavior which is confirmed by the present ab initio calculations. An important feature for the entire series is the strong ferromagnetic coupling between Ni(II) and W(V), which is due to an almost perfect trigonal dodecahedron geometry of the octacyano wolframate fragment. The reason why only 8b is an SMM is explained by positive zero-field splitting on the nickel

  14. The first pseudo-ternary thiocyanate containing two alkali metals. Synthesis and single-crystal structure of LiK{sub 2}[SCN]{sub 3}

    Energy Technology Data Exchange (ETDEWEB)

    Reckeweg, Olaf; DiSalvo, Francis J. [Cornell Univ., Ithaca, NY (United States). Baker Lab.

    2016-04-01

    A procedure was empirically developed to prepare the compound LiK{sub 2}[SCN]{sub 3}, which forms colorless, transparent, very fragile, and extremely hygroscopic thin rectangular plates. Its unique crystal structure was determined by single-crystal X-ray diffraction. LiK{sub 2}[SCN]{sub 3} adopts the orthorhombic space group Pna2{sub 1} (no. 33, Z = 4) with the cell parameters a = 1209.32(9), b = 950.85(9), and c = 849.95(6) pm.

  15. Synthesis, spectral characteristics, and the crystal and molecular structures of 2,3-dimethyl-1-phenyl-4-(N-phthalimido)pyrazolone-5

    International Nuclear Information System (INIS)

    Sokol, V. I.; Strashnova, S. B.; Kovalchukova, O. V.; Sergienko, V. S.; Davydov, V. V.; Zaitsev, B. E.; Evtushenko, Yu. M.

    2008-01-01

    2,3-Dimethyl-1-phenyl-4-(N-phthalimido)pyrazolone-5 (I) is synthesized and isolated in the form of single crystals. The crystal structure of compound I is determined using X-ray diffraction. The phthalimide and pyrazolone rings in the molecule are not coplanar: the angle between their median planes is 56.4 o . The bond lengths in the rings level off, which indicates the delocalization of the electron density. The spectral characteristics (IR and electronic spectra) of molecule I are determined.

  16. Synthesis and Crystal Structure of Benzyl [(1S-1-(5-amino-1,3,4-oxadiazol-2-yl-2-phenylethyl]carbamate

    Directory of Open Access Journals (Sweden)

    Reik Löser

    2012-08-01

    Full Text Available The conversion of Z-phenylalanine hydrazide with cyanogen bromide resulted in the formation of the corresponding 2-amino-1,3,4-oxadiazole by spontaneous cyclization of the intermediary cyanohydrazide. The molecular structure of the product was confirmed by single crystal X-ray diffraction. Crystals of the title compound where obtained from a saturated solution in a mixture of petroleum ether and ethyl acetate and belong to the monoclinic space group P21 with unit cell parameters a = 9.8152(2 Å, b = 9.6305(2 Å, c = 9.8465(2 Å, β = 116.785(1°. The asymmetric unit contains one molecule.

  17. Synthesis, crystal structure and Raman spectrum of K2[(Pt2(HPO44(H2O2] containing (Pt26+ ions

    Directory of Open Access Journals (Sweden)

    2009-03-01

    Full Text Available In the crystal structure of the acid platinum phosphate dipotassium di-μ-hydrogenphosphato-bis[aquaplatinum(III](Pt—Pt, K2[Pt2(HPO44(H2O2], the (Pt26+ dumbbells within the paddle-wheel complex show Pt—Pt distances of 2.4944 (5 and 2.4892 (5 Å. The pottassium ions are seven-fold coordinated by hydrogenphosphate groups. In the crystal, O—H...O hydrogen bonds help to establish the packing. The Raman spectrum was recorded.

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

    Science.gov (United States)

    Muche, Simon; Müller, Matthias; Hołyńska, Małgorzata

    2018-03-01

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

  19. Synthesis and crystal structure of a polymeric zinc(II complex derived from 4-nitro- phenylacetic acid and propane-1,3-diamine

    Directory of Open Access Journals (Sweden)

    G-H. Sheng

    2014-05-01

    Full Text Available A new polymeric zinc(II complex, [ZnL2(PDA]n, has been prepared by the reaction of zinc sulfate, 4-nitrophenylacetic acid, and propane-1,3-diamine (PDA in water. Structure of the complex has been characterized by single-crystal X-ray diffraction. The complex crystallizes as orthorhombic space group Pnma, with unit cell dimensions a = 15.732(1 Å, b = 23.912(1 Å, c = 5.5565(3 Å, V = 2090.2(2 Å3, Z = 4, R1 = 0.0427, wR2 = 0.0968, S = 1.048. The Zn atom is coordinated in a tetrahedral geometry. Single crystals of the complex are stabilized by hydrogen bonds and p···p interactions. DOI: http://dx.doi.org/10.4314/bcse.v28i2.17

  20. Synthesis and characterization of the crystal and magnetic structures and properties of the hydroxyfluorides Fe(OH)F and Co(OH)F.

    Science.gov (United States)

    Ben Yahia, Hamdi; Shikano, Masahiro; Tabuchi, Mitsuharu; Kobayashi, Hironori; Avdeev, Maxim; Tan, Thiam Teck; Liu, Samuel; Ling, Chris D

    2014-01-06

    The title compounds were synthesized by a hydrothermal route from a 1:1 molar ratio of lithium fluoride and transition-metal acetate in an excess of water. The crystal structures were determined using a combination of powder and/or single-crystal X-ray and neutron powder diffraction (NPD) measurements. The magnetic structure and properties of Co(OH)F were characterized by magnetic susceptibility and low-temperature NPD measurements. M(OH)F (M = Fe and Co) crystallizes with structures related to diaspore-type α-AlOOH, with the Pnma space group, Z = 4, a = 10.471(3) Å, b = 3.2059(10) Å, and c = 4.6977(14) Å and a = 10.2753(3) Å, b = 3.11813(7) Å, and c = 4.68437(14) Å for the iron and cobalt phases, respectively. The structures consist of double chains of edge-sharing M(F,O)6 octahedra running along the b axis. These infinite chains share corners and give rise to channels. The protons are located in the channels and form O-H···F bent hydrogen bonds. The magnetic susceptibility indicates an antiferromagnetic ordering at ∼40 K, and the NPD measurements at 3 K show that the ferromagnetic rutile-type chains with spins parallel to the short b axis are antiferromagnetically coupled to each other, similarly to the magnetic structure of goethite α-FeOOH.

  1. Materials research at Stanford University. [composite materials, crystal structure, acoustics

    Science.gov (United States)

    1975-01-01

    Research activity related to the science of materials is described. The following areas are included: elastic and thermal properties of composite materials, acoustic waves and devices, amorphous materials, crystal structure, synthesis of metal-metal bonds, interactions of solids with solutions, electrochemistry, fatigue damage, superconductivity and molecular physics and phase transition kinetics.

  2. A zero dimensional hybrid organic-inorganic perovskite ZnCl4 based: Synthesis, crystal structure, UV-vis, and electronic properties

    Science.gov (United States)

    El Mrabet, Rajae; Kassou, Said; Tahiri, Obaida; Belaaraj, Abdesselam; El Ammari, Lahcen; Saadi, Mohamed

    2017-08-01

    A low dimensional hybrid perovskite-like system [H3Nsbnd (CH2)8sbnd NH3]ZnCl4 was synthesized by slow evaporation method at room temperature. Single crystal X-ray diffraction was used to characterize the crystal structure. The compound crystallizes into triclinic system P-1 space group with mutually surrounded inorganic (ZnCl4)-2 organic (H3Nsbnd (CH2)8sbnd NH3) entities, and the following unit cell parameters: a = 6.9998(1) Å, b = 10.7846(2) Å, c = 11.0332(2) Å, α = 83.1730(10)°, β = 82.0490(10)°, γ = 73.2820(10)°, V = 787.27(2) Å3 and Z = 2. The optical band gap deduced from UV-visible spectroscopy was found to be 4.9 eV. Hirshfeld surface analysis shows the importance of hydrogen bonding interactions to ensure the cohesion of the studied crystal. The band structures and electronic properties, such as total and partial densities of state, were investigated by density functional theory (DFT) using a local LDA and semi local GGA approaches. The obtained results reveal the insulating behavior of the material.

  3. Synthesis, Crystal Structure, and Nonlinear Optical Properties of a New Alkali and Alkaline Earth Metal Carbonate RbNa5Ca5(CO38

    Directory of Open Access Journals (Sweden)

    Qiaoling Chen

    2016-12-01

    Full Text Available A new nonlinear optical (NLO material, RbNa5Ca5(CO38, has been synthesized by the hydrothermal method. The crystal structure is established by single-crystal X-ray diffraction. RbNa5Ca5(CO38 crystallizes in the hexagonal crystal system with space group P63mc (No. 186. The structure of RbNa5Ca5(CO38 can be described as the adjacent infinite [CaCO3]∞ layers lying in the a-b plane bridged through standing-on-edge [CO3] groups by sharing O atoms (two-fold coordinated to build a framework with four types of tunnels running through the b-axis. The Rb, Na, and [Na0.67Ca0.33] atoms reside in these tunnels, respectively. The measurement of second harmonic generation (SHG indicated that RbNa5Ca5(CO38 is a phase-matchable material, which had SHG responses of approximately 1×KH2PO4 (KDP. Meanwhile, the results from the UV-VIS diffuse reflectance spectroscopy study of the powder samples indicated that the UV cut-off edges of RbNa5Ca5(CO38 is about 203 nm.

  4. Synthesis and crystal structures of 2-methyl-4-aryl-5-oxo-5H-indeno [1,2-b] pyridine carboxylate derivatives

    DEFF Research Database (Denmark)

    Pandian, Ramesh; Naushad, Edayadulla; Vijayakumar, Vinodhkumar

    2014-01-01

    pyridine derivatives through oxidation. Consequently, the interest in this aromatization reaction, investigation of a wide range of 1, 4-DHPs continues to attract the attention of researchers. Herein, we report the preparation of pyridine derivatives and the crystal structures determined by X-ray...... crystallographic methods.Results: The crystal structures and conformational studies of two organic compounds, namely ethyl 2-methyl-4-phenyl-5-oxo-5H-indeno [1,2-b] pyridine-3-carboxylate (I) and ethyl 2-methyl-4-(4 chlorophenyl)-5-oxo-5H-indeno [1,2-b] pyridine-3-carboxylate (II) are reported. The terminal ethyl...... is disordered. In compound II, the substitution of Cl atom in the phenyl ring alters the configuration of carboxylate group with respect to the pyridine indane ring. © 2014 Pandian et al.; licensee Chemistry Central Ltd....

  5. Microwave-Assisted Synthesis and Crystal Structure of Oxo(diperoxo(4,4'-di-tert-butyl-2,2'-bipyridine-molybdenum(VI

    Directory of Open Access Journals (Sweden)

    Alírio E. Rodrigues

    2009-09-01

    Full Text Available The oxodiperoxo complex MoO(O22(tbbpy (tbbpy = 4,4'-di-tert-butyl-2,2'- bipyridine was isolated from the reaction of MoO2Cl2(tbbpy in water under microwaveassisted heating at 120 ºC for 4 h. The structure of the oxodiperoxo complex was determined by single crystal X-ray diffraction. The MoVI centre is seven-coordinated with a geometry which strongly resembles a highly distorted bipyramid. Individual MoO(O22(tbbpy complexes are interdigitated along the [010] direction to form a column. The crystal structure is formed by the close packing of the columnar-stacked complexes. Interactions between neighbouring columns are essentially of van der Waals type mediated by the need to effectively fill the available space.

  6. Synthesis and crystal structure of hydrogen phosphites RbH2PO3, CsH2PO3, and TlH2PO3

    International Nuclear Information System (INIS)

    Kosterina, E.V.; Troyanov, S.I.; Kemnits, Eh.; Aslanov, L.A.

    2001-01-01

    The crystal acid phosphites RbH 2 PO 3 , CsH 2 PO 3 and TlH 2 PO 3 were separated during reaction of Rb, Cs and Tl carbonates with phosphorous acid solution. The crystal structure of the compounds was analyzed by X-ray diffraction method at 150 K. CsH 2 PO 3 has a monoclinic system, a = 7.930(2), b = 8.929(2), c = 13.163(3) A, β = 104.84(3) Deg, V = 900.9(4) A 3 , Z 8, sp. gr. P2 1 /c, R 1 = 0.239. In the structure hydrogen bonds integrate the PHO 3 tetrahedrons in the unlimited zigzag chains [HPHO 3 ] n n- laying at the layers, which are alternate to the layers of metal cations. The layers of anion chains have a wavy form [ru

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

  8. Synthesis and crystal structures of 2-methyl-4-aryl-5-oxo-5H-indeno [1,2-b] pyridine carboxylate derivatives

    DEFF Research Database (Denmark)

    Pandian, Ramesh; Naushad, Edayadulla; Vijayakumar, Vinodhkumar

    2014-01-01

    pyridine derivatives through oxidation. Consequently, the interest in this aromatization reaction, investigation of a wide range of 1, 4-DHPs continues to attract the attention of researchers. Herein, we report the preparation of pyridine derivatives and the crystal structures determined by X......-ray crystallographic methods.Results: The crystal structures and conformational studies of two organic compounds, namely ethyl 2-methyl-4-phenyl-5-oxo-5H-indeno [1,2-b] pyridine-3-carboxylate (I) and ethyl 2-methyl-4-(4 chlorophenyl)-5-oxo-5H-indeno [1,2-b] pyridine-3-carboxylate (II) are reported. The terminal ethyl......) dimer running along 011 direction.Conclusion: The crystal structures ethyl 2-methyl-4-phenyl-5-oxo-5H-indeno [1,2-b] pyridine-3-carboxylate and ethyl 2-methyl-4-(4 chlorophenyl)-5-oxo-5H-indeno [1,2-b] pyridine-3-carboxylate have been investigated in detail. The terminal ethyl group of compound I...

  9. New Cu (II), Co(II) and Ni(II) complexes of chalcone derivatives: Synthesis, X-ray crystal structure, electrochemical properties and DFT computational studies

    Science.gov (United States)

    Tabti, Salima; Djedouani, Amel; Aggoun, Djouhra; Warad, Ismail; Rahmouni, Samra; Romdhane, Samir; Fouzi, Hosni

    2018-03-01

    The reaction of nickel(II), copper(II) and cobalt(II) with 4-hydroxy-3-[(2E)-3-(1H-indol-3-yl)prop-2-enoyl]-6-methyl-2H-pyran-2-one (HL) leads to a series of new complexes: Ni(L)2(NH3), Cu(L)2(DMF)2 and Co(L)2(H2O). The crystal structure of the Cu(L)2(DMF)2 complex have been determined by X-ray diffraction methods. The Cu(II) lying on an inversion centre is coordinated to six oxygen atoms forming an octahedral elongated. Additionally, the electrochemical behavior of the metal complexes were investigated by cyclic voltammetry at a glassy carbon electrode (GC) in CH3CN solutions, showing the quasi-reversible redox process ascribed to the reduction of the MII/MI couples. The X-ray single crystal structure data of the complex was matched excellently with the optimized monomer structure of the desired compound; Hirschfeld surface analysis supported the packed crystal lattice 3D network intermolecular forces. HOMO/LUMO energy level and the global reactivity descriptors quantum parameters are also calculated. The electrophilic and nucleophilic potions in the complex surface are theoretically evaluated by molecular electrostatic potential and Mulliken atomic charges analysis.

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

    Science.gov (United States)

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

    2018-03-01

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

  11. Synthesis, crystal structure and magnetic properties of the two polymorphs of novel S=1 osmate; Li{sub 4}MgOsO{sub 6}

    Energy Technology Data Exchange (ETDEWEB)

    Nguyen, Phoung-Hieu T. [Department of Chemistry and Biochemistry, California State University, 1250 Bellflower Blvd., Long Beach, CA 90840-3903 (United States); Kemei, Moureen C. [Materials Department and Materials Research Laboratory, University of California, Santa Barbara, CA 93106-5121 (United States); Tan, Malinda S. [Department of Chemistry and Biochemistry, California State University, 1250 Bellflower Blvd., Long Beach, CA 90840-3903 (United States); Derakhshan, Shahab, E-mail: shahab.derakhshan@csulb.edu [Department of Chemistry and Biochemistry, California State University, 1250 Bellflower Blvd., Long Beach, CA 90840-3903 (United States)

    2016-10-15

    Li{sub 4}MgOsO{sub 6} was synthesized by two different solid-state reaction procedures. The crystal structures were determined by X-ray powder diffraction technique and it was revealed that Li{sub 4}MgOsO{sub 6} crystallizes in two different crystal symmetries in ordered rock salt structure type, namely monoclinic C2/m and orthorhombic Fddd. The unit cell constants for the monoclinic system are a=5.1074(4) Å, b=8.8182(4) Å, c=5.0902(2) Å, and β=109.845(4)° and those of the orthorhombic structure are a=5.8485(1) Å, b=8.3821(1) Å, and c=17.6212(3) Å. In both systems, Os{sup 6+} ions reside exclusively in a specific crystallographic position while Li{sup +} and Mg{sup 2+} ions exhibit mix occupancy. The temperature dependent magnetic susceptibility data for both S=1 osmate systems do not support the occurrence of any magnetic transition down to 2 K. The Curie–Weiss fit to the paramagnetic regime of the magnetic susceptibility data reveal highly negative θ value (−114.81 K and −121.87 K for C2/m and for Fddd systems, respectively), which are indicative of predominant antiferromagnetic (AFM) interactions in both systems. The experimental effective magnetic moment (μ{sub eff}) value for the monoclinic phase is 2.13 μB and that of the orthorhombic system is 2.34 μB. Due to the rather strong AFM interactions and lack of magnetic transition down to 2 K, both of these novel osmates are placed in the class of highly frustrated magnets. Low temperature magnetic susceptibility (below 2 K) and dynamic magnetic properties studies (μsr studies) are in order to better understand the magnetic ground states of these two polymorphs of Li{sub 4}MgOsO{sub 6}. - Graphical abstract: The structural transformation between two modifications of highly frustrated Li{sub 4}MgOsO{sub 6}. - Highlights: • Li4MgOsO{sub 6} was synthesized in two different crystal systems. • The monoclinic variant crystallizes in C2/m space group, while the orthorhombic version forms in Fddd

  12. 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.

  13. Synthesis, Crystal Structure, and Magnetic Properties of Giant Unit Cell Intermetallics R117Co52+δSn112+γ (R = Y, La, Pr, Nd, Ho

    Directory of Open Access Journals (Sweden)

    Ping Chai

    2016-12-01

    Full Text Available Ternary intermetallics R117Co52+δSn112+γ (R = Y, La, Pr, Nd, and Ho have been prepared by arc-melting followed by annealing at 800 °C. All the compounds belong to the Tb117Fe52Ge112 structure type (space group Fm 3 ¯ m characterized by a complex giant cubic unit cell with a ~ 30 Å. The single-crystal structure determination of Y- and La-containing compounds reveals a significant structural disorder. A comparison of these and earlier reported crystal structures of R117Co52+δSn112+γ suggests that more extensive disorder occurs for structures that contain larger lanthanide atoms. This observation can be explained by the need to maintain optimal bonding interactions as the size of the unit cell increases. Y117Co56Sn115 exhibits weak paramagnetism due to the Co sublattice and does not show magnetic ordering in the 1.8–300 K range. Ho117Co55Sn108 shows ferromagnetic ordering at 10.6 K. Both Pr117Co54Sn112 and Nd117Co54Sn111 exhibit antiferromagnetic ordering at 17 K and 24.7 K, respectively, followed by a spin reorientation transition at lower temperature.

  14. Synthesis, crystal structure and electrical properties of N,N-dimethylanilinium trichloridostannate (II): (C8H12N)SnCl3

    Science.gov (United States)

    Chouaib, H.; Kamoun, S.; Costa, L. C.; Graça, M. P. F.

    2015-12-01

    A new (C8H12N)SnCl3 crystal of the general formula AMX3 was grown by soft chemistry method. X-ray study shows that the crystal crystallized in a monoclinic system with the space group P21/a. The structure was solved by Patterson method and refined to a final value of R = 0.0304 for 1157 independent observed reflections. The cohesion and the stability of the atomic arrangement result from the N-H … Cl hydrogen bonds between (C8H12N)+ cations and isolated (SnCl3)- anions. At high temperature this compound exhibits a structural phase transition at 340 K. This transition has been characterized by differential scanning calorimetric and impedance spectroscopy. The impedance data were well fitted to an Rp//CPE equivalent electrical circuit model. The close values of activation energies, obtained from the thermal behavior of the conductivity and the relaxation time confirm the presence of a hopping transport mechanism.

  15. A new copper(II) Schiff base complex containing asymmetrical tetradentate N2O2 Schiff base ligand: Synthesis, characterization, crystal structure and DFT study

    Science.gov (United States)

    Grivani, Gholamhossein; Baghan, Sara Husseinzadeh; Vakili, Mohammad; Khalaji, Aliakbar Dehno; Tahmasebi, Vida; Eigner, Václav; Dušek, Michal

    2015-02-01

    A new copper (II) Schiff base complex, CuL1, was prepared from the reaction of asymmetrical Schiff base ligand of L1 and Cu(OAC)2 (L1 = salicylidene imino-ethylimino-pentan-2-one). The Schiff base ligand, L1, and its copper (II) complex, CuL1, have been characterized by elemental analysis (CHN) and FT-IR and UV-vis spectroscopy. In addition, 1H NMR was employed for characterization of the ligand. Thermogrametric analysis of the CuL1 reveals its thermal stability and its decomposition pattern shows that it is finally decomposed to the copper oxide (CuO). The crystal structure of CuL1 was determined by the single crystal X-ray analysis. The CuL1 complex crystallizes in the monoclinic system, with space group P21/n and distorted square planar coordination around the metal ion. The Schiff base ligand of L1 acts as a chelating ligand and coordinates via two nitrogen and two oxygen atoms to the copper (II) ion with C1 symmetry. The structure of the CuL1 complex was also studied theoretically at different levels of DFT and basis sets. According to calculated results the Csbnd O bond length of the salicylate fragment is slightly higher than that in the acetylacetonate fragment of ligand, which could be interpreted by resonance increasing between phenyl and chelated rings in ligand in relative to the acetylacetonate fragment.

  16. Synthesis and thermoelectric properties of Re3As6.6In0.4 with Ir3Ge7 crystal structure

    Science.gov (United States)

    Verchenko, Valeriy Y; Vasiliev, Anton S; Tsirlin, Alexander A; Kulbachinskii, Vladimir A; Kytin, Vladimir G

    2013-01-01

    Summary The Re3As7− xInx solid solution was prepared for x ≤ 0.5 by heating the elements in stoichiometric ratios in evacuated silica tubes at 1073 K. It crystallizes with the Ir3Ge7 crystal structure, space group Im−3m, with a unit-cell parameter a ranging from 8.716 to 8.747 Å. The crystal structure and properties were investigated for a composition with x = 0.4. It is shown that indium substitutes arsenic exclusively at one crystallographic site, such that the As–As dumbbells with d As–As = 2.54 Å remain intact. Re3As6.6In0.4 behaves as a bad metal or heavily doped semiconductor, with electrons being the dominant charge carriers. It possesses high values of Seebeck coefficient and low thermal conductivity, but relatively low electrical conductivity, which leads to rather low values of the thermoelectric figure of merit. PMID:23946913

  17. Synthesis and thermoelectric properties of Re3As6.6In0.4 with Ir3Ge7 crystal structure

    Directory of Open Access Journals (Sweden)

    Valeriy Y. Verchenko

    2013-07-01

    Full Text Available The Re3As7−xInx solid solution was prepared for x ≤ 0.5 by heating the elements in stoichiometric ratios in evacuated silica tubes at 1073 K. It crystallizes with the Ir3Ge7 crystal structure, space group Im−3m, with a unit-cell parameter a ranging from 8.716 to 8.747 Å. The crystal structure and properties were investigated for a composition with x = 0.4. It is shown that indium substitutes arsenic exclusively at one crystallographic site, such that the As–As dumbbells with dAs–As = 2.54 Å remain intact. Re3As6.6In0.4 behaves as a bad metal or heavily doped semiconductor, with electrons being the dominant charge carriers. It possesses high values of Seebeck coefficient and low thermal conductivity, but relatively low electrical conductivity, which leads to rather low values of the thermoelectric figure of merit.

  18. Synthesis, crystal structure, Hirshfeld surface analysis, spectroscopic characterization, reactivity study by DFT and MD approaches and molecular docking study of a novel chalcone derivative

    Science.gov (United States)

    Arshad, Suhana; Pillai, Renjith Raveendran; Zainuri, Dian Alwani; Khalib, Nuridayanti Che; Razak, Ibrahim Abdul; Armaković, Stevan; Armaković, Sanja J.; Panicker, C. Yohannan; Van Alsenoy, C.

    2017-05-01

    In the present study, the title compound named as (E)-1-(4-bromophenyl)-3-(4-(trifluoromethyl)phenyl)prop-2-en-1-one was synthesized and structurally characterized by single-crystal X-ray diffraction. The compound crystallizes in monoclinic crystal system in P21/c space group, unit cell parameters a = 16.7629 (12) Å, b = 13.9681 (10) Å, c = 5.8740 (4) Å, β = 96.3860 (12)° and Z = 4. Hirshfeld surface analysis revealed that the molecular structure is dominated by H⋯H, C⋯H/H⋯C, Br⋯F/F⋯Br and F⋯F contacts. The FT-IR spectrum was recorded and interpreted in details with the aid of Density Functional Theory (DFT) calculations and Potential Energy Distribution (PED) analysis. Average local ionization energies (ALIE) and Fukui functions have been used as quantum-molecular descriptors to locate the molecule sites that could be of importance from the aspect of reactivity. Degradation properties have been assessed by calculations of bond dissociation energies (BDE) for hydrogen abstraction and the rest of the single acyclic bonds, while molecular dynamics (MD) simulations were used in order to calculate radial distribution functions and determine the atoms with significant interactions with water. In order to understand how the title molecule inhibits and hence increases the catalytic efficiency of MOA-B enzyme, molecular docking study was performed.

  19. Synthesis and crystal structure of tetra(quinolin-8-olatothorium ethanol solvate, Th(C9H6NO4*C2H5OH

    Directory of Open Access Journals (Sweden)

    Holger Kohlmann

    2014-07-01

    Full Text Available Metal quinolinolates (also known as oxinates have been widely used for gravimetric analysis and in recent days as materials for organic light emitting diodes (OLEDs. Recrystallisation of tetra(quinolin-8- olatothorium(IV (ThQ4 yielded yellow, translucent, prismatic crystals of the title compound, ThQ4*C2H5OH, the single-crystal structure of which is described. Only one crystallographically distinct molecule is found, all ligands are crystallographically inequivalent. Thorium is coordinated by four 8-hydroxyquinolinato with average Th-O distances of 233.3 pm and average Th-N distances of 272.4 pm, and one ethanol ligand with a Th-O distance 256.7 pm. O and N surroundings around thorium can be described by a tricapped trigonal prism. In contrast to quinolinates of the trivalent metals, ThQ4*C2H5OH does not fluoresce under UV irradiation, which is in accordance with the lack of π-π overlap in the crystal structure.

  20. Synthesis and Crystal Structure of a 4,4'-bipyridine Linked Dinuclear Copper(II) Complex Derived from 2-{[2-(2-hydroxyethylamino)ethylimino]methyl}-6-methylphenol.

    Science.gov (United States)

    Zhang, Xiu-Zhen; Gu, Yitong; Li, Yuntong; Liu, Andong; Liu, Fuyao; You, Zhonglu; Zhu, Hai-Liang

    2016-12-01

    A novel 4,4'-bipyridine linked dinuclear copper(II) complex, [Cu2L2(bipy)](NO3)2·bipy (L = 2-[2-(2-hydroxyethylamino) ethylimino]methyl-6-methylphenol; bipy = 4,4'-bipyridine), was prepared and characterized by elemental analyses, IR spectroscopy, and single-crystal X-ray diffraction. The Cu···Cu distance is 11.129(2) Å. The CuII atom is coordinated by one phenolate O, one imine N, and one amine N atoms of a Schiff base ligand, and one N atom of the bridging 4,4'-bipyridine ligand, forming a square planar geometry. In the crystal structure of the complex, the dinuclear copper complex cations are linked by 4,4'-bipyridine molecules through intermolecular O-H···N hydrogen bonds, to form 1D chains running in the [2 0 -1] direction.

  1. Study of the influence in crystallization period in MCM-22 zeolite synthesis

    International Nuclear Information System (INIS)

    Barbosa, A.S.; Santos, E.R.F.; Rodrigues, M.G.F.

    2011-01-01

    The synthesis of MCM-22 is accomplished by hydrothermal treatment and long periods needed for crystallization, with the gradual growth of crystals of 10-14 days. MCM-22 catalyst is studied intensively as promising, with high thermal stability. As part of a line of research focused on the development of zeolite with lowest cost, this study aimed to examine the effect in decreasing the period of crystallization in the synthesis of zeolite MCM-22. The materials were characterized by X-ray diffraction (XRD) spectroscopy, X-ray Energy Dispersive (EDX) and Fourier transform infrared spectroscopy and Fourier transform (FT-IR). By XRD it was observed that the hydrothermal treatment used in the synthesis was effective during periods of crystallization and EDX was observed that the samples have a high percentage of silica and low alumina content, which gives them a high ratio SiO 2 /Al 2 O 3 characteristic of the MWW structure. (author)

  2. Synthesis, crystal structure, catalytic and anti-Trypanosoma cruzi activity of a new chromium(III) complex containing bis(3,5-dimethylpyrazol-1-yl)methane

    Science.gov (United States)

    Hurtado, John; Ibarra, Laura; Yepes, David; García-Huertas, Paola; Macías, Mario A.; Triana-Chavez, Omar; Nagles, Edgar; Suescun, Leopoldo; Muñoz-Castro, Alvaro

    2017-10-01

    The reaction of CrCl36H2O with the ligand bis(3,5-dimethylpyrazol-1-yl)methane (L) yielded the cationic complex [(Cr(L)(H2O)2Cl2]+, which crystallized as the chloride trihydrate [(Cr(L)(H2O)2Cl2]Cl·3H2O. The chromium complex was characterized by elemental analysis, electrical conductivity, Infrared and Ultraviolet/Visible spectroscopy. The crystal structure determination using single-crystal X-ray diffraction showed a chromium center in a distorted octahedral coordination sphere. In the crystal, the packing was directed by Osbnd H⋯(O,Cl) hydrogen bonds and weak Csbnd H⋯O interactions to build a monoclinic P21/c supramolecular structure. The complex showed excellent properties as an initiator for the ring opening polymerization of є-caprolactone (CL) under solvent-free conditions. The obtained polymer showed high crystallinity (89.9%) and a decomposition temperature above 475 °C. In addition, the new complex was evaluated against epimastigotes from Trypanosoma cruzi (T. cruzi) strains. The results indicated that this complex has a high activity against this parasite with a minimum inhibitory concentration 50 (MIC50) of 1.08 μg/mL. Interestingly, this compound showed little effect on erythrocytes, indicating that it is not cytotoxic. These results provide interesting contributions to the design of metal complexes by using simple and accessible ligands with activity against T. cruzi and with potential applications in the polymerization of CL.

  3. Synthesis and ultrastructure of plate-like apatite single crystals as a model for tooth enamel

    Energy Technology Data Exchange (ETDEWEB)

    Zhuang, Zhi, E-mail: zhuang@meiji.ac.jp [Department of Applied Chemistry, School of Science and Technology, Meiji University, 1-1-1 Higashimita, Tama-ku, Kawasaki, Kanagawa 214-8571 (Japan); Yoshimura, Hideyuki, E-mail: hyoshi@isc.meiji.ac.jp [Department of Physics, School of Science and Technology, Meiji University, 1-1-1 Higashimita, Tama-ku, Kawasaki, Kanagawa 214-8571 (Japan); Aizawa, Mamoru, E-mail: mamorua@isc.meiji.ac.jp [Department of Applied Chemistry, School of Science and Technology, Meiji University, 1-1-1 Higashimita, Tama-ku, Kawasaki, Kanagawa 214-8571 (Japan)

    2013-07-01

    Hydroxyapatite (HAp) is an inorganic constituent compound of human bones and teeth, with superior biocompatibility and bioactivity characteristics. Its crystal structure is hexagonal, characterized by a(b)- and c-planes. In vertebrate long bones, HAp crystals have a c-axis orientation, while in tooth enamel, they have an a(b)-axis orientation. Many methods can be used to synthesize c-axis oriented HAp single crystals; however, to the best of our knowledge, there have been no reports on a synthesis method for a(b)-axis oriented HAp single crystals. In this study, we successfully synthesized plate-like HAp crystals at the air–liquid interface of a starting solution via an enzyme reaction of urea with urease. Crystal phase analysis and ultrastructure observations were carried out, and the results indicated that the particles were single crystals, with almost the same a(b)-axis orientation as tooth enamel. It is hoped that by utilizing their unique surface charge and atomic arrangement, the resulting particles can be used as a high-performance biomaterial, capable of adsorbing bio-related substances and a model for tooth enamel. - Highlights: ► Synthesis of plate-like hydroxyapatite crystals at air–liquid interface ► Ultrastructural analysis of plate-like hydroxyapatite crystals ► Plate-like hydroxyapatite single crystals with a high a(b)-axis orientation ► Plate-like hydroxyapatite single crystals as a model for tooth enamel.

  4. Synthesis and Physical Properties of Liquid Crystals: An Interdisciplinary Experiment

    Science.gov (United States)

    Van Hecke, Gerald R.; Karukstis, Kerry K.; Hanhan Li; Hendargo, Hansford C.; Cosand, Andrew J.; Fox, Marja M.

    2005-01-01

    A study involves multiple chemistry and physics concepts applied to a state of matter that has biological relevance. An experiment involving the synthesis and physical properties of liquid crystals illustrates the interdisciplinary nature of liquid crystal research and the practical devices derived from such research.

  5. Synthesis, crystal structure and magnetic properties of a new pillared perovskite La5Mo2.75V1.25O16

    International Nuclear Information System (INIS)

    Ramezanipour, Farshid; Derakhshan, Shahab; Greedan, John E.; Cranswick, Lachlan M.D.

    2008-01-01

    A new pillared perovskite compound La 5 Mo 2.76(4) V 1.25(4) O 16 , has been synthesized by solid-state reaction and its crystal structure has been characterized using powder X-ray and neutron diffraction. The magnetic properties of this compound have been investigated using SQUID magnetometry, and the magnetic structure has been studied using neutron diffraction data. A theoretical calculation of relative strengths of spin interactions among different magnetic ions and through different pathways has been performed using extended Hueckel, spin dimer analysis. The crystal structure of this material contains perovskite-type layers that are connected through edge-sharing dimeric units of octahedra. The structure is described in space group C2/m with unit cell parameters a=7.931(2) A, b=7.913(2) A, c=10.346(5) A and β=95.096(5) o . The material shows both short-range ferrimagnetic correlations from ∼200 to 110 K and long-range antiferromagnetic order below T c ∼100 K. The magnetic structure was investigated by neutron diffraction and is described by k=(0 0 1/2 ) as for other pillared perovskites. It consists of a ferrimagnetic arrangement of Mo and V within the layers that are coupled antiferromagnetically between layers. This is the first magnetic structure determination for any Mo-based pillared perovskite. - Graphical abstract: Long-range magnetic order below 100 K in the pillared perovskite La 5 Mo 2.75 V 1.25 O 16 . The magnetic structure is shown in the inset

  6. Synthesis and single crystal X-ray analysis of two griseofulvin metabolites

    DEFF Research Database (Denmark)

    Rønnest, Mads Holger; Harris, Pernille; Gotfredsen, Charlotte Held

    2010-01-01

    The two phenols, 6-O-desmethyl griseofulvin and 4-O-desmethyl griseofulvin are metabolites of the antifungal drug griseofulvin. Herein, we present an improved synthesis of the 6-phenol derivative, and an unequivocal proof of both structures by single-crystal X-ray analysis.......The two phenols, 6-O-desmethyl griseofulvin and 4-O-desmethyl griseofulvin are metabolites of the antifungal drug griseofulvin. Herein, we present an improved synthesis of the 6-phenol derivative, and an unequivocal proof of both structures by single-crystal X-ray analysis....

  7. New isoxazole(3,5)substituted thiosemicarbazone: Synthesis, crystal structure and spectroscopic studies of the binding mode to protein and calf thymus DNA

    Science.gov (United States)

    Bomfim Filho, Lucius F. O.; Barbosa, Rafaela S.; Burgos C., Ana E.; Rodrigues, Bernardo L.; Teixeira, Letícia R.

    2017-12-01

    Six new 3,5-isoxazole thiosemicarbazone derivatives (ITCs) (HL1 - HL6) were synthesized and characterized using microanalysis, spectroscopic methods and for HL2, HL3, HL5 and HL6a by a single crystal X-ray diffraction. The combined analyses, utilizing NMR and X-ray techniques, showed that the compounds presented an E conformation both in solution and solid state. The intermolecular N3sbnd H3N···S1 hydrogen bonds, between the thiosemicarbazone groups, resulted in rings for all crystals. For HL2 and HL5, one medium strength (N4sbnd H4N···S1) and one weak (C8sbnd H8···N1) intermolecular hydrogen bond was also observed. HL3 presented a π(ar)- π(ar) stacking interaction and HL6a was stabilized by three hydrogen bonds involving DMSO oxygen. The interconnections in the crystal structures were analyzed using Hirshfeld surfaces. The interaction studies, using fluorescence and absorbance spectroscopy, showed that the ITCs interacted with DNA and human serum albumin (HSA).

  8. Synthesis, characterization, crystal structure, DNA/BSA binding ability and antibacterial activity of asymmetric europium complex based on 1,10- phenanthroline

    Science.gov (United States)

    Alfi, Nafiseh; Khorasani-Motlagh, Mozhgan; Rezvani, Ali Reza; Noroozifar, Meissam; Molčanov, Krešimir

    2017-06-01

    A heteroleptic europium coordination compound formulated as [Eu(phen)2(OH2)2(Cl)2](Cl)(H2O) (phen = 1,10-phenanthroline), has been synthesized and characterized by elemental analysis, FT-IR spectroscopy, and single-crystal X-ray diffractometer. Crystal structure analysis reveals the complex is crystallized in orthorhombic system with Pca21 space group. Electronic absorption and various emission methods for investigation of the binding system of europium(III) complex to Fish Salmon deoxyribonucleic acid (FS-DNA) and Bovamin Serum Albumin (BSA) have been explored. Furthermore, the binding constants, binding sites and the corresponding thermodynamic parameters of the interaction system based on the van't Hoff equation for FS-DNA and BSA were calculated. The thermodynamic parameters reflect the exothermic nature of emission process (ΔH°<0 and ΔS°<0). The experimental results seem to indicate that the [Eu(phen)2(OH2)2(Cl)2](Cl)(H2O) bound to FS-DNA by non-intercalative mode which the groove binding is preferable mode. Also, the complex exhibits a brilliant antimicrobial activity in vitro against standard bacterial strains.

  9. Synthesis, structure, antitumor activity of novel pharmaceutical co-crystals based on bispyridyl-substituted α, β-unsaturated ketones with gallic acid

    Science.gov (United States)

    Liu, Lian-Dong; Liu, Shu-Lian; Liu, Zhi-Xian; Hou, Gui-Ge

    2016-05-01

    Three novel pharmaceutical co-crystals, (A)·(gallic acid) (1), (B)·(gallic acid) (2), and (C)·(gallic acid) (3) were generated based on 2,6-bis((pyridin-4-yl)methylene)cyclohexanone (A), N-methyl-3,5-bis((pyridin-3-yl)methylene)-4-piperidone (B), N-methyl-3,5-bis((pyridin-4-yl)methylene)-4-piperidone (C) with gallic acid, respectively. They are characterized by elemental analysis, FTIR spectroscopy, 1H NMR and single-crystal X-ray diffraction. Structural analysis reveals that two pharmaceutical ingredients link each other into H-bonding-driven 3D network in 1, 2, or 2D plane in 3. In addition, their antitumor activities against human neoplastic cell lines A549, SGC-7901, MCF-7, OVCA-433, HePG2 and cytotoxicity for HUVEC cell lines by CCK-8 method were evaluated primarily. Compared with gallic acid and free A, B and C, their antitumor activities have improved distinctly, while cytotoxicities have reduced markedly, especially for co-crystal 1. This is mainly because of the synergistic effect between pharmaceutical ingredients A, B, and C and gallic acid.

  10. Synthesis, antityrosinase activity of curcumin analogues, and crystal structure of (1E,4E)-1,5-bis(4-ethoxyphenyl)penta-1,4-dien-3-one

    Energy Technology Data Exchange (ETDEWEB)

    Chantrapromma, S., E-mail: suchada.c@psu.ac.th; Ruanwas, P. [Prince of Songkla University, Department of Chemistry, Faculty of Science (Thailand); Boonnak, N. [Thaksin University, Department of Basic Science and Mathematics, Faculty of Science (Thailand); Chantrapromma, K. [Hatyai University, Faculty of Science and Technology (Thailand); Fun, H.-K. [Universiti Sains Malaysia, X-ray Crystallography Unit, School of Physics (Malaysia)

    2016-12-15

    Five derivatives of curcumin analogue (R = OCH{sub 2}CH{sub 3} (1), R = N(CH{sub 3}){sub 2} (2), R = 2,4,5-OCH{sub 3} (3), R = 2,4,6-OCH{sub 3} (4), and R = 3,4,5-OCH{sub 3} (5)) were synthesized and characterized by {sup 1}H NMR, FT-IR and UV–Vis spectroscopy. The synthesized derivatives were screened for antityrosinase activity, and found that 4 and 5 possess such activity. The crystal structure of 1 was determined by single crystal X-ray diffraction: monoclinic, sp. gr. P2{sub 1}/c, a = 17.5728(15) Å, b = 5.9121(5) Å, c = 19.8269(13) Å, β = 121.155(5)°, Z = 4. The molecule 1 is twisted with the dihedral angle between two phenyl rings being 15.68(10)°. In the crystal packing, the molecules 1 are linked into chains by C−H···π interactions and further stacked by π···π interactions with the centroid–centroid distance of 3.9311(13) Å.

  11. Synthesis, Crystal Structure and Thermal Stability of 1D Linear Silver(I Coordination Polymers with 1,1,2,2-Tetra(pyrazol-1-ylethane

    Directory of Open Access Journals (Sweden)

    Evgeny Semitut

    2016-10-01

    Full Text Available Two new linear silver(I nitrate coordination polymers with bitopic ligand 1,1,2,2-tetra(pyrazol-1-ylethane were synthesized. Synthesized compounds were characterized by IR spectroscopy, elemental analysis, powder X-ray diffraction and thermal analysis. Silver coordination polymers demonstrated a yellow emission near 500 nm upon excitation at 360 nm. Crystal structures of coordination polymers were determined and structural peculiarities are discussed. In both of the structures, silver ions are connected via bridging ligand molecules to form polymeric chains with a five-atomic environment. The coordination environment of the central atom corresponds to a distorted trigonal bipyramid with two N atoms of different ligands in apical positions. The Ag–N bond distances vary in a wide range of 2.31–2.62 Å, giving strongly distorted metallacycles. Thermolysis of coordination polymers in reductive atmosphere (H2/He leads to the formation of silver nanoparticles with a narrow size distribution.

  12. Synthesis, crystal structure and ionic conductivity of the Ba3Mo1-xWxNbO8.5 solid solution

    Science.gov (United States)

    Bernasconi, Andrea; Tealdi, Cristina; Mühlbauer, Martin; Malavasi, Lorenzo

    2018-02-01

    Ba3MoNbO8.5 compound has been recently discovered as novel oxide ionic conductor with a structure that is a hybrid between 9R hexagonal perovskite and palmierite. In this work, the full substitution of Mo with W has been demonstrated as possible, without altering significantly the conductivity of the material. The crystal structure of the Ba3Mo1-xWxNbO8.5 solid solution (with x equals 0, 0.25, 0.5, 0.75 and 1) has been investigated by X-ray powder diffraction, showing a reduction of the unit cell by increasing the molybdenum content, despite the larger size of tungsten compared to molybdenum. Neutron powder diffraction measurements have been performed, indicating different levels of contribution of 9R polytype and of palmierite to the hybrid structure of the material as a function of the W-content.

  13. Synthesis, characterization, crystal structure, superoxide dismutase and biological activities of nickel (II) complexes with bidentate ligands possessing N and O donor atoms

    Science.gov (United States)

    Sangeeta, S.; Ahmad, K.; Noorussabah, N.; Bharti, S.; Mishra, M. K.; Sharma, S. R.; Choudhary, M.

    2017-12-01

    Two new Schiff bases 2-((E)-(4-bromo-2-chlorophenylimino)methyl)-4-bromophenol(HL1) and1-((E)-(4-bromo-2-chlorophenylimino)methyl)naphthalene-2-ol (HL2) and their new nickel (II) complexes [Ni(L1)2]·DMF(1) and [Ni(L2)2] (2) have been synthesized and characterized by various physico- chemical and spectroscopic methods. The solid-state structures of synthesized compounds were determined by single crystal X-ray crystallography, which revealed square planar geometry around Ni (II) ion. Infrared spectra, UV-Vis, thermal analysis and magnetic susceptibility measurements agreed with the observed crystal structures. The ligand (HL1) crystallized in the Orthorhombic system of the space group Pbca,a = 7.5485(4)Å, b = 11.5514(5) Å, c = 30.1370(14)Å, α = 90°, β = 90°, γ = 90°and Z = 8. Complex[Ni(L1)2]·DMF(1) crystallized in the Triclinic system of the space group P-1, a = 8.9954(3) Å, b = 9.4593(4) Å, c = 13.2657(5) Å, α = 101.478°, β = 99.595°, γ = 117.651°and Z = 2, whereas complex [Ni(L2)2]·(2) crystallized in the Monoclinic system of the space group P21/c, a = 9.301(9)Å, b = 12.149(8)Å, c = 13.792(10)Å, α = 90°, β = 106.35(4).°, γ = 90°and Z = 2. The Schiff bases (HL1and HL2) behaved as monobasic bidentate ligands possessing N and O donor atoms. The SOD activities of HL1 and its Ni (II) complex[Ni(L1)2]·DMF(1) have been measured using xanthine-xanthine oxidase as a source of superoxide radical and NBT assay as O2- scavenger. In vitro antimicrobial activities of the Ni(II) complexes (1) and (2)against Bacillus cereus and Staphylococcus aureus as Gram + ve and Salmonella typhi, Klebsiella pneumonia and Escherichia coli as Gram-ve species have been investigated comparing with the Schiff base ligands (HL1and HL2).

  14. A new (4, 6)-connected Cu(I) coordination polymer based on rare tetranuclear [Cu4I2] clusters: Synthesis, crystal structure, luminescent and photocatalytic properties

    Science.gov (United States)

    Cui, Li-Jing; Liu, Chun-Yan; Bian, Ming; Yu, Li-Jun

    2018-03-01

    A new Cu(I) coordination polymer, namely [Cu5I3(L)2]n (1 HL = 3-(4-pyridyl)-5-(3-pyridyl)-1,2,4-triazolyl), was solvothermally synthesized using CuI, HL and NaI as the starting materials. Single crystal X-ray structural analysis shows that compound 1 features a (4, 6)-connected 3D framework employing rare tetranuclear [Cu4I2] clusters as building subunits. It exhibits intense metal-to-ligand luminescence and excellent photocatalytic activity on degradation of methylene blue (MB).

  15. Synthesis, characterization, crystal structure, in-vitro anti-inflammatory and molecular docking studies of 5-mercapto-1-substituted tetrazole incorporated quinoline derivative

    Science.gov (United States)

    Sureshkumar, K.; Maheshwaran, V.; Dharma Rao, T.; Themmila, Khamrang; Ponnuswamy, M. N.; Kadhirvel, Saraboji; Dhandayutham, Saravanan

    2017-10-01

    A novel 5-mercapto-1-substituted tetrazole incorporated quinoline analog was synthesized. The compound 2-Cyclopropyl-4-(4-fluorophenyl)-3-{1-[2-(4-methoxybenzyloxy)ethyl]1H-tetrazol-5-ylsulfanylmethyl}quinoline was characterized by IR, Mass, 1H and 13C NMR spectroscopic techniques. Molecular structure was confirmed by using single crystal X-ray diffraction technique. Thermal behavior was studied by using TGA and DSC techniques. Further, in vitro anti-inflammatory and in silico docking analysis has been carried out to study the activity of the compound.

  16. Synthesis, crystal structure and optical properties of two new layered cadmium iodates: Cd(IO3)X (X=Cl, OH)

    International Nuclear Information System (INIS)

    Yang, Bing-Ping; Mao, Jiang-Gao

    2014-01-01

    Systematic explorations of new compounds in the cadmium iodate system by hydrothermal reactions led to two layered iodates, namely, Cd(IO 3 )X (X=Cl, OH). Cd(IO 3 )Cl crystallizes in the orthorhombic space group Cmca (No. 64) whereas Cd(IO 3 )(OH) crystallizes in the orthorhombic space group Pnma (No. 62). Cd(IO 3 )Cl displays a unique double layered structure composed of 1 ∞ [Cd−O 3 Cl] n chains. Cadmium octahedrons form a 1D chain along the a-axis through edge sharing, and such chains are further interconnected via IO 3 groups to form a special double layer on (020) plane. Cd(IO 3 )(OH) also exhibits a layered structure that is composed of cadmium cations, IO 3 groups and hydroxyl ions. Within a layer, chains of CdO 6 edge-shared octahedra are observed along the b-axis. And these chains are connected by IO 3 groups into a layer parallel to the bc plane. Spectroscopic characterizations, elemental analysis, and thermogravimetric analysis for the reported two compounds are also presented. - Graphical abstract: Two new layered cadmium iodates Cd(IO 3 )X (X=Cl, OH) are reported. Cd(IO 3 )Cl features a unique double layered structure whereas Cd(IO 3 )(OH) displays an ordinary layered structure. - Highlights: • Two new layered cadmium iodates Cd(IO 3 )X (X=Cl, OH) are reported. • Cd(IO 3 )Cl features a unique double layered structure. • Cd(IO 3 )(OH) displays an ordinary layered structure. • The spectroscopic and thermal properties have been studied in detail

  17. Synthesis, crystal structure, and transport properties of Fe substituted rhombohedral skutterudite derivatives Co4−xFexGe6Se6

    KAUST Repository

    Wei, Kaya

    2014-11-01

    We report on the synthesis and low temperature transport properties of rhombohedral derivatives of the cubic skutterudite CoSb3, namely Co4-xFexGe6Se6 with x = 0, 1, 1.5. Rietveld refinement and elemental analyses were used to identify the structure and stoichiometry of the compositions. The thermal conductivity was investigated by employing the Debye model with different phonon-scattering parameters. This investigation demonstrates that Fe substitution is feasible in these skutterudite derivatives and can significantly affect the transport properties as compared with Co4Ge6Se6. © 2014 Elsevier B.V. All rights reserved.

  18. Synthesis, crystal and electronic structures and optical properties of (HIm)2 Hg3Cl8 and (HIm)HgI3 (HIm = imidazolium)

    Energy Technology Data Exchange (ETDEWEB)

    Nhalil, Hariharan [Univ. of Oklahoma, Norman, OK (United States). Dept. of Chemistry and Biochemistry; Whiteside, Vincent R. [Univ. of Oklahoma, Norman, OK (United States). Homer L. Dodge Dept. of Physics & Astronomy; Sellers, Ian R. [Univ. of Oklahoma, Norman, OK (United States). Homer L. Dodge Dept. of Physics & Astronomy; Ming, Wenmei [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Materials Science & Technology Division; Du, Mao-Hua [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Materials Science & Technology Division; Saparov, Bayrammurad [Univ. of Oklahoma, Norman, OK (United States). Dept. of Chemistry and Biochemistry

    2017-11-22

    Here, we report synthesis, crystal and electronic structures, and optical properties of two new Hg-based zero-dimensional hybrid organic-inorganic halides (HIm)2Hg3Cl8 and (HIm)HgI3 (HIm = imidazolium). (HIm)2Hg3Cl8 crystallizes in the triclinic P-1 space group with a pseudo-layered structure made of organic imidazolium cation layers and anionic inorganic layers containing [Hg2Cl6]2- units and linear [HgCl2]0 molecules. (HIm)HgI3 crystallizes in the monoclinic P21/c space group featuring anionic [HgI3]- units that are surrounded by imidazolium cations. Based on density functional theory calculations, (HIm)2Hg3Cl8 has an indirect band gap, whereas (HIm)HgI3 has a direct band gap with the measured onsets of optical absorption at 3.43 and 2.63 eV, respectively. (HIm)2Hg3Cl8 and (HIm)HgI3 are broadband light emitters with broad photoluminescence peaks centered at 548 nm (2.26 eV) and 582 nm (2.13 eV), respectively. In conclusion, following the crystal and electronic structure considerations, the PL peaks are assigned to self-trapped excitons.

  19. Synthesis, crystal growth, thermal studies and scaled quantum chemical studies of structural and vibrational spectra of the highly efficient organic NLO crystal: 1-(4-Aminophenyl)-3-(3,4-dimethoxyphenyl)-prop-2-en-1-one

    Energy Technology Data Exchange (ETDEWEB)

    Joseph, Lynnette [Department of Physics, Bishop Moore College, Mavelikara, Alappuzha 690110, Kerala (India); Department of Physics, C.M.S College, Kottayam 686001, Kerala (India); Sajan, D., E-mail: dsajand@gmail.com [Department of Physics, Bishop Moore College, Mavelikara, Alappuzha 690110, Kerala (India); Shettigar, Venkataraya [Department of Physics, Gokhale Centenary College, Ankola 581 314, Karnataka (India); Chaitanya, K. [Key Laboratory of Soft Chemistry and Functional Materials of MOE, School of Chemical Engineering, Nanjing University of Science and Technology, Nanjing 210094 (China); Misra, Neeraj [Department of Physics, University of Lucknow, Lucknow 22607 (India); Sundius, Tom [Department of Physics, University of Helsinki, P.O. Box 64, FIN-00014 Helsinki (Finland); Němec, I. [Charles University in Prague, Faculty of Science, Department of Inorganic Chemistry, Hlavova 8, 128 40 Prague 2 (Czech Republic)

    2013-08-15

    A new chalcone derivative, 1-(4-aminophenyl)-3-(3,4-dimethoxyphenyl)-prop-2-en-1-one (DMAC) was synthesized and single crystals were grown by slow evaporation technique. The FT-Raman and FT-IR spectra of the sample were recorded in the region 3700–100 cm{sup −1} and 4000–400 cm{sup −1}, respectively. The spectra were interpreted with the aid of normal coordinate analysis following structure optimizations and force field calculations based on density functional theory (DFT) at the B3LYP/6-311+G(d,p) level of theory. Normal coordinate calculations were performed using the DFT force field, corrected by a recommended set of scaling factors, yielding fairly good agreement between the observed and calculated wavenumbers. DMAC is thermally stable up to 220.0 °C and optically transparent in the visible region. Information about the size, shape, charge density distribution and site of chemical reactivity of the molecule has been obtained by mapping electron density isosurface with electrostatic potential surfaces (ESP). The SHG efficiency of DMAC is observed to be 10 times that of standard urea crystal of identical particle size. - Highlights: • A chalcone derivative, DMAC has been synthesized and crystals are grown. • FT-IR and FT-Raman spectra, thermogravimetric and UV–Vis studies were carried out. • SHG effect from a centrosymmetric crystal has been reported.

  20. Synthesis, characterization and single crystal structures of chiral Schiff base and its tetranuclear palladium complex with Pdsbnd Osbnd Pd bridging and Pdsbnd Pd bonds

    Science.gov (United States)

    Rajegowda, H. R.; Kumar, P. Raghavendra; Hosamani, Amar; Butcher, R. J.; Naveen, S.; Lokanath, N. K.

    2018-03-01

    A new chiral Schiff base ligand 2-{N-[(2S)-(1-hydroxy-3-phenylpropan-2-yl]ethanimidoyl} phenol ((S)sbnd H2L) was obtained by acid catalyzed condensation of (2S)-(-)-2-amino-3-phenyl-1-propanol with 2‧-hydroxyacetophenone. The palladium complex was prepared by treating a solution of (S)sbnd H2L in acetone with a solution of Na2PdCl4 in water in 1:1 M ratio. The new ligand and its complex were characterized by FT-IR, 1H, 13C{1H} NMR spectroscopy, polarimetry and elemental analysis and their molecular structures were determined by single crystal X-ray diffraction. Both the compounds crystallizes in monoclinic system in the space group P21. There exists an intra [Osbnd H ⋯N (1.62(5) Å)] and intermolecular [Osbnd H ⋯O (1.53(5) Å) and Csbnd H ⋯O (2.59 Å)] hydrogen bonding and secondary interactions in the crystal of (S)sbnd H2L. The structure of the palladium complex was found very interesting wherein the ligand coordinated to metal center as tridentate dianionic (O-, N, O-) fashion, (S)-L, resulting in a tetranuclear palladium cluster, [Pd4((S)-L)4]. In these supramolecular structures phenolate oxygen coordinated to Pd(II) ion as Pdsbnd O terminal bonds [1.934(12) - 1.977(11) Å] and the alkoxide oxygen coordinated as Pdsbnd Osbnd Pd bridging bonds [1.993(11) - 2.012(12) Å]. The Pdsbnd N bond lengths found were in the range of 1.949(13) to 1.919(12) Å. There exists two asymmetric tetranuclear complex molecules in its crystal lattice. There exists very strong metal-metal bond interaction, Pd(2)sbnd Pd(3) [3.0410(18) Å] and Pd(6)sbnd Pd(7) [3.0517(19) Å] respectively in the two asymmetric units.

  1. 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.

  2. Distorted square-antiprism geometry of new zirconium (IV) Schiff base complexes: Synthesis, spectral characterization, crystal structure and investigation of biological properties

    Science.gov (United States)

    Sahraei, Atefeh; Kargar, Hadi; Hakimi, Mohammad; Tahir, Muhammad Nawaz

    2017-12-01

    A series of zirconium (IV) Schiff-base complexes formulated as [Zr (Lx)2] and [Zr (Lx‧)2] were synthesized by reaction of tetradentate salicylaldimine Schiff-base ligands with [Zr (acac)4] in methanol. These ligands are as follows: H2Lx and H2Lx‧ (x = x‧ = 1,2,3,4). The new complexes have been characterized using FT-IR, lH NMR, 13C{1H} NMR spectroscopic techniques, elemental analyses (CHN) and the crystal structure of Zr (L3)2, Zr (L1‧)2 and Zr (L3‧)2 were determined by X-ray crystallography. The crystal structure analysis revealed that the coordination environment of the metal in all complexes is eight-coordinate occupied by N2O2 sets of the coordinated ligands in distorted square-antiprism geometry. The in vitro biological screening effects of the synthesized compounds were tested against different microbial kinds and the zirconium (IV) complexes exhibit antimicrobial activity.

  3. Design, Synthesis, and X-ray Crystal Structures of 2,4-Diaminofuro[2,3-d]pyrimidines as Multireceptor Tyrosine Kinase and Dihydrofolate Reductase Inhibitors

    Science.gov (United States)

    Gangjee, Aleem; Li, Wei; Lin, Lu; Zeng, Yibin; Ihnat, Michael; Warnke, Linda A.; Green, Dixy W.; Cody, Vivian; Pace, Jim; Queener, Sherry F.

    2009-01-01

    To optimize dual receptor tyrosine kinase (RTK) and dihydrofolate reductase (DHFR) inhibition, the E- and Z-isomers of 5-[2-(2-methoxyphenyl)prop-1-en-1-yl]furo[2,3-d]pyrimidine-2,4-diamines (1a and 1b) were separated by HPLC and the X-ray crystal structures (2.0 Å and 1.4 Å respectively) with mouse DHFR and NADPH as well as 1b with human DHFR (1.5 Å) were determined. The E- and Z-isomers adopt different binding modes when bound to mouse DHFR. A series of 2,4-diaminofuro[2,3-d]pyrimidines 2–13 were designed and synthesized using the X-ray crystal structures of 1a and 1b with DHFR to increase their DHFR inhibitory activity. Wittig reactions of appropriate 2-methoxyphenyl ketones with 2,4-diamino-6-chloromethyl furo[2,3-d]pyrimidine afforded the C8–C9 unsaturated compounds 2–7 and catalytic reduction gave the saturated 8–13. Homologation of the C9-methyl analog maintains DHFR inhibitory activity. In addition, inhibition of EGFR and PDGFR-β were discovered for saturated C9-homologated analogs 9 and 10 that were absent in the saturated C9-methyl analogs. PMID:19748785

  4. Facile eco-friendly synthesis of 3,4,6,7-tetrahydro-3,3,6,6-tetramethyl-2H-xanthene 1,8(5H,9H)-dione, crystal structure and theoretical study

    Science.gov (United States)

    Tarannum, N.; Singh, M.

    2014-12-01

    New biologically active coumarin derivative, substituted xanthene-dione was synthesized by an easy, facile, cost-effective and efficient method from dimedone and diethylene glycol diacrylate without use of expensive and hazardous catalyst. The synthesis is simple, short, high-yielding and moreover does not require expensive solvents. The compound was characterized by IR, NMR and X-ray crystallography study. DFT (Density Functional Theory) calculations were performed at Becke's three-parameter functional and Lee-Yang-Parr functional (B3LYP) level of calculation and the 6-31G++ basis set was used for ground state geometry optimization. A comparison of the selected bond lengths and bond angles of the crystal structure and theoretically optimized structure by DFT have shown good agreement. The DFT study of electron surface potential (ESP), showed a large intramolecular charge transfer efficiency of the molecule indicating optical activity of xanthene dione.

  5. Two-dimensional layer architecture assembled by Keggin polyoxotungstate, Cu(II)-EDTA complex and sodium linker: Synthesis, crystal structures, and magnetic properties

    International Nuclear Information System (INIS)

    Liu Hong; Xu Lin; Gao Guanggang; Li Fengyan; Yang Yanyan; Li Zhikui; Sun Yu

    2007-01-01

    Reaction of Keggin polyoxotungstate with copper(II)-EDTA (EDTA=ethylenediamine tetraacetate) complex under mild conditions led to the formation of hybrid inorganic-organic compounds Na 4 (OH)[(Cu 2 EDTA)PW 12 O 40 ].17H 2 O (1) and Na 4 [(Cu 2 EDTA)SiW 12 O 40 ].19H 2 O (2). The single-crystal X-ray diffraction analyses reveal their two structural features: (1) one-dimensional chain structure consisting of Keggin polyoxotungstate and copper(II)-EDTA complex; (2) Two-dimensional layer architecture assembled by the one-dimensional chain structure and sodium linker. The results of magnetic measurements in the temperature range 300-2 K indicated the existence of ferromagnetic exchange interactions between the Cu II ions for both compounds. In addition, TGA analysis, IR spectra, and electrochemical properties were also investigated to well characterize these two compounds. - Graphical abstract: Two new polyoxometalate-based hybrids, Na 4 (OH)[Cu 2 (EDTA)PW 12 O 40 ].17H 2 O (1) and Na 4 [Cu 2 (EDTA)SiW 12 O 40 ].19H 2 O (2), have been synthesized and structurally characterized, which consist of one-dimensional chain structure assembled by Keggin polyoxotungstate and copper(II)-EDTA complex. The chains are further connected to form two-dimensional layer architecture assembled by the one-dimensional chain structure and sodium linker

  6. Tris dithiocarbamate of Co(III) complexes: Synthesis, characterization, thermal decomposition studies and experimental and theoretical studies on their crystal structures

    Science.gov (United States)

    Sonia, Ayyavoo Sait; Bhaskaran, Ramalingam

    2017-04-01

    New homoleptic complexes of the form [Co(L1)3] & [Co(L2)3] where L1 = (ethylaminoethanol dithiocarbamate) 1 and L2 = (methylaminoethanol dithiocarbamate) 2 have been prepared and characterized by elemental analysis, IR, UV-visible absorption spectra, Cyclic voltammetry,1H and C13 NMR. The thermal properties were studied using a simultaneous thermal analyzer, and showed two main steps of decomposition. In addition, structures for 1 and 2 have been elucidated by X-ray crystallography. The single-crystal X-ray analysis for both the complexes showed distorted octahedral geometry. The optimized molecular structure, natural bond orbital analysis, electrostatic potential map, HOMO-LUMO energies, molecular properties, and atomic charges of these molecules have been studied by performing DFT/B3LYP/6-31G(d,p) level of theory in gas phase.

  7. Heterobimetallic thiocyanato-bridged coordination polymers based on [Hg(SCN)4]2-: Synthesis, crystal structure, magnetic properties and ESR studies

    International Nuclear Information System (INIS)

    Jian Fangfang; Xiao Hailian; Liu Faqian

    2006-01-01

    Three new M/Hg bimetallic thiocyanato-bridged coordination polymers; [Hg(SCN) 4 Ni(Im) 3 ] ∞ 1, [Hg(SCN) 4 Mn(Im) 2 ] ∞ 2, and [Hg(SCN) 4 Cu(Me-Im) 2 Hg(SCN) 4 Cu(Me-Im) 4 ] ∞ 3, (Im=imidazole, Me-Im=N-methyl-imidazole), have been synthesized and characterized by means of elemental analysis, ESR, and single-crystal X-ray. X-ray diffraction analysis reveals that these three complexes all form 3D network structure, and their structures all contain a thiocyanato-bridged Hg...Hg chain (M=Mn, Ni, Cu) in which the metal and mercury centers exhibit different coordination environments. In complex 1, the [Hg(SCN) 4 ] 2- anion connects three [Ni(Im) 3 ] 2+ using three SCN ligands giving rise to a 3D structure, and in complex 2, four SCN ligands bridge [Hg(SCN) 4 ] 2- and [Mn(Im) 2 ] 2+ to form a 3D structure. The structure of 3 contains two copper atoms with distinct coordination environment; one is coordinated by four N-methyl-imidazole ligands and two axially elongated SCN groups, and another by four SCN groups (two elongated) and two N-methyl-imidazole ligands. The magnetic property of complex 1 has been investigated. The spin state structure in hetermetallic NiHgNi systems of complex 1 is irregular. The ESR spectra results of complex 3 demonstrate Cu 2+ ion lie on octahedral environment. -- Graphical abstract: Three new M/Hg bimetallic thiocyanato-bridged coordination polymers; [Hg(SCN) 4 Ni(Im) 3 ] ∞ 1, [Hg(SCN) 4 Mn(Im) 2 ] ∞ 2, and [Hg(SCN) 4 Cu(Me-Im) 2 Hg(SCN) 4 Cu(Me-Im) 4 ] ∞ 3, (Im=imidazole, Me-Im=N-methyl-imidazole), have been synthesized and characterized by single-crystal X-ray. All coordination polymers possess 3-D structures, and consist of organic base neutral ligands (imidazole and N-methyl-imidazole) and SCN -1 anions. Their structural difference is mainly caused by the role of the organic base and metal ions. The complex 1 shows the irregular spin state structure

  8. What makes a crystal structure report valid?

    NARCIS (Netherlands)

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

    2018-01-01

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

  9. Crystal structure analysis of intermetallic compounds

    Science.gov (United States)

    Conner, R. A., Jr.; Downey, J. W.; Dwight, A. E.

    1968-01-01

    Study concerns crystal structures and lattice parameters for a number of new intermetallic compounds. Crystal structure data have been collected on equiatomic compounds, formed between an element of the Sc, Ti, V, or Cr group and an element of the Co or Ni group. The data, obtained by conventional methods, are presented in an easily usable tabular form.

  10. Synthesis, crystal structures and thermodynamic properties of two novel lanthanide complexes based on 3,4-diethoxybenzoic acid and 2,2′-bipyridine

    International Nuclear Information System (INIS)

    Jin, Cheng-Wei; Wang, Ye; Ren, Ning; Geng, Li-Na; Zhang, Jian-Jun

    2016-01-01

    Highlights: • Two novel complexes crystal structures are obtained. • The 1-D chain and 2D layer structures were formed via π–π stacking interactions. • The pathway of thermal decomposition for title complexes were investigated. • The molar heat capacities and thermodynamic functions were calculated. - Abstract: Two binuclear lanthanide complexes [Ln(3,4,-DEOBA) 3 DIPY] 2 DIPY (Ln = Tb (1), Dy (2); 3,4,-DEOBA = 3,4-diethoxybenzoate; DIPY = 2,2′-bipyridine) have been synthesized and characterized. The single crystals of complexes 1 and 2 were obtained. And the two complexes are isostructural with a coordination number of eight to form a distorted square antiprism. Carboxylic groups adopt two modes coordinating with Ln(III) ions: bidentate chelate, and bridging bidentate. Binuclear complexes 1 and 2 are stitched together via π–π stacking interactions to form 1D chain and 2D layer supramolecular structures. The two complexes were characterized by elemental analysis, IR spectra, and powder X-ray diffraction. The luminescence spectra of complexes 1 and 2 show the characteristic emissions of Tb 3+ ( 5 D 4 → 7 F 6-3 ) and Dy 3+ ( 4 F 9/2 → 6 H 15/2 , 6 H 13/2 ). The thermal decomposition mechanisms for title complexes were studied by the technology of TG-FTIR. And the heat capacities of two complexes were measured by DSC in the temperature range from 258.15 to 343.15 K. The smoothed heat capacities and thermodynamic functions for complexes 1 and 2 were calculated by fitted polynomial and thermodynamic equations.

  11. Crystal chemistry of uranyl halides containing mixed(UO2)(XmOn)5 bipyramids (X = Cl,Br). Synthesis and crystal structure of Cs2(UO2)(NO3)Cl3

    International Nuclear Information System (INIS)

    Nazarchuk, Evgeny V.; Siidra, Oleg I.; Krivovichev, Sergey V.

    2011-01-01

    Single crystals of Cs 2 (UO 2 )(NO 3 )Cl 3 were prepared by a hydrothermal method at 205 C. The crystal structure has been solved by Direct Methods: monoclinic, P2 1 /n, a = 10.3748(13), b = 9.4683(13), c = 12.5535(16) A β, = 110.280(2) , V = 1156.7(3) A 3 , R 1 = 0.029. In the structure, strongly bonded linear uranyl cations UO 2 2+ are equatorially coordinated by two O and three Cl atoms to form (UO 2 )Cl 3 O 2 pentagonal bipyramids. Each bipyramid shares its O.O edge with an adjacent (NO 3 ) - anion to form finite clusters with the chemical composition [(UO 2 )(NO 3 )Cl 3 ] 2- . The Cs + cations provide three-dimensional connectivity of the structure by forming Cs-O and Cs-Cl contacts to the uranyl nitrate chloride complexes. Related structures of mixed-ligand uranyl halides are compared. (orig.)

  12. Hydrothermal synthesis of single crystals of transition metal vanadates in the glaserite phase

    Energy Technology Data Exchange (ETDEWEB)

    Sanjeewa, Liurukara D.; McMillen, Colin D.; Willett, Daniel; Chumanov, George; Kolis, Joseph W., E-mail: kjoseph@clemson.edu

    2016-04-15

    A series of transition metal vanadate crystals were prepared using a high temperature (580 °C) hydrothermal method. The compounds all had the general formula A{sub 2}AEM(VO{sub 4}){sub 2} (A=K, Na, Li; AE=Ba, Sr; M=Co, Fe, Mn). They are all variations of the glaserite structural type and range in symmetry from P-3m1 to P-3 to P2{sub 1}/c. Most of the derivatives contain a planar three-fold rotation operation, making them possible spin frustration candidates. Single crystal structural analyses were performed on many of the derivatives to obtain a detailed understanding of the distortions of the tetrahedral building blocks that accommodate the symmetry distortions. A hydrothermal growth method was developed to grow high quality single crystals of sizes up to 2–3 mm/edge. This method can be generalized for large crystal growth to enable magnetic and neutron diffraction studies that require relatively large single crystals. - Highlights: • The hydrothermal synthesis of glaserite-type vanadates is demonstrated. • Synthesis from stoichiometric component reactions yields 0.2–0.5 mm size crystals. • Hydrothermal recrystallization of glaserite powder yields 2–3 mm size crystals. • The structure varies according to the alkali and alkaline earth metals selected. • Ideal (P-3m1) and distorted (P-3 and P2{sub 1}/c) glaserite structures are observed.

  13. Synthesis and crystal structure of Cd-based metal-organic framework for removal of methyl-orange from aqueous solution

    Science.gov (United States)

    Tella, Adedibu C.; Olawale, Margaret D.; Neuburger, Markus; Obaleye, Joshua A.

    2017-11-01

    A novel [Cd(INA)2(H2O)]. ISB (1) (INA = isonicotinate; ISB = isobutanol) was synthesized through the reaction between the isonicotinic acid ligand and cadmium (II) salt and characterized by elemental analysis, FTIR and UV-Visible spectroscopies, SEM and Single crystal X-ray diffraction. The crystal is orthorhombic, space group Pbca, a = 12.24(10) Å, b = 15.4646(13) Å, c = 18.8445(17) Å, V = 3569(3) Å3, Z = 8. The pentagonal bipyramid (seven coordinate) around the cadmium (II) ion is of the form CdN2O5 coordinating to four oxygen atoms from carboxylates, one oxygen atom from water molecule and two nitrogen atoms of pyridine. The structure of compound is stabilized by two hydrogen bonds namely intermolecular (O-H-O) and intramolecular type C-H-O accounting for polymeric nature of the metal-organic frameworks. 1 was studied for adsorptive removal of methyl orange (MO) from aqueous solution. Equilibrium isotherm study reveals that Langmuir model gave a better fitting result than the Freundlich model. The pseudo-second order model could be used to interpret adsorption kinetics. The maximum adsorption capacity calculated by Langmuir was 166 mg/g at 300 K. These results indicate the adsorption of MO on 1 is partly due to electrostatic interaction between methyl orange and the adsorbent. 1 could be used as adsorbent to remove methyl orange from aqueous solution.

  14. A new tridentate Schiff base Cu(II) complex: synthesis, experimental and theoretical studies on its crystal structure, FT-IR and UV-Visible spectra.

    Science.gov (United States)

    Saheb, Vahid; Sheikhshoaie, Iran; Setoodeh, Nasim; Rudbari, Hadi Amiri; Bruno, Giuseppe

    2013-06-01

    A new Cu(II) complex [Cu(L)(NCS)] has been synthesized, using 1-(N-salicylideneimino)-2-(N,N-methyl)-aminoethane as tridentate ONN donor Schiff base ligand (HL). The dark green crystals of the compound are used for single-crystal X-ray analysis and measuring Fourier Transform Infrared (FT-IR) and UV-Visible spectra. Electronic structure calculations at the B3LYP and MP2 levels of theory are performed to optimize the molecular geometry and to calculate the UV-Visible and FT-IR spectra of the compound. Vibrational assignments and analysis of the fundamental modes of the compound are performed. Time-dependent density functional theory (TD-DFT) method is used to calculate the electronic transitions of the complex. A scaling factor of 1.015 is obtained for vibrational frequencies computed at the B3LYP level using basis sets 6-311G(d,p). It is found that solvent has a profound effect on the electronic absorption spectrum. The UV-Visible spectrum of the complex recorded in DMSO and DMF solution can be correctly predicted by a model in which DMSO and DMF molecules are coordinated to the central Cu atom via their oxygen atoms. Copyright © 2013 Elsevier B.V. All rights reserved.

  15. Synthesis, crystal structures, and thermal and spectroscopic properties of two Cd(II) metal-organic frameworks with a versatile ligand

    Energy Technology Data Exchange (ETDEWEB)

    Li, Jia-Ming; He, Kun-Huan; Shi, Zhong-Feng [Qinzhou Univ. (China). Guangxi Colleges and Univs. Key Lab. of Beibu Gulf Oil and Natural Gas Resource Effective Utilization; Gao, Hui-Yuan; Jiang, Yi-Min [Guangxi Normal Univ., Guilin (China). Key Lab. for the Chemistry and Molecular Engineering of Medicinal Resources

    2016-11-01

    Two new metal-organic frameworks, namely, [Cd(L)(H{sub 2}O)]{sub n} (1) and {[Cd_0_._5(L)(4,4"'-bipy)_0_._5][Cd_0_._5(H_2O)(4,4"'-bipy)_0_._5].H_2O}{sub n} (2), where H{sub 2}L = N-pyrazinesulfonyl-glycine and 4,4{sup '}-bipy = 4,4{sup '}-bipyridine, have been synthesized and characterized by single-crystal X-ray diffraction, IR spectroscopy, elemental, thermogravimetric, and photoluminescent analysis. X-ray diffraction crystallographic analyses indicate that 1 displays a distorted octahedral metal coordination in a 3-connected (4, 8{sup 2}) topology, while the molecular structure of 2 has a 4-connected (4, 4) topology with two perfectly octahedrally coordinated Cd centers. The L{sup 2-} ligand serves as a N,N,O-tridentate, μ{sub 2}-pyrazine-bridging, and μ{sub 2}-carboxylate-bridging ligand in 1, and as a N,O-bidentate and μ{sub 2}-carboxylate-bridging ligand in 2. In the crystal, a 3D supramolecular architecture is formed by O-H..O hydrogen bond interactions in 1, but through O-H..O as well as π..π stacking in 2. The two compounds show intense fluorescence in the solid state at room temperature.

  16. Synthesis, crystal structure and thermal decomposition mechanism of the complex [Sm(p-BrBA)3bipy.H2O]2.H2O

    International Nuclear Information System (INIS)

    Zhang Haiyan; Zhang Jianjun; Ren Ning; Xu Suling; Tian Liang; Bai Jihai

    2008-01-01

    A new binuclear samarium (III) complex [Sm(p-BrBA) 3 bipy.H 2 O] 2 .H 2 O (p-BrBA = p-bromobenzoic acid; bipy = 2,2'-bipyridine) has been synthesized and characterized by elemental analysis, UV, IR, molar conductance and TG-DTG techniques. The structure of the complex was established by single crystal X-ray diffraction. It crystallizes in triclinic, space group P1-bar with a = 8.2476(7) A, b = 13.3483(10) A, c = 15.9035(13) A, α 73.9160(10) o , β = 78.9630(10) o , γ = 74.4770(10) o , Z = 1, D c 1.947 g cm -3 , F(000) = 910. The carboxylic groups are bonded to the samarium ion in two modes: bidentate bridging, monodentate. Each center Sm 3+ ion is eight-coordinated by one 2,2'-bipyridine molecular, four bidentate bridging and a monodentate carboxylic group, as well as one water molecular. The coordination polyhedron around each Sm 3+ ion can be described as bi-capped triangular prism geometry. The thermal decomposition behavior of the title complex in a static air atmosphere was investigated by TG-DTG and IR techniques

  17. Synthesis, Characterization, and X-Ray Crystal Structure of Bis(O-amyl dithiocarbonato-κ2S,S′bis(4-cyanopyridine-κNnickel(II

    Directory of Open Access Journals (Sweden)

    Kuldeep Singh

    2014-01-01

    Full Text Available The [Ni(S2CO-n-C5H112(C6H4N22] adduct of 4-cyanopyridine with [Ni(S2CO-n-C5H112] was synthesized and characterized by elemental analysis, magnetic susceptibility measurement, IR, electronic spectral data, and X-ray diffraction analysis. The Ni atom in the title complex is octahedrally coordinated within a trans-N2S4 donor set, with the Ni atom located on a centre of inversion. The title compound exhibits magnetic moment value (3.20 B.M which is in agreement with magnetic moment values observed for paramagnetic octahedral complexes of nickel(II. The title complex crystallizes in the orthorhombic space group Pbca with unit cell parameters a = 11.455(5, b = 9.602(4, and c = 26.374(1 Å. Crystal structure was solved by direct methods and refined by full matrix least-squares procedures to a final R value of 0.0499 for 2004 observed reflections. The amyl chain is disordered over two sets of sites, with occupancy ratios of 0.595 : 0.405. Infinite long chains of molecules are formed with the help of C–H⋯N hydrogen bond.

  18. Synthesis, Crystal Structure, Absolute Configuration and Antitumor Activity of the Enantiomers of 5-Bromo-2-chloro-N-(1-phenylethylpyridine-3-sulfonamide

    Directory of Open Access Journals (Sweden)

    Zhixu Zhou

    2015-11-01

    Full Text Available Pyridinesulfonamide is an important fragment which has a wide range of applications in novel drugs. R- and S-isomers of 5-bromo-2-chloro-N-(1-phenylethylpyridine-3-sulfonamide have been synthesized, and the stereostructures have been researched. Single crystals of both compounds were obtained for X-ray analysis, and the absolute configurations (ACs have been further confirmed by electronic circular dichroism (ECD, optical rotation (OR and quantum chemical calculations. The crystal structures and calculated geometries were extremely similar, which permitted a comparison of the relative reliabilities of ACs obtained by ECD analyses and theoretical simulation. In addition, the effect of stereochemistry on the PI3Kα kinase and anticancer activity were investigated. Compounds 10a and 10b inhibit the activity of PI3Kα kinase with IC50 values of 1.08 and 2.69 μM, respectively. Furthermore, molecular docking was performed to analyze the binding modes of R- and S-isomers.

  19. Crystal structure of prethrombin-1

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-11-15

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

  20. Synthesis, crystal structure and thermal properties of Ca6(C12H14O4)4(CO3)(OH)2(H2O)x – a 3D inorganic hybrid material

    DEFF Research Database (Denmark)

    Nielsen, Renie Birkedal; Norby, Poul; Kongshaug, Kjell Ove

    2012-01-01

    The inorganic–organic compound Ca6(1,3-adamantanedicarboxylate)4(CO3)(OH)2(H2O)x with 0 crystal structure was determined on the basis of high resolution synchrotron powder diffraction data and poly-crystal measurements. The crystal structure o...

  1. PCR-based gene synthesis to produce recombinant proteins for crystallization

    Directory of Open Access Journals (Sweden)

    Byrne-Steele Miranda L

    2008-04-01

    Full Text Available Abstract Background Gene synthesis technologies are an important tool for structural biology projects, allowing increased protein expression through codon optimization and facilitating sequence alterations. Existing methods, however, can be complex and not always reproducible, prompting researchers to use commercial suppliers rather than synthesize genes themselves. Results A PCR-based gene synthesis method, referred to as SeqTBIO, is described to efficiently assemble the coding regions of two novel hyperthermophilic proteins, PAZ (Piwi/Argonaute/Zwille domain, a siRNA-binding domain of an Argonaute protein homologue and a deletion mutant of a family A DNA polymerase (PolA. The gene synthesis procedure is based on sequential assembly such that homogeneous DNA products can be obtained after each synthesis step without extensive manipulation or purification requirements. Coupling the gene synthesis procedure to in vivo homologous recombination techniques allows efficient subcloning and site-directed mutagenesis for error correction. The recombinant proteins of PAZ and PolA were subsequently overexpressed in E. coli and used for protein crystallization. Crystals of both proteins were obtained and they were suitable for X-ray analysis. Conclusion We demonstrate, by using PAZ and PolA as examples, the feasibility of integrating the gene synthesis, error correction and subcloning techniques into a non-automated gene to crystal pipeline such that genes can be designed, synthesized and implemented for recombinant expression and protein crystallization.

  2. Crystal structure resolution by X-rays

    International Nuclear Information System (INIS)

    Jeannin, Y.

    1998-01-01

    This paper deals with the crystal structure analysis by X-rays. It details the different steps of the crystal structure resolution, the measured parameters and the possible errors with appropriate corrections. The presentation includes the x-rays intensity measurement, the structure factor calculus, the Patterson method, the direct methods, the structure analysis, the parameters refinement by least square fit, the temperature factors, disorder and twinning, the primary and secondary extinctions and a absolute configuration determination. (A.L.B.)

  3. Second-sphere coordination complex via hydrogen bonding: Synthesis, characterization, X-ray crystal structure determination and packing of hexaamminecobalt(III) chloride di( para-nitrobenzoate)

    Science.gov (United States)

    Sharma, Raj Pal; Bala, Ritu; Sharma, Rajni; Perez, Julio; Miguel, Daniel

    2006-09-01

    A reddish orange coloured crystalline solid of hexaamminecobalt(III) chloride di( para-nitrobenzoate) was obtained when hexaamminecobalt(III) chloride was reacted with the sodium salt of para-nitrobenzoic acid (1:3 molar ratio) in hot aqueous medium. This cobalt(III) complex salt has been characterized by elemental analyses and spectroscopic techniques (e.g. UV/visible, IR and NMR). Single-crystal X-ray structure determination of the title complex salt revealed that it contains the cationic cobaltammine ([Co(NH 3) 6] 3+) and mixed anions (Cl -, NO 2C 6H 4COO -), which are held together by electrostatic forces attractions through second-sphere coordination, i.e. N-H⋯O (carboxylate and nitro) and N-H⋯Cl hydrogen bonds, resulting in a three-dimensional network.

  4. Synthesis, crystal structure and properties of K2Ta2S10: A novel ternary tantalum polysulfide with TaS8 polyhedra forming infinite anionic chains

    International Nuclear Information System (INIS)

    Wu Yuandong; Naether, Christian; Bensch, Wolfgang

    2005-01-01

    The new ternary alkali tantalum polysulfide K 2 Ta 2 S 10 has been synthesized by reacting TaS 2 with an in situ formed melt of K 2 S 3 and S at 773K. The compound crystallizes with four formula units in the monoclinic space group P2 1 /n (No. 14) with lattice parameters of a=14.9989(13)A,b=6.4183(4)A,c=15.1365(13)A,β=117.629(9) o . The structure contains two different zigzag chain anions [TaS 5 ] - , running parallel to the crystallographic b-axis separated by potassium cations. The two crystallographically independent tantalum atoms are in a distorted bi-capped trigonal prismatic environment of eight sulfur atoms which was never observed before. The TaS 8 polyhedra share three S atoms on each side to form the anionic chains. The compound was characterized with FIR and Raman spectroscopy

  5. The new barium zinc mercurides Ba3ZnHg10 and BaZn0.6Hg3.4 – Synthesis, crystal and electronic structure

    International Nuclear Information System (INIS)

    Schwarz, Michael; Wendorff, Marco; Röhr, Caroline

    2012-01-01

    The title compounds Ba 3 ZnHg 10 and BaZn 0.6 Hg 3.4 were synthesized from stoichiometric ratios of the elements in Ta crucibles. Their crystal structures, which both represent new structure types, have been determined using single crystal X-ray data. The structure of Ba 3 ZnHg 10 (orthorhombic, oP28, space group Pmmn, a=701.2(3), b=1706.9(8), c=627.3(3)pm, Z=2, R1=0.0657) contains folded 4 4 Hg nets, where the meshes form the bases of flat rectangular pyramids resembling the structure of BaAl 4 . The flat pyramids are connected via Hg–Zn/Hg bonds, leaving large channels at the folds, in which Ba(1) and Hg(2) atoms alternate. Whereas the remaining Hg/Zn atoms form a covalent 3D network of three- to five-bonded atoms with short M–M distances (273–301 pm; CN 9–11), the Hg(2) atoms in the channels adopt a comparatively large coordination number of 12 and increased distances (317–348 pm) to their Zn/Hg neighbours. In the structure of BaZn 0.6 Hg 3.4 (cubic, cI320, space group I4 ¯ 3d, a=2025.50(7) pm, Z=64, R1=0.0440), with a chemical composition not much different from that of Ba 3 ZnHg 10 , the Zn/Hg atoms of the mixed positions M(1/2) are arranged in an slightly distorted primitive cubic lattice with a 4×4×4 subcell relation to the unit cell. The 24 of the originating 64 cubes contain planar cis tetramers Hg(5,6) 4 with Hg in a nearly trigonal planar or tetrahedral coordination. In another 24 of the small cubes, two opposing faces are decorated by Hg(3,4) 2 dumbbells, two by Ba(2) atoms respectively. The third type of small cubes are centered by Ba(1) atoms only. The complex 3D polyanionic Hg/Zn network thus formed is compared with the Hg partial structure in Rb 3 Hg 20 applying a group-subgroup relation. Despite their different overall structures, the connectivity of the negatively charged Hg atoms, the rather metallic Zn bonding characteristic (as obtained from FP-LAPW band structure calculations) and the coordination number of 16 for all Ba cations

  6. Method of fabricating patterned crystal structures

    KAUST Repository

    Yu, Liyang

    2016-12-15

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

  7. Crystal structure 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. 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.

  9. Synthesis, Characterization, Crystal Structure and Antimicrobial Activity of Copper(II Complexes with the Schiff Base Derived from 2-Hydroxy-4-Methoxybenzaldehyde

    Directory of Open Access Journals (Sweden)

    Elena Pahonțu

    2015-04-01

    Full Text Available A novel Schiff base, ethyl 4-[(E-(2-hydroxy-4-methoxyphenylmethylene-amino]benzoate (HL, was prepared and structurally characterized on the basis of elemental analyses, 1H NMR, 13C NMR, UV-Vis and IR spectral data. Six new copper(II complexes, [Cu(L(NO3(H2O2] (1, [Cu(L2] (2, [Cu(L(OAc] (3, [Cu2 (L2Cl2(H2O4] (4, [Cu(L(ClO4(H2O] (5 and [Cu2(L2S(ClO4(H2O]ClO4·H2O (6 have been synthesized. The characterization of the newly formed compounds was done by IR, UV-Vis, EPR, FAB mass spectroscopy, elemental and thermal analysis, magnetic susceptibility measurements and molar electric conductivity. The crystal structures of Schiff base and the complex [Cu2(L2S(ClO4(H2O]ClO4·H2O (6 have been determined by single crystal X-ray diffraction studies. Both copper atoms display a distorted octahedral coordination type [O4NS]. This coordination is ensured by three phenol oxygen, two of which being related to the µ-oxo-bridge, the nitrogen atoms of the azomethine group and the sulfur atoms that come from the polydentate ligand. The in vitro antimicrobial activity against Escherichia coli ATCC 25922, Salmonella enteritidis, Staphylococcus aureus ATCC 25923, Enterococcus and Candida albicans strains was studied and compared with that of free ligand. The complexes 1, 2, 5 showed a better antimicrobial activity than the Schiff base against the tested microorganisms.

  10. Coligand-directed synthesis of five Co(II)/Ni(II) coordination polymers with a neutral tetradentate ligand: syntheses, crystal structures, and properties.

    Science.gov (United States)

    Qin, Ling; Wang, Zhong-Jie; Wang, Ting; Zheng, He-Gen; Chen, Jin-Xi

    2014-09-07

    The solvothermal reactions of 1,1'-oxybis[3,5-di-4-pyridine]-benzene (L) and transition metal cations (Co and Ni) afford five novel coordination polymers in the presence of flexible bridging ligands (4,4'-H2nba = 4,4'-dicarboxydiphenylamine, H2cam = d-camphoric acid, 4,4'-H2sdb = 4,4'-sulfonyldibenzoic acid, H2chdc = 1,4-trans-cyclohexanedicarboxylic acid), namely {[Co2L2(OH)2(nba)]·2DMF}n (), {[CoL(cam)(H2O)]}n (), {[Co3(L)(4,4'-sdb)3(H2O)]·1.5CH3CN·4H2O}n (), {[Ni3(L)(4,4'-sdb)3(H2O)]·1.5CH3CN·4H2O}n (), and {[Ni2L2(chdc)2(H2O)2]·(H2O)3}n () (DMF = N,N-dimethylformamide). Their structures have been determined by single-crystal X-ray diffraction analyses and further characterized by elemental analyses, IR spectroscopy, and powder X-ray diffraction. Complex reveals a 2-fold interpenetrating three-dimensional (3D) framework with the Schläfli symbol {4·8·10(4)}{4·8·10} topology. Compound crystallizes in the achiral space group with the d-camphorate ligand racemized. Compounds and reveal similar structure with the {3·4(4)·6}{3(2)·4(8)·5(9)·6(9)} topology based on a linear trinuclear building block M3(OOCR)6 (M = Co(ii) or Ni(ii)). Compound is a wavy sheet, where both carboxylate and L ligands act as bidentate ligands. Moreover, UV-Visible absorption spectra of complexes , and the magnetic properties of have been investigated.

  11. Synthesis of 5-hydroxyectoine from ectoine: crystal structure of the non-heme iron(II and 2-oxoglutarate-dependent dioxygenase EctD.

    Directory of Open Access Journals (Sweden)

    Klaus Reuter

    2010-05-01

    Full Text Available As a response to high osmolality, many microorganisms synthesize various types of compatible solutes. These organic osmolytes aid in offsetting the detrimental effects of low water activity on cell physiology. One of these compatible solutes is ectoine. A sub-group of the ectoine producer's enzymatically convert this tetrahydropyrimidine into a hydroxylated derivative, 5-hydroxyectoine. This compound also functions as an effective osmostress protectant and compatible solute but it possesses properties that differ in several aspects from those of ectoine. The enzyme responsible for ectoine hydroxylation (EctD is a member of the non-heme iron(II-containing and 2-oxoglutarate-dependent dioxygenases (EC 1.14.11. These enzymes couple the decarboxylation of 2-oxoglutarate with the formation of a high-energy ferryl-oxo intermediate to catalyze the oxidation of the bound organic substrate. We report here the crystal structure of the ectoine hydroxylase EctD from the moderate halophile Virgibacillus salexigens in complex with Fe(3+ at a resolution of 1.85 A. Like other non-heme iron(II and 2-oxoglutarate dependent dioxygenases, the core of the EctD structure consists of a double-stranded beta-helix forming the main portion of the active-site of the enzyme. The positioning of the iron ligand in the active-site of EctD is mediated by an evolutionarily conserved 2-His-1-carboxylate iron-binding motif. The side chains of the three residues forming this iron-binding site protrude into a deep cavity in the EctD structure that also harbours the 2-oxoglutarate co-substrate-binding site. Database searches revealed a widespread occurrence of EctD-type proteins in members of the Bacteria but only in a single representative of the Archaea, the marine crenarchaeon Nitrosopumilus maritimus. The EctD crystal structure reported here can serve as a template to guide further biochemical and structural studies of this biotechnologically interesting enzyme family.

  12. Dependence of Crystal Quality and β Value on Synthesis Temperature in Growing Gem Diamond Crystals

    International Nuclear Information System (INIS)

    Hong-Yu, Xiao; Xiao-Peng, Jia; Shang-Sheng, Li; Yu, Tian; Ya-Fei, Zhang; Guo-Feng, Huang; Li-Qiu; Hong-An, Ma; Chuan-Yi, Zang

    2008-01-01

    High quality Ib gem diamond single crystals were synthesized in cubic anvil high-pressure apparatus (SPD-6 × 1200) under 5.4 GPa and 1230°C-1280°C. The (100) face of seed crystal was used as growth face, and Ni 70 Mn 25 Co 5 alloy was used as solvent/catalyst. The dependence of crystal quality and β value (the ratio of height to diameter of diamond crystal) on synthesis temperature was studied. When the synthesis temperature is between 1230°C and 1280°C, the β value of the synthetic high-quality gem diamond crystals is between 0.4 and 0.6. The results show that when the β value is between 0.4 and 0.45, the synthetic diamonds are sheet-shape crystals; however, when the β value is between 0.45 and 0.6, the synthetic diamonds are tower-shape crystals. In addition, when the β value is less than 0.4, skeleton crystals will appear. When the β value is more than 0.6, most of the synthetic diamond crystals are inferior crystals

  13. 2-((E)-(6-fluorobenzo[d]thiazol-2-ylimino) methyl)-4-chlorophenol; synthesis, characterization, crystal structure, Hirshfeld surface analysis and BSA binding studies

    Science.gov (United States)

    Kumar, Savithri; Basappa Chidananda, Vasantha Kumar; Hosakere Doddarevanna, Revanasiddappa; Hamse Kameshwar, Vivek; Kaur, Manpreet; Jasinski, Jerry P.

    2017-08-01

    A new imine-based molecule 2-((E)-(6-fluorobenzo[d]thiazol-2-ylimino) methyl)-4-chlorophenol (FBt) was synthesized by microwave and conventional method. It was structurally characterized by spectral techniques (NMR, FT-IR, LC-MS and electronic absorption), elemental analysis and single-crystal X-ray diffraction methods. Hirshfeld surface analysis was employed to ensure the existence of intermolecular interactions in FBt structure. A preliminary in vitro susceptibility test against two pathogenic fungi with respect to standard has shown that the ligand is proved to be a potent antifungal agent. Since the carrying of a drug by BSA may effect on its structure and action, the investigation on the interaction between model protein BSA and FBt was carried out by employing UV-Vis and fluorescence spectroscopy. The characteristics of the binding, i.e., binding constant, number of binding sites, and nature of binding were determined. Besides, the Förster's parameters associated with the binding process were calculated. Molecular docking was also carried on interaction study of the FBt with BSA.

  14. Synthesis, crystal structures, and properties of two novel cadmium(II)-organic frameworks based on asymmetric dicarboxylate and N-donor ligands

    Science.gov (United States)

    Chen, Xiaoli; Gao, Loujun; Zhang, Xiaoge; Han, Xuhua; Wang, Yao; Sun, Rong

    2014-08-01

    Two novel cadmium(II)-organic frameworks with asymmetric dicarboxylate and N-donor ligands, namely [Cd(cpa)(phen)]n (1) and {[Cd2(cpa)2(bpy)1.5]·0.5H2O}n (2) (H2cpa = 3-(4-benzoic)propionic acid, phen = 1,10-phenanthroline, bpy = 4,4";-bipyridine) have been hydrothermally synthesized and characterized by elemental analyses, FT-IR spectra, single-crystal X-ray diffraction analyses, TGA, powder XRD and fluorescent measurements. 1 displays a double zigzag chain structure containing 8-number and 22-number circles. 2 Shows a 6-connected 3D polymer network based on tetranuclear cadmium cluster units. The most striking feature of 2 is that a pair of identical 3D networks are interlocked with each other to the form a 2-fold interpenetrated 3D α-Po structural topology. The diverse structures of two complexes indicate that the skeleton of N-donor ligands plays a great role in the assembly of such different frameworks. In addition, the thermal stabilities, XRD and photoluminescence properties of 1-2 were also studied.

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

    International Nuclear Information System (INIS)

    Saeednia, S.; Iranmanesh, P.; Ardakani, M. Hatefi; Mohammadi, M.; Norouzi, Gh.

    2016-01-01

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

  16. 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.

  17. Synthesis and crystal structure of copper (II) uracil ternary polymeric complex with 1,10-phenanthroline along with the Hirshfeld surface analysis of the metal binding sites for the uracil ligand

    Science.gov (United States)

    Patil, Yogesh Prakash; Nethaji, Munirathinam

    2015-02-01

    The study of models for "metal-enzyme-substrate" interaction has been a proactive area of research owing to its biological and pharmacological importance. In this regard the ternary copper uracil complex with 1,10-phenanthroline represents metal-enzyme-substrate system for DNA binding enzymes. The synthesis of the complex, followed by slow evaporation of the reaction mixture forms two concomitant solvatomorph crystals viz., {[Cu(phen)(μ-ura)(H2O)]n·H2O (1a)} and {[Cu(phen)(μ-ura)(H2O)]n·CH3OH (1b)}. Both complexes are structurally characterized, while elemental analysis, IR and EPR spectra were recorded for 1b (major product). In both complexes, uracil coordinates uniquely via N1 and N3 nitrogen atom acting as a bidentate bridging ligand forming a 1-D polymer. The two solvatomorphs were quantitatively analyzed for the differences with the aid of Hirshfeld surface analysis.

  18. Synthesis, structural, optical and thermal properties of N-methyl-N-aryl benzamide organic single crystals grown by a slow evaporation technique

    Science.gov (United States)

    Prabukanthan, P.; Lakshmi, R.; Harichandran, G.; Kumar, C. Sudarsana

    2018-03-01

    The organic materials, N-methyl-N-aryl benzamides were synthesized from benzoylation of N-methyl-4-nitrobenzenamine (MNBA) using suitably substituted benzoyl chlorides. The products were purified by recrystallization and their single crystal were grown by a slow evaporation technique. The crystals were characterized by FTIR, UV-Vis-NIR, 1H &13C NMR, and single & powder X-ray diffraction. Thermal stability of the crystals was studied by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). Dielectric and NLO properties of MNPB, FMNPB and MMNPB crystals were studied. The second harmonic generation (SHG) has been confirmed by the Kurtz powder test for all these crystals and the SHG efficiency of MMNPB crystal was found to be 2.25 times higher than that of KDP crystal.

  19. Synthesis, crystal structure analysis, spectral investigations, DFT computations and molecular dynamics and docking study of 4-benzyl-5-oxomorpholine-3-carbamide, a potential bioactive agent

    Science.gov (United States)

    Murthy, P. Krishna; Sheena Mary, Y.; Shyma Mary, Y.; Panicker, C. Yohannan; Suneetha, V.; Armaković, Stevan; Armaković, Sanja J.; Van Alsenoy, C.; Suchetan, P. A.

    2017-04-01

    4-benzyl-5-oxomorpholine-3-carbamide has been synthesized; single crystals were grown by slow evaporation solution growth technique at room temperature and characterized by single crystal X-ray diffraction, FT-IR, FT-Raman and 1H-NMR. The compound crystallizes in the monoclinic space group P21/n. The molecular geometry of the compound was optimized by using Density Functional Theory (DFT/B3LYP) method with 6-311++G(d,p) basis set in the ground state and geometric parameters are in agreement with the X-ray analysis results of the structure. The experimental vibrational spectra were compared with the calculated spectra and each vibrational wave number was assigned on the basis of potential energy distribution (PED). The electronic and charge transfer properties have been explained on the basis of highest occupied molecular orbital's (HOMOs) and lowest unoccupied molecular orbital's (LUMOs). Besides molecular electrostatic potential (MEP), frontier molecular orbital's (FMOs), some global reactivity descriptors, thermodynamic properties, non-linear optical (NLO) behavior and Mullikan charge analysis of the title compound were computed with the same method in gas phase, theoretically. Potential reactive sites of the title compound have been identified by average local ionization energy and Fukui functions, both mapped to the electron density surface. Bond dissociation energies for all single acyclic bonds have been calculated in order to investigate autoxidation and degradation properties of the title compound. Atoms with pronounced interactions with water molecules have been detected by calculations of radial distribution functions after molecular dynamics simulations. The experimental results are compared with the theoretical calculations using DFT methods for the fortification of the paper. Further the docking studies revealed that the title compound as a docked ligand forms a stable complex with pyrrole inhibitor with a binding affinity value of -7.5 kcal/mol. This

  20. Synthesis, crystal structure, thermal and luminescence properties of CuX(2,3-dimethylpyrazine) (X=Cl, Br, I) coordination polymers.

    Science.gov (United States)

    Jess, Inke; Taborsky, Petr; Pospísil, Jirí; Näther, Christian

    2007-06-14

    Three new coordination polymers based on CuI and 2,3-dimethylpyrazine (2,3-dmpyz) were prepared, structurally characterized and investigated for their thermal and luminescence properties. In the ligand rich 2:3 compound [(CuI)2(2,3-dmpyz)3] (CuI)2 dimers are found, which are connected by the N-donor ligands into chains, whereas in the structure of the 1:1 intermediate [(CuI)(2,3-dmpyz)] (CuI)4 tetramers are found, which are also connected into chains. The crystal structure of the ligand deficient 2:1 compound [(CuI)2(2,3-dmpyz)] is built up of CuI double chains, which are connected by the 2,3-dmpyz ligands into layers. Thermal decomposition of results in its direct transformation into the ligand deficient compound , without the formation of the 1:1 compound as an intermediate. A similar thermal reactivity is found for compound , which transforms into on heating. Stirring of a crystalline suspension of pure or in acetonitrile, always leads to a transformation into the ligand deficient compound indicating that compound is the most stable of all the coordination polymers, whereas compounds and are metastable. The luminescence properties of the CuCl and CuI coordination polymers were investigated at 298 and 77K. It was observed that the emission maxima strongly depends on the nature of the halide atom and the composition and structure of the coordination polymers. In addition, several of these compounds show luminescence thermochromism. These results are compared with those obtained for the previously reported CuCl and CuBr(2,3-dimethylpyrazine) coordination polymers.

  1. Mild hydrothermal synthesis, crystal structure, thermal behaviour, spectroscopic and magnetic properties of (NH4)0.80Li0.20[Fe(AsO4)F

    International Nuclear Information System (INIS)

    Berrocal, Teresa; Mesa, Jose L.; Larrea, Edurne S.; Bazan, Begona; Pizarro, Jose L.; Lezama, Luis; Rojo, Teofilo; Arriortua, Maria I.

    2011-01-01

    The (NH 4 ) 0.80 Li 0.20 [Fe(AsO 4 )F] compound has been synthesized under mild hydrothermal conditions. The compound crystallize in the orthorhombic Pna2 1 space group, with cell parameters a=13.352(9), b=6.7049(9), c=10.943(2) A and Z=8. The compound belongs to the KTiO(PO 4 ) structure type, with chains alternating FeO 4 F 2 octahedra and AsO 4 tetrahedra, respectively, running along the 'a' and 'b' crystallographic axes. The diffuse reflectance spectrum in the visible region shows the forbidden electronic transitions characteristic of the Fe(III) d 5 -high spin cation in slightly distorted octahedral geometry. The Moessbauer spectrum at room temperature is characteristic of iron (III) cations. The ESR spectra, carried out from room temperature to 200 K, remain isotropic with variation in temperature; the g-value being 1.99(1). Magnetic measurements indicate the predominance of strong antiferromagnetic interactions. - Graphical Abstract: Three-dimensional structure of (NH 4 ) 0.80 Li 0.20 [Fe(AsO 4 )F], a fluoroarsenate containing lithium and ammonium in the structural cavities. Highlights: → (NH 4 ) 0.80 Li 0.20 [Fe(AsO 4 )F] has been synthesized by mild hydrothermal technique. → The compound exhibits a three-dimensional structure. → Moessbauer spectrum indicates the existence of Fe(III) cations. → Visible spectroscopy confirms the hexacoordination of Fe(III). → Magnetic measurements indicate the existence of a global antiferromagnetic ordering.

  2. SYNTHESIS AND CRYSTAL STRUCTURE OF A NA(I COMPLEX WITH 4,4’-BIPYRIDINE AND 2-FORMYL- BENZENESULFONATE-HYDRAZINE

    Directory of Open Access Journals (Sweden)

    TAI XI-SHI

    2015-07-01

    Full Text Available A Na(I complex, [Na(4,4’-bipyridine2·(H2O4]·L·OH·2H2O (L = 2-formyl-benzenesulfonate-hydrazine, has been synthesized. And its structure was determined by X-ray single crystal diffraction analysis. The Na(I complex belongs to orthorhombic, space group C2221 with a = 7.9162(16 Å, b = 18.451(4 Å, c = 26.397(5 Å, V= 3855.7(13 Å3, Z = 4, Dc = 1.394 mg·m-3, μ = 0.218 mm-1, F(000 =1689, and final R1 = 0.0683, ωR2 = 0.2017. The result shows that the Na(I center is six-coordination with a N2O4 distorted octahedral coordination environment. The Na(I complex forms 1D chain structure by the π-π stacking interaction.

  3. High-Pressure Synthesis, Crystal Structure, and Magnetic Properties of Sr2MnO3F: A New Member of Layered Perovskite Oxyfluorides.

    Science.gov (United States)

    Su, Yu; Tsujimoto, Yoshihiro; Matsushita, Yoshitaka; Yuan, Yahua; He, Jianfeng; Yamaura, Kazunari

    2016-03-07

    We have successfully synthesized Sr2MnO3F, a new layered perovskite oxyfluoride with a n = 1 Ruddlesden-Popper-type structure using a high-pressure, high-temperature method. Structural refinements against synchrotron X-ray diffraction data collected from manganese oxyfluoride demonstrated that it crystallizes in a tetragonal cell with the space group I4/mmm, in which the Mn cation is located at the octahedral center position. This is in stark contrast to the related oxyhalides that have square-pyramidal coordination such as Sr2MO3X (M = Fe, Co, Ni; X = F, Cl) and Sr2MnO3Cl. There was no evidence of O/F site order, but close inspection of the anion environment centered at the Mn cation on the basis of bond-valence-sum calculation suggested preferential occupation of the apical sites by the F ion with one oxide ion in a random manner. Magnetic susceptibility and heat capacity measurements revealed an antiferromagnetic ordering at 133 K (=TN), which is much higher than that of the chloride analogue with corrugated MnO2 planes (TN = 80 K).

  4. A novel copper (II) complex containing a tetradentate Schiff base: Synthesis, spectroscopy, crystal structure, DFT study, biological activity and preparation of its nano-sized metal oxide

    Science.gov (United States)

    Tohidiyan, Zeinab; Sheikhshoaie, Iran; Khaleghi, Mouj; Mague, Joel T.

    2017-04-01

    A new nano-sized copper (II) complex, [Cu(L)] with a tetra dentate Schiff base ligand, 2-((E)-(2-(E-5- bromo-2-hydroxybezenylideneamino) methyl)-4-bromophenol [H2L] was prepared by the reaction between of Cu (CH3COO)2·2H2O and (H2L) ligand with the ratio of 1:1, at the present of triethylamine by sonochemical method. The structure of [Cu (L)] complex was determined by FT-IR, UV-Vis, FESEM and molar conductivity. The structure of [Cu (L)] complex was characterized by single crystal X-ray diffraction. The geometry of [Cu (L)] complex was optimized using density functional theory (DFT) method with the B3LYP/6-31(d) level of theory. The calculated bond lengths and bond angles are in good agreement with the X-ray data. This complex was used as a novel precursor for preparing of CuO nano particles by the thermal decomposition method. The antibacterial activities of [H2L] ligand, nano-sized [Cu (L)] complex and nano-sized CuO have been screened against various strains of bacteria. According to the results, nano-sized CuO can be considered as an appropriate antibiotic agent.

  5. imide, crystal structure, thermal and dielectric studies

    Indian Academy of Sciences (India)

    Abstract. A new geminal di-cationic ionic liquid (IL) containing a central cationic unit methylidene capped by a basic functionality (imidazole) is synthesized. The compound was characterized by means of 1H, 13C, 19F NMR,. IR and Raman spectroscopies and its crystal structure is confirmed by single crystal X-ray diffraction ...

  6. Crystal structures of MBP fusion proteins.

    Science.gov (United States)

    Waugh, David S

    2016-03-01

    Although chaperone-assisted protein crystallization remains a comparatively rare undertaking, the number of crystal structures of polypeptides fused to maltose-binding protein (MBP) that have been deposited in the Protein Data Bank (PDB) has grown dramatically during the past decade. Altogether, 102 fusion protein structures were detected by Basic Local Alignment Search Tool (BLAST) analysis. Collectively, these structures comprise a range of sizes, space groups, and resolutions that are typical of the PDB as a whole. While most of these MBP fusion proteins were equipped with short inter-domain linkers to increase their rigidity, fusion proteins with long linkers have also been crystallized. In some cases, surface entropy reduction mutations in MBP appear to have facilitated the formation of crystals. A comparison of the structures of fused and unfused proteins, where both are available, reveals that MBP-mediated structural distortions are very rare. © 2016 The Protein Society.

  7. Crystal Engineering

    Indian Academy of Sciences (India)

    Nangia (2002). “Today, research areas under the wide umbrella of crystal engineering include: supramolecular synthesis; nanotechnology; separation science and catalysis; supramolecular materials and devices; polymorphism; cocrystals, crystal structure prediction; drug design and ligand–protein binding.”

  8. Holmium polysulfide crystals: Structure, shape and composition

    International Nuclear Information System (INIS)

    Belaya, S.V.; Vasilyeva, I.G.; Naumov, D.Yu.; Podberezskaya, N.V.

    2006-01-01

    The variety of morphology, chemical composition and density of holmium polysulfide crystals grown from the flux in different as well as in the same experiments is observed. It was found that the crystals of different habits have the monoclinic structure, P2 1 /m, a=10.95, b=11.45, c=10.97A, β=91.3 o , as already known, and identical composition HoS 1.837 . All the crystals are twinned by the plane (101-bar ). It is shown that the diversity of crystal compositions and density values are due to the constitution of the flux in a crystal and displacement of a crystal in the growth zone. The formation of non-equilibrium growth forms is discussed

  9. Structural synthesis of parallel robots

    CERN Document Server

    Gogu, Grigore

    This book represents the fifth part of a larger work dedicated to the structural synthesis of parallel robots. The originality of this work resides in the fact that it combines new formulae for mobility, connectivity, redundancy and overconstraints with evolutionary morphology in a unified structural synthesis approach that yields interesting and innovative solutions for parallel robotic manipulators.  This is the first book on robotics that presents solutions for coupled, decoupled, uncoupled, fully-isotropic and maximally regular robotic manipulators with Schönflies motions systematically generated by using the structural synthesis approach proposed in Part 1.  Overconstrained non-redundant/overactuated/redundantly actuated solutions with simple/complex limbs are proposed. Many solutions are presented here for the first time in the literature. The author had to make a difficult and challenging choice between protecting these solutions through patents and releasing them directly into the public domain. T...

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

    Science.gov (United States)

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

    2014-05-05

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

  11. Synthesis, crystal structure, electric and magnetic properties of LaVO{sub 2.78}N{sub 0.10}

    Energy Technology Data Exchange (ETDEWEB)

    Yoon, Songhak; Maegli, Alexandra E.; Karvonen, Lassi; Shkabko, Andrey; Populoh, Sascha; Sagarna, Leyre; Aguirre, Myriam H.; Pokrant, Simone [Laboratory for Solid State Chemistry and Catalysis, Empa - Swiss Federal Laboratories for Materials Science and Technology, Duebendorf (Switzerland); Galazka, Krzysztof [Laboratory for Solid State Chemistry and Catalysis, Empa - Swiss Federal Laboratories for Materials Science and Technology, Duebendorf (Switzerland); Department of Chemistry and Biochemistry, University of Berne (Switzerland); Jakes, Peter; Eichel, Ruediger A. [Institut fuer Energie und Klimaforschung IEK-9, Forschungszentrum Juelich (Germany); Ebbinghaus, Stefan G. [Institut fuer Chemie, Martin-Luther Universitaet Halle-Wittenberg, Halle/Saale (Germany); Weidenkaff, Anke [Laboratory for Solid State Chemistry and Catalysis, Empa - Swiss Federal Laboratories for Materials Science and Technology, Duebendorf (Switzerland); Institute for Materials Science, University of Stuttgart (Germany)

    2014-04-15

    Perovskite-type LaVO{sub 2.78}N{sub 0.10} powder was synthesized by thermal ammonolysis of the oxide precursor LaVO{sub 4}. By X-ray, neutron, and electron diffraction an orthorhombic crystal structure with space group Pnma was identified. XANES spectra showed that the oxidation state of vanadium changes from 5+ in LaVO{sub 4} to approximately 3+ in LaVO{sub 2.78}N{sub 0.10}. The temperature dependence of the electrical conductivity revealed an Arrhenius-type behavior with an activation energy of 0.103 eV in the temperature range of 119-302 K indicating that the conduction process is thermally activated band transition. Based on the positive Seebeck coefficient, holes were identified as the dominant charge carriers in the temperature range of 100-302 K. Both the Seebeck coefficient and the thermal conductivity showed an anomaly at 138 K, which is attributed to the Neel temperature for antiferromagnetic ordering according to magnetic susceptibility measurements. (Copyright copyright 2014 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  12. Synthesis and crystal structure of a new Cu3Au-type ternary phase in the Au-In-Pd system: distribution of atoms over crystallographic positions.

    Science.gov (United States)

    Ptashkina, Evgeniya A; Kabanova, Elizaveta G; Tursina, Anna I; Yatsenko, Alexandr V; Kuznetsov, Victor N

    2018-03-01

    A new Cu 3 Au-type ternary phase (τ phase) is found in the AuPd-rich part of the Au-In-Pd system. It has a broad homogeneity range based on extensive (Pd,Au) and (In,Au) replacement, with the composition varying between Au 17.7 In 25.3 Pd 57.0 and Au 50.8 In 16.2 Pd 33.0 . The occupancies of the crystallographic positions were studied by single-crystal X-ray diffraction for three samples of different composition. The sites with m-3m symmetry are occupied by atoms with a smaller scattering power than the atoms located on 4/mmm sites. Two extreme structure models were refined. Within the first, the occupation type changes from (Au,In,Pd) 3 (Pd,In) to (Au,Pd) 3 (In,Pd,Au) with an increase in the Au gross content. For the second model, the occupation type (Au,In,Pd) 3 (Pd,Au) remains essentially unchanged for all Au concentrations. Although the diffraction data do not allow the choice of one of these models, the latter model, where Au substitutes In on 4/mmm sites, seems to be preferable, since it agrees with the fact that the homogeneity range of the τ phase is inclined to the Au corner and provides the same occupation type for all the studied samples of different compositions.

  13. Ferromagnetic interactions in new double end-on-azide-bridged dinuclear Ni(II) complex: Synthesis, crystal structures, magnetic and photoluminescence properties

    Science.gov (United States)

    Donmez, Adem; Oylumluoglu, Gorkem; Coban, M. Burak; Kocak, Cagdas; Aygun, Muhittin; Kara, Hulya

    2017-12-01

    A new double end-on azide-bridged dinuclear nickel(II) Schiff base complex, [Ni2(μ1,1-N3)2(HL)2(MeOH)2], [HL = 2-[(2-hydroxypropylimino)methyl)-3,5-chlorophenol] has been synthesized and characterized by elemental analysis, UV and IR spectroscopy, single crystal X-ray diffraction, magnetic and photoluminescence study. The asymmetric unit contains half of the dinuclear unit. The Ni(HL) units in each dinuclear molecule are connected to each other by two bridging end-on azide ligands. In the crystalline architecture of the Ni(II) complex, intermolecular Osbnd H⋯N hydrogen bonds link the molecules which form one-dimensional structure. Additionally, low temperature magnetic measurements indicate a dominant intradimer ferromagnetic interactions in double end-on azide-bridged dinuclear Ni(II) complex. Room temperature solid state photoluminescence measurements of Ni(II) complex show strong green emission band at λmax = 508 nm while its free ligand H2L shows broad yellow emission band at λmax = 594 nm. The luminescent performances making Ni(II) complex may be good candidates for potential luminescence materials.

  14. Design, synthesis and crystallization of a novel glucagon analog as a therapeutic agent

    Energy Technology Data Exchange (ETDEWEB)

    Li, Pengyun; Rogers, Tanya; Smiley, David; DiMarchi, Richard D.; Zhang, Faming, E-mail: fzhang@indiana.edu [Department of Chemistry and Biochemistry Program, Indiana University, Bloomington, Indiana 47405 (United States)

    2007-07-01

    The synthesis and crystallization of glucagon-Cex are reported. Glucagon and glucagon-like peptide 1 (GLP-1) are drugs or drug candidates for the treatment of metabolic diseases such as diabetes and obesity. The native hormones have pharmacological deficiencies such as short half-life and poor solubility. A novel glucagon receptor agonist named glucagon-Cex has been designed, synthesized and crystallized. This peptide was highly soluble under physiological conditions and crystallized readily. The crystal diffracted X-rays to 2.2 Å resolution and the diffraction was consistent with space group P23, with unit-cell parameters a = b = c = 48.20 Å, α = β = γ = 90.0°. The crystals were suitable for a full structural determination to reveal the conformational differences between glucagon-Cex and the native hormone.

  15. Design, synthesis and crystallization of a novel glucagon analog as a therapeutic agent

    International Nuclear Information System (INIS)

    Li, Pengyun; Rogers, Tanya; Smiley, David; DiMarchi, Richard D.; Zhang, Faming

    2007-01-01

    The synthesis and crystallization of glucagon-Cex are reported. Glucagon and glucagon-like peptide 1 (GLP-1) are drugs or drug candidates for the treatment of metabolic diseases such as diabetes and obesity. The native hormones have pharmacological deficiencies such as short half-life and poor solubility. A novel glucagon receptor agonist named glucagon-Cex has been designed, synthesized and crystallized. This peptide was highly soluble under physiological conditions and crystallized readily. The crystal diffracted X-rays to 2.2 Å resolution and the diffraction was consistent with space group P23, with unit-cell parameters a = b = c = 48.20 Å, α = β = γ = 90.0°. The crystals were suitable for a full structural determination to reveal the conformational differences between glucagon-Cex and the native hormone

  16. Controlled synthesis of thorium and uranium oxide nano-crystals

    International Nuclear Information System (INIS)

    Hudry, Damien; Apostolidis, Christos; Walter, Olaf; Gouder, Thomas; Courtois, Eglantine; Kubel, Christian; Meyer, Daniel

    2013-01-01

    Very little is known about the size and shape effects on the properties of actinide compounds. As a consequence, the controlled synthesis of well-defined actinide-based nano-crystals constitutes a fundamental step before studying their corresponding properties. In this paper, we report on the non-aqueous surfactant-assisted synthesis of thorium and uranium oxide nano-crystals. The final characteristics of thorium and uranium oxide nano-crystals can be easily tuned by controlling a few experimental parameters such as the nature of the actinide precursor and the composition of the organic system (e.g., the chemical nature of the surfactants and their relative concentrations). Additionally, the influence of these parameters on the outcome of the synthesis is highly dependent on the nature of the actinide element (thorium versus uranium). By using optimised experimental conditions, monodisperse isotropic uranium oxide nano-crystals with different sizes (4.5 and 10.7 nm) as well as branched nano-crystals (overall size ca. 5 nm), nano-dots (ca. 4 nm) and nano-rods (with ultra-small diameters of 1 nm) of thorium oxide were synthesised. (authors)

  17. Crystal structure prediction accelerated by Bayesian optimization

    Science.gov (United States)

    Yamashita, Tomoki; Sato, Nobuya; Kino, Hiori; Miyake, Takashi; Tsuda, Koji; Oguchi, Tamio

    2018-01-01

    We propose a crystal structure prediction method based on Bayesian optimization. Our method is classified as a selection-type algorithm which is different from evolution-type algorithms such as an evolutionary algorithm and particle swarm optimization. Crystal structure prediction with Bayesian optimization can efficiently select the most stable structure from a large number of candidate structures with a lower number of searching trials using a machine learning technique. Crystal structure prediction using Bayesian optimization combined with random search is applied to known systems such as NaCl and Y2Co17 to discuss the efficiency of Bayesian optimization. These results demonstrate that Bayesian optimization can significantly reduce the number of searching trials required to find the global minimum structure by 30-40% in comparison with pure random search, which leads to much less computational cost.

  18. Synthesis and photocatalytic activity of mesoporous – (001) facets TiO{sub 2} single crystals

    Energy Technology Data Exchange (ETDEWEB)

    Dong, Yeshuo [School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072 (China); Fei, Xuening, E-mail: xueningfei@126.com [School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072 (China); School of Science, Tianjin Chengjian University, Tianjin 300384 (China); Zhou, Yongzhu [School of Science, Tianjin Chengjian University, Tianjin 300384 (China)

    2017-05-01

    Highlights: • The (001) facets of TiO{sub 2} single crystals with mesoporous structure. • The (010) and (100) facets of TiO{sub 2} single crystals were covered by the flower – shaped TiO{sub 2} crystals. • This special structure could promote charge separation and provide more active sites, which will lead to a substantial increase in photocatalytic activity. - Abstract: In this work, the mesoporous – (001) facets TiO{sub 2} single crystals have been successfully synthesized through a two-step solvothermal route without any template. Their structure and morphology were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), ultraviolet-visible (UV–vis) diffuse reflectance spectroscopy and energy dispersive X-ray spectrometer (EDX). Based on the different characteristics and atomic arrangements on each facet of anatase TiO{sub 2} single crystals, we synthesized these mesoporous – (001) facets TiO{sub 2} single crystals by controlling the interaction characteristics of hydrofluoric acid (HF) and isopropanol (i-PrOH) on the crystal facets. It can been seen that the (001) facets of these as-synthesized TiO{sub 2} single crystals have a clear mesoporous structure through the SEM images and BET methods. Moreover, the other four facets were covered by the flower – shaped TiO{sub 2} crystals with the generation of the mesoporous – (001) facets. This special and interesting morphology could promote charge separation and provide more active sites, which will lead to a substantial increase in photocatalytic activity. Moreover, it is more intuitive to reflect that the different crystal facets possess the different properties due to their atomic arrangement. Besides, according to the different synthetic routes, we proposed and discussed a plausible synthesis mechanism of these mesoporous – (001) facets TiO{sub 2} single crystals.

  19. Abstract: Synthesis, structure and density functional theory (DFT ...

    Indian Academy of Sciences (India)

    Ruthenium Complexes of Chelating Amido-functionalized N-heterocyclic Carbene Ligands: Synthesis, Structure and DFT Studies. Sachin Kumar,† Anantha Narayanan,† Mitta Nageswar Rao,† Mobin M. Shaikh§ and Prasenjit Ghosh*,†. †Department of Chemistry and. §National Single Crystal X-ray Diffraction Facility,.

  20. UHMW Ziegler–Natta polyethylene: Synthesis, crystallization, and melt behavior

    KAUST Repository

    Atiqullah, Muhammad

    2017-04-26

    The fabrication of normal and UHMW PE end-products involves melting and crystallization of the polymer. Therefore, the melt behavior and crystallization of as-synthesized UHMW PE, and NMW PE and E-1-hexene copolymer have been studied using a new nonisothermal crystallization model, Flory\\'s equilibrium theory and ethylene sequence length distribution concept (SLD), Gibbs–Thompson equation, and DSC experiments. By using this approach, the effects of MW, 1-hexene incorporation, ethylene SLD, the level of undercooling θ, and crystal surface free energy D on crystallite stability, relative crystallinity α, instantaneous crystallinity χ, the crystallization kinetic triplet, crystallization entropy, and lamellar thickness distribution (LTD) have been evaluated. Consequently, this study reports insightful new results, interpretations, and explanations regarding the melting and crystallization of the aforementioned polymers. The UHMW PE results significantly differ from the NMW PE and E-1-hexene copolymer ones. Ethylene sequences shorter than the so called minimum crystallizable ethylene sequence length, irrespective of E-1-hexene copolymer MW, can also crystallize. Additionally, the polymer preparation shows that the catalyst coordination environment and symmetry, as well as achiral ethylene versus prochiral α-olefin steric encumbrance and competitive diffusion affect the synthesis of UHMW PE, particularly the corresponding UHMW copolymers.

  1. Liquid crystal light valve structures

    Science.gov (United States)

    Koda, N. J. (Inventor)

    1985-01-01

    An improved photosensor film and liquid crystal light valves embodying said film is provided. The photosensor film and liquid crystal light valve is characterized by a significant lower image retention time while maintaining acceptable photosensitivity. The photosensor film is produced by sputter depositing CdS onto an ITO substrate in an atmosphere of argon/H2S gas while maintaining the substrate at a temperature in the range of about 130 C to about 200 C and while introducing nitrogen gas into the system to the extent of not more than about 1% of plasma mixture. Following sputter deposition of the CdS, the film is annealed in an inert gas at temperatures ranging from about 300 C to about 425 C.

  2. [μ-1,1'-Bis(diphenylphosphine)ferrocene]bis(chlorogold): Synthesis, iron-57 and gold-197 Moessbauer spectroscopy, x-ray crystal structure, and antitumor activity

    International Nuclear Information System (INIS)

    Hill, D.T.; Girard, G.R.; McCabe, F.L.; Johnson, R.K.; Eggleston, D.S.; Stupik, P.D.; Zhang, J.H.; Reiff, W.M.

    1989-01-01

    The title compound 2, Fdpp(AuCl) 2 , synthesized via the addition of Fdpp (1) to an aqueous solution of [(HOCH 2 CH 2 ) 2 S]AuCl generated in situ by the thiodiglycol reduction of HAuCl 4 showed a 31 P[ 1 H] NMR chemical shift at δ 27.39, which was downfield from that of 1 at δ -17.34 relative to (CH 3 O)PO. The 57 Fe Moessbauer spectrum of 2 is a doublet with parameters (IS = 0.50 mm/s relative to Fe, QS = 2.33 mm/s) similar to those of ferrocene. The 197 Au Moessbauer spectrum of 2 is an asymmetric doublet (QS = 6.93 mm/s) with an IS of 3.81 mm/s relative to Au metal. Fdpp(AuCl) 2 crystallized in space group P bar 1 with lattice constants a = 16.192 (4) angstrom, b = 16.921 (4) angstrom, and c = 10.878 (5) angstrom with Z = 3. Two crystallographically independent molecules, A and B, were observed in the structure of 2 with a chloroform solvate molecule per 1.5 formula units of the gold complex. For A, the P atoms are 180 degree opposed and the rings exactly staggered, while in B the P atoms are 150 degree apart and the rings are partially staggered. The P-Au-Cl linkage is nearly linear, and the bond distances fall within normal ranges. Evaluation in an ip P388 leukemia mouse model showed 1 and 2 to have only marginal activity with an increased life span (ILS) relative to untreated controls of 30% at a maximally tolerated dose (MTD) of 231 μmol/kg and 40% ILS at 4 μmol/kg, respectively. 27 refs., 4 figs., 3 tabs

  3. 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.

  4. Study on potential antitumor mechanism of a novel Schiff base copper(II) complex: synthesis, crystal structure, DNA binding, cytotoxicity and apoptosis induction activity.

    Science.gov (United States)

    Qiao, Xin; Ma, Zhong-Ying; Xie, Cheng-Zhi; Xue, Fei; Zhang, Yan-Wen; Xu, Jing-Yuan; Qiang, Zhao-Yan; Lou, Jian-Shi; Chen, Gong-Jun; Yan, Shi-Ping

    2011-05-01

    A new cytotoxic copper(II) complex with Schiff base ligand [Cu(II)(5-Cl-pap)(OAc)(H(2)O)]·2H(2)O (1) (5-Cl-pap=N-2-pyridiylmethylidene-2-hydroxy-5-chloro-phenylamine), was synthesized and structurally characterized by X-ray diffraction. Single-crystal analysis revealed that the copper atom shows a 4+1 pyramidal coordination, a water oxygen appears in the apical position, and three of the basal positions are occupied by the NNO tridentate ligand and the fourth by an acetate oxygen. The interaction of Schiff base copper(II) complex 1 with DNA was investigated by UV-visible spectra, fluorescence spectra and agarose gel electrophoresis. The apparent binding constant (K(app)) value of 6.40×10(5) M(-1) for 1 with DNA suggests moderate intercalative binding mode. This copper(II) complex displayed efficient oxidative cleavage of supercoiled DNA, which might indicate that the underlying mechanism involve hydroxyl radical, singlet oxygen-like species, and hydrogen peroxide as reactive oxygen species. In addition, our present work showed the antitumor effect of 1 on cell cycle and apoptosis. Flow cytometric analysis revealed that HeLa cells were arrested in the S phase after treatment with 1. Fluorescence microscopic observation indicated that complex 1 can induce apoptosis of HeLa cells, whose process was mediated by intrinsic mitochondrial apoptotic pathway owing to the activation of caspase-9 and caspase-3. Copyright © 2011 Elsevier Inc. All rights reserved.

  5. The meloxicam complexes of Co(II) and Zn(II): Synthesis, crystal structures, photocleavage and in vitro DNA-binding

    Science.gov (United States)

    Sanatkar, Tahereh Hosseinzadeh; Hadadzadeh, Hassan; Simpson, Jim; Jannesari, Zahra

    2013-10-01

    Two neutral mononuclear complexes of Co(II) and Zn(II) with the non-steroidal anti-inflammatory drug meloxicam (H2mel, 4-hydroxy-2-methyl-N-(5-methyl-2-thiazolyl)-2H-1,2-benzothiazine-3-carboxammide-1,1-dioxide), [Co(Hmel)2(EtOH)2] (1), and [Zn(Hmel)2(EtOH)2] (2), were synthesized and characterized by elemental analysis, IR and UV-Vis spectroscopy and their solid-state structures were studied by single-crystal diffraction. The complexes have a distorted octahedral geometry around the metal atom. The experimental data indicate that the meloxicam acts as a deprotonated bidentate ligand (through the amide oxygen and the nitrogen atom of the thiazolyl ring) in the complexes, and a strong intramolecular hydrogen bond between the amide N-H function and the enolate O atom stabilizes the ZZZ conformation of meloxicam ligands. Absorption, fluorescence spectroscopy and cyclic voltammetry have been used to investigate the binding of the complexes with fish sperm DNA (FS-DNA). Additionally, the photocleavage studies have been also used to investigate the binding of the complexes with plasmid DNA. The interaction of the complexes with DNA was monitored by a blue shift and hyperchromism in the UV-Vis spectra attributed to an electrostatic binding mode. A competitive study with ethidium bromide (EB) has shown that the complexes can displace the DNA-bound EB indicating that they bind to DNA in strong competition with EB. The experimental results show that the complexes can cleave pUC57 plasmid DNA.

  6. Detonation-synthesis nanodiamonds: synthesis, structure, properties and applications

    International Nuclear Information System (INIS)

    Dolmatov, Valerii Yu

    2007-01-01

    The review outlines the theoretical foundations and industrial implementations of modern detonation synthesis of nanodiamonds and chemical purification of the nanodiamonds thus obtained. The structure, key properties and promising fields of application of detonation-synthesis nanodiamonds are considered.

  7. Structures of cyano-biphenyl liquid crystals

    Science.gov (United States)

    Chu, Yuan-Chao; Tsang, Tung; Rahimzadeh, E.; Yin, L.

    1989-01-01

    The structures of p-alkyl- p'-cyano- bicyclohexanes, C(n)H(2n+1) (C6H10)(C6H10) CN (n-CCH), and p-alkyl- p'-cyano- biphenyls, C(n)H(2n+1) (C6H4)(C6H4) CN (n-CBP), were studied. It is convenient to use an x ray image intensification device to search for symmetric x ray diffraction patterns. Despite the similarities in molecular structures of these compounds, very different crystal structures were found. For the smectic phase of 2CCH, the structure is close to rhombohedral with threefold symmetry. In contrast, the structure is close to hexagonal close-packed with two molecules per unit cell for 4CCH. Since intermolecular forces may be quite weak for these liquid crystals systems, it appears that crystal structures change considerably when the alkyl chain length is slightly altered. Different structures were also found in the crystalline phase of n-CBP for n = 6 to 9. For n = 7 to 9, the structures are close to monclinic. The structures are reminiscent of the smectic-A liquid crystal structures with the linear molecules slightly tilted away from the c-axis. In contrast, the structure is quite different for n = 6 with the molecules nearly perpendicular to the c-axis.

  8. Novel CoIII complexes containing fluorescent coumarin-N-acylhydrazone hybrid ligands: Synthesis, crystal structures, solution studies and DFT calculations

    Science.gov (United States)

    Areas, Esther S.; Bronsato, Bruna Juliana da S.; Pereira, Thiago M.; Guedes, Guilherme P.; Miranda, Fábio da S.; Kümmerle, Arthur E.; da Cruz, Antônio G. B.; Neves, Amanda P.

    2017-12-01

    A series of new CoIII complexes of the type [Co(dien)(L1 -L3)]ClO4 (1-3), containing fluorescent coumarin-N-acylhydrazonate hybrid ligands, (E)-N‧-(1-(7-oxido-2-oxo-2H-chromen-3-yl)ethylidene)-4-R-benzohydrazonate [where R = H (L12 -), OCH3 (L22 -) or Cl (L32 -)], were obtained and isolated in the low spin CoIII configuration. Single-crystal X-ray diffraction showed that the coumarin-N-acylhydrazones act as tridentate ligands in their deprotonated form (L2 -). The cation (+ 1) complexes contain a diethylenetriamine (dien) as auxiliary ligand and their structures were calculated by DFT studies which were also performed for the CoII (S = 1/2 and S = 3/2) configurations. The LS CoII (S = 1/2) concentrated the spin density on the O-Co-O axis while the HS CoII (S = 3/2) exhibited a broad spin density distribution around the metallic center. Cyclic voltammetry studies showed that structural modifications made in the L2 - ligands caused a slight influence on the electronic density of the metal center, and the E1/2 values for the CoIII/CoII redox couple increased following the electronic effect of the R-substituent, in the order: 2 (R = OCH3) experimental values vs SHE (E°calc = - 0.37, - 0.36 and - 0.32 V vs E°exp. = - 0.371, - 0.406 and - 0.358 V, for 1-3 respectively). Complexes 1-3 exhibited a very intense absorption band around 470 nm, assigned by DFT calculations as π-π* transitions from the delocalized coumarin-N-acylhydrazone system. 1-3 were very stable in MeOH for several days. Likewise, 1-3 were stable in phosphate buffer containing sodium ascorbate after 15 h, which was attributed to the high chelate effect and σ-donor ability of the L2 - and dien ligands.

  9. Synthesis, crystal structure, thermal analysis and dielectric properties of Rb4(SO4)(HSO4)2(H3AsO4) compound

    Science.gov (United States)

    Belhaj Salah, M.; Nouiri, N.; Jaouadi, K.; Mhiri, T.; Zouari, N.

    2018-01-01

    A new inorganic Rb4(SO4)(HSO4)2(H3AsO4) compound was prepared. It was found to crystallize in the monoclinic system (P21 space group) with the following lattice parameters: a = 5868 (1) Å, b = 13,579(2) Å, c = 11,809 (3) Å and β = 94,737 (1)°. The structure is characterized by SO42-, HSO4- and H3AsO4 tetrahedra connected by hydrogen bridge to form two types of dimmer (H(8)S(2)O4- … S(1)O42- and H(12)S(2)O4- … H3AsO4). These dimmers are interconnected by both hydrogen bonds O(14)sbnd H(14)· · ·O(4) and O(15)sbnd H(15)· · ·O(2). They are also linked by the hydrogen bridge assured by the hydrogen atoms H(2), H(3) and H(4) of the H3AsO4 group to build the chain S(1)O4⋯H3AsO4 which are parallel to the ''a'',direction. The rubidium cations are coordinated by eight oxygen atoms with Rbsbnd O distance ranging from 2893(8) to 3.415(6) Å. The existence of Osbnd H and (S/As)sbnd O bonds in the structure at room temperature has been confirmed by IR and Raman spectroscopy in the frequency ranges 4000-400 cm-1and 1200 - 50 cm-1, respectively. Thermal analysis of Rb4(HSO4)(HSO4)2(H3AsO4) showed that the transformation to high temperature phase occurs at 407 K by one-step process. Thermal decomposition of the product takes place at much higher temperatures, with an onset of approximately 522 K. The first transition detected by differential scanning calorimetry (DSC) was also analyzed by dielectric and conductivity measurements using the impedance spectroscopy techniques. The conductivity in the high temperature phase at 428 K is 1.04 × 10-3 Ω-1 cm-1, and the activation energy for the proton transport is 0.36 eV. The conductivity relaxation parameters associated with the high disorder protonic conduction have been examined from analysis of the M"/M"max spectrum measured in a wide temperature range. Transport properties of this material appear to be due to the proton hopping mechanism. The obtained results show that this transition is protonic by nature.

  10. Synthesis and structure of bis(β-dibenzoyl methanato -O,O') (aquo-O ...

    Indian Academy of Sciences (India)

    Synthesis and structure of bis(β-dibenzoyl methanato -O,O') (aquo-O) dioxouranium (VI) compound ... Keywords. β-diketonates; uranyl ion; adduct compound; crystal structure; hydrogen bonding. 1. Introduction. Structural studies on uranyl ... crystalline product obtained was filtered, washed with ether and dried. The crystal ...

  11. Fusion proteins as alternate crystallization paths to difficult structure problems

    Science.gov (United States)

    Carter, Daniel C.; Rueker, Florian; Ho, Joseph X.; Lim, Kap; Keeling, Kim; Gilliland, Gary; Ji, Xinhua

    1994-01-01

    The three-dimensional structure of a peptide fusion product with glutathione transferase from Schistosoma japonicum (SjGST) has been solved by crystallographic methods to 2.5 A resolution. Peptides or proteins can be fused to SjGST and expressed in a plasmid for rapid synthesis in Escherichia coli. Fusion proteins created by this commercial method can be purified rapidly by chromatography on immobilized glutathione. The potential utility of using SjGST fusion proteins as alternate paths to the crystallization and structure determination of proteins is demonstrated.

  12. Synthesis of zeolite-like crystals by means of sorption of bases on polysilicic acids

    International Nuclear Information System (INIS)

    Belyakova, L.A.; Il'in, V.G.; Peresun'ko, T.F.; Kryuchkova, I.I.; Nejmark, I.E.

    1974-01-01

    Investigation into the sorption of bases on crystalline polysilicic acids is of particular interest from the viewpoint of synthesis of new types of porous zeolite-like materials. A synthesis of polysilicate acids was carried out by treating respective sodium polysilicates with mineral acid solutions. The sorption of alkali metal hydroxides in the neutral and alkaline pH region was studied by the method of potentiometric titration of individual weighed quantities. A marked sorption of alkali metal hydroxides on polysilicic acids starts in the weakly acid and neutral regions and reaches saturation at pHapproximately10.5. The process of ion exchange is accompanied by a change in the crystal structure of polysilicic acids. The sorption of bases on polysilicic acids may be used as a method of synthesis of zeolite-like porous crystals in different cationic forms

  13. Synthesis, Crystal Structure, Gas Absorption, and Separation Properties of a Novel Complex Based on Pr and a Three-Connected Ligand

    Directory of Open Access Journals (Sweden)

    Jie Sun

    2017-12-01

    Full Text Available A novel Pr complex, constructed from a rigid three-connected H3TMTA and praseodymium(III ion, has been synthesized in a mixed solvent system and characterized by X-ray single crystal diffraction, infrared spectroscopy, a thermogravimetric analysis, an element analysis, and powder X-ray diffraction, which reveals that complex 1 crystallizes in a three-dimensional porous framework. Moreover, the thermal stabilities and the fluorescent and gas adsorption and separation properties of complex 1 were investigated systematically.

  14. Tailoring quantum structures for active photonic crystals

    DEFF Research Database (Denmark)

    Kuznetsova, Nadezda

    This work is dedicated to the tailoring of quantum structures, with particular attention to the integration of selective area grown (SAG) active material into photonic crystal (PhC) slabs. The platform based on active PhC is vital to the realization of highly efficient elements with low energy......; in particular, the emission control of SAG QW matched the operating wavelength of photonic crystals. A strong photoluminescence signal in the slow light regime with the group index of 18 was demonstrated....

  15. Heteropentanuclear Oxalato-Bridged nd–4f (n=4, 5) Metal Complexes with NO Ligand: Synthesis, Crystal Structures, Aqueous Stability and Antiproliferative Activity

    KAUST Repository

    Kuhn, Paul-Steffen

    2015-08-10

    A series of heteropentanuclear oxalate-bridged Ru(NO)-Ln (4d–4f) metal complexes of the general formula (nBu4N)5[Ln{RuCl3(μ-ox)(NO)}4], where Ln=Y (2), Gd (3), Tb (4), Dy (5) and ox=oxalate anion, were obtained by treatment of (nBu4N)2[RuCl3(ox)(NO)] (1) with the respective lanthanide salt in 4:1 molar ratio. The compounds were characterized by elemental analysis, IR spectroscopy, electrospray ionization (ESI) mass spectrometry, while 1, 2, and 5 were in addition analyzed by X-ray crystallography, 1 by Ru K-edge XAS and 1 and 2 by 13C NMR spectroscopy. X-ray diffraction showed that in 2 and 5 four complex anions [RuCl3(ox)(NO)]2− are coordinated to YIII and DyIII, respectively, with formation of [Ln{RuCl3(μ-ox)(NO)}4]5− (Ln=Y, Dy). While YIII is eight-coordinate in 2, DyIII is nine-coordinate in 5, with an additional coordination of an EtOH molecule. The negative charge is counterbalanced by five nBu4N+ ions present in the crystal structure. The stability of complexes 2 and 5 in aqueous medium was monitored by UV/Vis spectroscopy. The antiproliferative activity of ruthenium-lanthanide complexes 2–5 were assayed in two human cancer cell lines (HeLa and A549) and in a noncancerous cell line (MRC-5) and compared with those obtained for the previously reported Os(NO)-Ln (5d–4f) analogues (nBu4N)5[Ln{OsCl3(ox)(NO)}4] (Ln=Y (6), Gd (7), Tb (8), Dy (9)). Complexes 2–5 were found to be slightly more active than 1 in inhibiting the proliferation of HeLa and A549 cells, and significantly more cytotoxic than 5d–4f metal complexes 6–9 in terms of IC50 values. The highest antiproliferative activity with IC50 values of 20.0 and 22.4 μM was found for 4 in HeLa and A549 cell lines, respectively. These cytotoxicity results are in accord with the presented ICP-MS data, indicating five- to eightfold greater accumulation of ruthenium versus osmium in human A549 cancer cells.

  16. A 2D nickel-based energetic MOFs incorporating 3,5-diamino-1,2,4-triazole and malonic acid: Synthesis, crystal structure and thermochemical study

    International Nuclear Information System (INIS)

    Yang, Qi; Song, Xiaxia; Ge, Jing; Zhao, Guowei; Zhang, Wendou; Xie, Gang; Chen, Sanping; Gao, Shengli

    2016-01-01

    Highlights: • An energetic MOFs with dinuclear nickel unit has been synthesized and characterized. • The Arrhenius equation, derived from kinetics analysis, is ln k = 55.89 − 332.01 × 10 3 /RT. • The standard molar enthalpy of formation of the compound is determined by a thermochemical cycle. • The molar heat capacity at T = 298.15 K is determined to be 1.42 ± 0.11 J · K −1 · g −1 . - Abstract: A new energetic MOFs, {[Ni 2 (C 2 H 5 N 5 ) 2 (C 3 H 2 O 4 ) 2 (H 2 O)]·3H 2 O} n (Hdatrz (C 2 H 5 N 5 ) = 3,5-diamino-1,2,4-triazole, H 2 mal (C 3 H 4 O 4 ) = malonic acid), has been synthesized and characterized by element analysis, chemical analysis, IR spectroscopy, single-crystal X-ray diffraction and thermal analysis. X-ray diffraction analysis confirmed that the compound featured a 2D layer structure with dinuclear Ni(II) unit. Thermal analysis demonstrated that the compound after dehydration have good thermostability with decomposition temperature up to 633 K. The non-isothermal kinetics for the compound was studied by Kissinger’s and Ozawa’s methods. The Arrhenius equation of initial thermal decomposition process of compound can be expressed as ln k = 55.89 − 332.01 × 10 3 /RT. Furthermore, a reasonable thermochemical cycle was designed based on the preparation reaction of the compound, and standard molar enthalpy of dissolution of reactants and products were measured by RD496-2000 calorimeter. Finally, the standard molar enthalpy of formation of the compound was determined to be −(2766.3 ± 2.3) kJ · mol −1 in accordance with Hess’s law. In addition, the specific heat capacity of the compound at T = 298.15 K was determined to be 1.42 ± 0.11 J · K −1 · g −1 by RD496-2000 calorimeter.

  17. Efficient hydrolytic cleavage of plasmid DNA by chloro-cobalt(II) complexes based on sterically hindered pyridyl tripod tetraamine ligands: synthesis, crystal structure and DNA cleavage.

    Science.gov (United States)

    Massoud, Salah S; Perkins, Richard S; Louka, Febee R; Xu, Wu; Le Roux, Anne; Dutercq, Quentin; Fischer, Roland C; Mautner, Franz A; Handa, Makoto; Hiraoka, Yuya; Kreft, Gabriel L; Bortolotto, Tiago; Terenzi, Hernán

    2014-07-14

    Four new cobalt(ii) complexes [Co(6-MeTPA)Cl]ClO4/PF6 (2/2a), [Co(6-Me2TPA)Cl]ClO4/PF6 (3/3a), [Co(BPQA)Cl]ClO4/PF6 (4/4a) and [Co(BQPA)Cl]ClO4/PF6 (5/5a) as well as [Co(TPA)Cl]ClO4 (1) where TPA = tris(2-pyridylmethyl)amine, 6-MeTPA = ((6-methyl-2-pyridyl)methyl)bis(2-pyridylmethyl)amine, 6-Me2TPA = bis(6-methyl-2-pyridyl)methyl)-(2-pyridylmethyl)amine, BPQA = bis(2-pyridylmethyl)-(2-quinolylmethyl)-amine and BQPA = bis(2-quinolylmethyl)-(2-pyridylmethyl)amine were synthesized and structurally characterized. Single crystal X-ray crystallography confirmed the distorted trigonal bipyramidal geometries of complexes 2a-5a. Spectrophotometric titrations and conductivity measurements of the complexes in the CH3CN-H2O mixture showed that the chloro complexes exist in equilibrium with the corresponding hydrolyzed aqua species, [Co(L)(H2O)](2+). The pKa values of the coordinated H2O in aqua complexes vary from 8.4 to 8.7 (37 °C). The interactions of the complexes (1-5) with DNA have been investigated at pH = 7.0 and 9.0 (10 mM Tris-HCl buffer) and 37 °C where very high catalytic cleavage was observed. Under pseudo Michaelis-Menten kinetic conditions, the catalytic rate constants, kcat, decrease in the order 4>2>5>1>3. At pH 7.0 (10 mM Tris-HCl buffer) and 37 °C, the kcat value for complex 4 (6.02 h(-1)), where [Co(BPQA)(H2O)](2+) is the major species, corresponds to 170 million rate enhancement over the non-catalyzed DNA. Electrophoretic experiments conducted in the presence and absence of radical scavengers (DMSO, KI, NaN3) ruled out the oxidative mechanistic pathway of the reaction and suggested that the hydrolytic mechanism is the preferred one. This finding was in agreement with the observed increase in the kcat values at pH 9.0 compared to the corresponding values at pH 7.0 as a result of the increased concentration of the reactive hydroxo species, [Co(L)(OH)](+). The reactivity of the synthesized complexes in catalyzing the DNA cleavage is discussed in relation to

  18. 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.

  19. Two-dimensional photonic crystal accelerator structures

    Directory of Open Access Journals (Sweden)

    Benjamin M. Cowan

    2003-10-01

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

  20. Crystal structure of enolase from Drosophila melanogaster.

    Science.gov (United States)

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

    2017-04-01

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

  1. Generalized synthesis of mesoporous shells on zeolite crystals

    KAUST Repository

    Han, Yu

    2010-12-30

    A simple and generalized synthetic approach is developed for creating mesoporous shells on zeolite crystals. This method allows for the tailoring of thickness, pore size, and composition of the mesoporous shell, and can be applied to zeolites of various structures, compositions, and crystal sizes. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. synthesis and structures

    Indian Academy of Sciences (India)

    Priya Saxena

    2017-08-29

    Aug 29, 2017 ... complexes as well as for biological applications.16–24. Of particular mention here are the nickel and palladium complexes of ..... tion and indexing were performed with CrysAlisPro software suite.42 WinGX module was used to perform all the cal- culations.43 The structures were solved by direct methods.

  3. Synthesis, experimental and theoretical studies on its crystal structure and FT-IR spectrum of new thiosemicarbazone compound E-2-(4-isopropylbenzylidene)thiosemicarbazone

    Czech Academy of Sciences Publication Activity Database

    Khalaji, A.D.; Mehrani, S.; Eigner, Václav; Dušek, Michal

    2013-01-01

    Roč. 1047, SEP (2013), s. 87-94 ISSN 0022-2860 Grant - others:AV ČR(CZ) AP0701 Program:Akademická prémie - Praemium Academiae Institutional support: RVO:68378271 Keywords : thiosemicarbazide * single crystal * FT-IR * 1 H NMR * DFT Subject RIV: CB - Analytical Chemistry , Separation Impact factor: 1.599, year: 2013

  4. 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

  5. Design and Synthesis of Novel Discotic Liquid Crystals

    Science.gov (United States)

    Kayal, Himadri Sekhar

    Columnar mesophases of discotic liquid crystals (DLCs) have attracted much attention as organic semiconductors and have been tested as active materials in light-emitting diodes, photovoltaic solar cells, and field-effect transistors. However, devices based on DLCs have shown lower performance than devices based on polymeric and small molecule glass semiconductors, despite their superior charge conducting and advantages self-organizing properties. Most DLCs also require relatively complex processing conditions for the preparation of electronic devices, which is another significant disadvantage. Consequently, new types of DLCs are sought-after to overcome these limitations and described in this thesis are new types of discotic materials and their synthesis. Chapters 2 and 3 describe star-shaped discotic molecules for donor-acceptor columnar structures and as novel flexible core discotic molecules. Presented are the first examples of star-shaped heptamers of donor and acceptor discotic molecules which have six hexaalkoxy triphenylene ligands and a hexaazatriphenylene hexacarboxylate core or a hexaazatriphenylene hexaamide core. The hexaazatriphenylene cores were chosen because of their electron deficient character while the hexaalkoxy triphenylenes are known to be electron rich. Envisioned is the formation of super-columns in which the heptamers stack on top of each other and generate a material with electron acceptor and electron donor channels separated by aliphatic chains. This is an important difference to previously reported donor-acceptor star-shaped structures that were connected via conjugated linkers and do not form separate columnar stacks. Star-shaped DLCs based on small aromatic groups linked together by short flexible spacers may represent a novel type of discotic core structure that does not require peripheral flexible chains. Softening of the core by the spacer group is expected to sufficiently lower melting points and not interfere with the columnar

  6. 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.

  7. Nucleation and structural growth of cluster crystals

    International Nuclear Information System (INIS)

    Leitold, Christian; Dellago, Christoph

    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, we study the particle mobility in the supercooled liquid and in the cluster crystal. In the cluster crystal, the motion of individual particles is captured by a simple reaction-diffusion model introduced previously to model the kinetics of hydrogen bonds.

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

    Science.gov (United States)

    Evans, H.T.; 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

  9. Synthesis, structural characterization and Hirshfeld analysis studies of three novel co-crystals of trans-4-[(2-amino-3,5-dibrobenzyl) amino] cyclohexanol with hydroxyl benzoic acids

    Science.gov (United States)

    Ma, Yu-heng; Lou, Ming; Sun, Qing-yang; Ge, Shu-wang; Sun, Bai-wang

    2015-03-01

    Combination of active pharmaceutical ingredients, trans-4-[(2-amino-3,5-dibrobenzyl) amino] cyclohexanol (AMB) and some organic acids, e.g., p-hydroxybenzoic acid (PHBA), m-hydroxybenzoic acid (MHBA), and 3,4-dihydroxy benzoic acid (DHBA), yield three novel co-crystals characterized by X-ray single-crystal, Fluorescence spectroscopy and thermal analysis (DSC and TGA), which included co-crystal 1 with 2:2: 1 stoichiometry of AMB, PHBA and H2O, co-crystal 2 with 1:1 stoichiometry of AMB and MHBA, and co-crystal 3 with 1:1:1 stoichiometry of AMB, DHBA and CH3OH. Constituents of the co-crystalline phase were also investigated in terms of Hirshfeld surfaces. In the crystal lattice, a three-dimensional hydrogen-bonded network is observed, including formation of a two-dimensional molecular scaffolding motif. Hirshfeld surfaces and fingerprint plots of three co-crystals show that structures are stabilized by H⋯H, N-H⋯O, H⋯Br and C⋯H intermolecular interactions. Besides, the studies of the solubility showed that this co-crystal strategy could promote the solubility of AMB and follow the order: co-crystal 1 < co-crystal 2 < co-crystal 3.

  10. Synthesis and Crystal Structure of a Five-Coordinate Complex of Copper(II) with 4-Nitrobenzenesulfonate and 2, 2'-Bipyridine.

    Science.gov (United States)

    Sharif, Mahboubeh A; Tabatabaee, Masoumeh; Beik, Vahideh; Khavasi, Hamid Reza

    2012-06-01

    [Cu(bipy)2Cl](nbs) (1) (bipy = 2,2'-bipyridine, nbs = 4-nitrobenzenesulfonate) was obtained from the reaction of 4-nitrobenzenesulfonyl chloride and 2-amine-4-methylopyridine with CuCl2 in the presence of 2,2'-bipyridine and characterized by elemental analysis, IR spectra and X-ray single-crystal diffraction. The asymmetric unit of (1) contains the cationic complex [Cu(bipy)2Cl]+ and, in the outer coordination sphere, an (nbs)- counter ion.

  11. Synthesis, crystal structure and photoluminescence study of green light emitting bis(1[(4-butylphenylimino]methyl naphthalen-2-ol Ni(II complex

    Directory of Open Access Journals (Sweden)

    M. Srinivas

    2016-09-01

    Full Text Available Synthetically feasible and cost effective Ni(II complex phosphor (4 as green organic light emitting diode (OLED was prepared by using Schiff base 1-[(4-butylphenylimino]methyl naphthalen-2-ol (3. The single crystals of Ni(II complex were grown from chloroform and hexane (1:1 v/v solution. The green crystals of the complex were characterized by using single crystal XRD studies and were evaluated for their photophysical properties. From the Diffused Reflectance Spectrum of the complex, the measured band gap energy was found to be 1.83 eV and the PL spectrum of the complex showed emission peak at 519 nm. The excitation peaks at 519 nm were appeared at 394 nm and 465 nm. The Commission Internationale De L'Eclairage (CIE chromaticity diagram indicated that, the complex exhibit green color. Hence, Ni(II complex (4 could be a promising green OLED for developing strong electroluminescent materials for flat panel display applications.

  12. Synthesis, crystal structure and excellent photoluminescence properties of copper (II and cobalt (II complexes with Bis(1[(4-butylphenylimino]methyl naphthalen-2-ol Schiff base

    Directory of Open Access Journals (Sweden)

    V.B. Nagaveni

    2018-03-01

    Full Text Available Copper (II and Cobalt (II metal complexes (4a- and 4b-complexes using Schiff base ligand 1-[(4-butylphenylimino]methyl naphthalen-2-ol (3 have been synthesized. The single crystals of Copper (II and Cobalt (II complex phosphors were grown and characterized by Fourier-Transform Infrared (FT-IR, single crystal X-ray diffraction (XRD, SEM (Scanning Electron Microscope and EDS (Energy Dispersive X-ray spectroscopy. Photoluminescence study of the phosphors revealed the presence of excitation peaks at 333 nm and 360 nm for 4a-complex (λemi = 495 nm and excitation peaks at 300 nm and 360 nm for 4b-complex (λemi = 496 nm. The calculated CCT values of the complexes pointed out that these materials can be used to obtain cold white light from the light emitting devices. Diffuse reflectance spectra (DRS showed the measured band gap energies of 1.78 eV and 1.44 eV for Cu (II and Co (II complexes, respectively. It is concluded that the 4a- and 4b-complexes become white and blue green light emitting diodes respectively and will be useful in the development of strong electroluminescent materials. Keywords: 1[(4-butylphenylimino]methylnaphthalen-2-ol, Schiff base, Cu (II and Co (IIcomplex, Photoluminescence, Single crystal XRD, OLED

  13. Synthesis and crystal structure of Na6[(UO2)3O(OH)3(SeO4)2]2·10H2O

    International Nuclear Information System (INIS)

    Baeva, E.Eh.; Serezhkina, L.B.; Virovets, A.V.; Peresypkina, E.V.

    2006-01-01

    The complex Na 6 [(UO 2 ) 3 O(OH) 3 (SeO 4 ) 2 ] 2 ·10H 2 O (I) is synthesized and studied by monocrystal X-ray diffraction. The compound crystallizes in the orthorhombic crystal system with the unit cell parameters: a=14.2225(7) A, b=18.3601(7) A, c=16.5406(6) A, V=4319.2(3) A 3, Z=4, space group Cmcm, R 1 =0.0406. Compound I is found to be a representative of the crystal-chemical group A 3 M 3 M 3 2 T 2 3 (A=UO 2 2+ , M 3 =O 2- , M 2 =OH - , T 3 =SeO 4 2- ) of the uranyl complexes; it contains layer uranium-containing groups [(UO 2 ) 3 O(OH) 3 (SeO 4 ) 2 ] 3- . These layers are linked to form a three-dimensional cage through bonds formed by the sodium atoms with the oxygen atoms of the uranyl ions and SeO 4 groups that belong to different layers [ru

  14. Three Novel Lanthanide Metal-Organic Frameworks (Ln-MOFs Constructed by Unsymmetrical Aromatic Dicarboxylatic Tectonics: Synthesis, Crystal Structures and Luminescent Properties

    Directory of Open Access Journals (Sweden)

    Ya-Pan Wu

    2014-09-01

    Full Text Available Three novel Ln(III-based coordination polymers, {[Ln2 (2,4-bpda3 (H2Ox]·yH2O}n (Ln = La (III (1, x = 2, y = 0, Ce (III (2, Pr (III (3, x = 4, y = 1 (2,4-H2bpda = benzophenone-2,4-dicarboxylic acid have been prepared via a solvothermal method and characterized by elemental analysis, IR, and single-crystal X-ray diffraction techniques. Complex 1 exhibits a 3D complicated framework with a new 2-nodal (3,7-connected (42·5 (44·51·66·8 topology. Complexes 2 and 3 are isomorphous, and feature a 3D 4-connected (65·8-CdSO4 network. Moreover, solid-state properties such as thermal stabilities and luminescent properties of 1 and 2 were also investigated. Complex 1 crystallized in a monoclinic space group P21/c with a = 14.800 (3, b = 14.500 (3, c = 18.800 (4 Å, β = 91.00 (3, V = 4033.9 (14 Å3 and Z = 4. Complex 2 crystallized in a monoclinic space group Cc with a = 13.5432 (4, b = 12.9981 (4, c = 25.7567 (11 Å, β = 104.028 (4, V = 1374.16 (7 Å3 and Z = 4.

  15. VO{sub 2} (A): Reinvestigation of crystal structure, phase transition and crystal growth mechanisms

    Energy Technology Data Exchange (ETDEWEB)

    Rao Popuri, Srinivasa [ICMCB, CNRS, UPR 9048, F-33608 Pessac (France); University of Bordeaux, ICMCB, UPR 9048, F-33608 Pessac (France); National Institute for Research and Development in Electrochemistry and Condensed Matter, Timisoara, Plautius Andronescu Str. No. 1, 300224 Timisoara (Romania); Artemenko, Alla [ICMCB, CNRS, UPR 9048, F-33608 Pessac (France); University of Bordeaux, ICMCB, UPR 9048, F-33608 Pessac (France); Labrugere, Christine [CeCaMA, University of Bordeaux 1, ICMCB, 87 Avenue du Dr. A. Schweitzer, F-33608 Pessac (France); Miclau, Marinela [National Institute for Research and Development in Electrochemistry and Condensed Matter, Timisoara, Plautius Andronescu Str. No. 1, 300224 Timisoara (Romania); Villesuzanne, Antoine [ICMCB, CNRS, UPR 9048, F-33608 Pessac (France); University of Bordeaux, ICMCB, UPR 9048, F-33608 Pessac (France); Pollet, Michaël, E-mail: pollet@icmcb-bordeaux.cnrs.fr [ICMCB, CNRS, UPR 9048, F-33608 Pessac (France); University of Bordeaux, ICMCB, UPR 9048, F-33608 Pessac (France)

    2014-05-01

    Well crystallized VO{sub 2} (A) microrods were grown via a single step hydrothermal reaction in the presence of V{sub 2}O{sub 5} and oxalic acid. With the advantage of high crystalline samples, we propose P4/ncc as an appropriate space group at room temperature. From morphological studies, we found that the oriented attachment and layer by layer growth mechanisms are responsible for the formation of VO{sub 2} (A) micro rods. The structural and electronic transitions in VO{sub 2} (A) are strongly first order in nature, and a marked difference between the structural transition temperatures and electronic transitions temperature was evidenced. The reversible intra- (LTP-A to HTP-A) and irreversible inter- (HTP-A to VO{sub 2} (M1)) structural phase transformations were studied by in-situ powder X-ray diffraction. Attempts to increase the size of the VO{sub 2} (A) microrods are presented and the possible formation steps for the flower-like morphologies of VO{sub 2} (M1) are described. - Graphical abstract: Using a single step and template free hydrothermal synthesis, well crystallized VO{sub 2} (A) microrods were prepared and the P4/ncc space group was assigned to the room temperature crystal structure. Reversible and irreversible phase transitions among different VO{sub 2} polymorphs were identified and their progressive nature was highlighted. Attempts to increase the microrods size, involving layer by layer formation mechanisms, are presented. - Highlights: • Highly crystallized VO{sub 2} (A) microrods were grown via a single step hydrothermal process. • The P4/ncc space group was determined for VO{sub 2} (A) at room temperature. • The electronic structure and progressive nature of the structural phase transition were investigated. • A weak coupling between structural and electronic phase transitions was identified. • Different crystallite morphologies were discussed in relation with growth mechanisms.

  16. Nano crystals-Related Synthesis, Assembly, and Energy Applications

    International Nuclear Information System (INIS)

    Dai, Q.; Hu, M.Z.; Yu, B.Z.; William, W.; Seo, J.

    2011-01-01

    Fundamental material properties have been dramatically altered in the nano scale regime because of quantum confinement effect. The unique size-tunable functionalities of nano materials make them involved in an extensive variety of energy applications, such as light-emitting diodes and solar cells. These applications have been demonstrated to cut energy consumption. In response to the ever-growing energy demands as well as the concerns of global warming, researchers are actively placing their enormous emphasis on the exploration of energy savings. During this exploration, the primary stage requires the design of appropriate strategies for the synthesis of high-quality nano crystals in terms of size uniformity and superior optical/electronic properties. Especially, there is a need to seek green-chemistry approaches for the synthesis of environmentally benign and user-friendly nano crystals. Another recent area of focus is the use of individual nano crystals as building blocks for self-assembly, providing new opportunities to improve the nano crystal performance

  17. Synthesis, crystal structure, vibrational profiling, DFT studies and molecular docking of N-(4-chloro-2-{[2-(1H-indol-2-ylcarbonyl) hydrazinyl](oxo)acetyl}phenyl)acetamide.DMSO: A new antiproliferative agent

    Science.gov (United States)

    Al-Wabli, Reem I.; Salman, Asmaa; Shyni, V.; Ghabbour, Hazem A.; Joe, I. Hubert; Almutairi, Maha S.; Maklad, Yousreya A.; Attia, Mohamed I.

    2018-03-01

    Cancer is one of the most serious health problems worldwide and it is considered the second major cause of mankind deaths. We report the synthesis and spectroscopic characterization of N-(4-chloro-2-{[2-(1H-indol-2-ylcarbonyl)hydrazinyl](oxo)acetyl}phenyl)acetamide (CICHOPA, 5) as a new antiproliferative glyoxylamide derivative. Molecular structure of CICHOPA (5) was unequivocally confirmed via X-ray analysis and it was crystallized in the monoclinic, P21/c, a = 14.3956 (4) Å, b = 8.9307 (3) Å, c = 34.9507 (10) Å, β = 94.439 (1)°, V = 4479.9 (2) Å3, Z = 8. The in vitro anticancer potential of the title molecule 5 was examined toward four types of human cancer cell lines. Vibrational profile of the CICHOPA molecule was investigated with the aid of density functional theory approach. Natural bond orbital, and natural population analyses as well as HOMO and LUMO molecular orbitals studies were carried out in order to explore the possible intermolecular delocalization or hyperconjugation in the title compound. The binding mode of compound 5 to its target protein was predicted through a molecular docking investigation. The in vitro antiproliferative activity of the title compound 5 was examined against four human cancer cell lines and showed growth inhibitory activity at concentrations of 25 and 50 μM.

  18. Synthesis and X-ray crystal structure of cationic polynuclear hydroxide acetylacetonate lanthanide(III) clusters with homodinuclear or heterodinuclear decacarbonyl hydrides: [HMo2(CO)1]- and [HCrW(CO)1]-

    International Nuclear Information System (INIS)

    Volpe, M.; Bombieri, G.; Marchini, N.

    2006-01-01

    The synthesis and characterization of new polynuclear lanthanide(III) ionic clusters of general formula [Ln 9 (acac) 16 (OH) 1 ] + [Mo 2 (CO) 1 (μ-H)] - (Ln = Sm, Eu, Gd, Dy, Yb) and [Sm 9 (acac) 16 (OH) 1 ] + [CrW(CO) 1 (μ-H)] - is reported. The polynuclear complexes, prepared under pure nitrogen atmosphere by interaction of the hydridic metal carbonyls with the β-dichetonate Ln(acac) 3 .3H 2 O (Ln = Sm, Eu, Gd, Dy, Yb). The new clusters were characterized by elemental analysis, complexometric titration for Ln, atomic absorption for Cr, W and Mo, gas-volumetric analysis for CO, FTIR spectroscopy and single crystal X-ray structure determination of [Sm 9 (acac) 16 (OH) 1 ][Mo 2 (CO) 1 (μ-H)]. The Eu and Yb complexes are isostructural to the Sm one for which, similarly to their homonuclear chromium and tungsten derivative analogues, a square antiprismatic arrangement of eight Sm ions with the ninth at the center of the antiprism has been found

  19. Synthesis and crystal structures and luminescent properties of divalent europium-doped Ba2ZnSi2O7 and BaZn2Si2O7

    International Nuclear Information System (INIS)

    Yao Shanshan; Xue Lihong; Yan Youwei

    2011-01-01

    The monoclinic Ba 2 ZnSi 2 O 7 :Eu 2+ blue-green-emitting phosphor and the orthorhombic BaZn 2 Si 2 O 7 :Eu 2+ green-emitting phosphor were prepared by combustion-assisted synthesis method as the fluorescent materials for ultraviolet-light-emitting diodes (UV-LEDs) performed as a light source. The crystallinity and luminescence were investigated using X-ray diffraction (XRD) and photoluminescence (PL) spectroscopy. Pure monoclinic Ba 2 ZnSi 2 O 7 and orthorhombic BaZn 2 Si 2 O 7 crystallize completely at 1100 o C. The doped Eu 2+ ions did not cause any significant change in the host structure. The emission spectra presented an emission position red shift of up to 16 nm from Ba 2 ZnSi 2 O 7 :Eu 2+ to BaZn 2 Si 2 O 7 :Eu 2+ . The excitation spectra of Ba 2 ZnSi 2 O 7 :Eu 2+ and BaZn 2 Si 2 O 7 :Eu 2+ were broad-banding, extending from 260 to 465 nm, which match the emission of UV-LEDs.

  20. Synthesis and crystal structures and luminescent properties of divalent europium-doped Ba{sub 2}ZnSi{sub 2}O{sub 7} and BaZn{sub 2}Si{sub 2}O{sub 7}

    Energy Technology Data Exchange (ETDEWEB)

    Yao Shanshan [State Key Laboratory of Materials Processing and Die and Mould Technology, College of Materials Science and Engineering, Huazhong University of Science and Technology, Wuhan 430074 (China); Xue Lihong, E-mail: xuelh@mail.hust.edu.c [State Key Laboratory of Materials Processing and Die and Mould Technology, College of Materials Science and Engineering, Huazhong University of Science and Technology, Wuhan 430074 (China); Yan Youwei [State Key Laboratory of Materials Processing and Die and Mould Technology, College of Materials Science and Engineering, Huazhong University of Science and Technology, Wuhan 430074 (China)

    2011-01-15

    The monoclinic Ba{sub 2}ZnSi{sub 2}O{sub 7}:Eu{sup 2+} blue-green-emitting phosphor and the orthorhombic BaZn{sub 2}Si{sub 2}O{sub 7}:Eu{sup 2+} green-emitting phosphor were prepared by combustion-assisted synthesis method as the fluorescent materials for ultraviolet-light-emitting diodes (UV-LEDs) performed as a light source. The crystallinity and luminescence were investigated using X-ray diffraction (XRD) and photoluminescence (PL) spectroscopy. Pure monoclinic Ba{sub 2}ZnSi{sub 2}O{sub 7} and orthorhombic BaZn{sub 2}Si{sub 2}O{sub 7} crystallize completely at 1100 {sup o}C. The doped Eu{sup 2+} ions did not cause any significant change in the host structure. The emission spectra presented an emission position red shift of up to 16 nm from Ba{sub 2}ZnSi{sub 2}O{sub 7}:Eu{sup 2+} to BaZn{sub 2}Si{sub 2}O{sub 7}:Eu{sup 2+}. The excitation spectra of Ba{sub 2}ZnSi{sub 2}O{sub 7}:Eu{sup 2+} and BaZn{sub 2}Si{sub 2}O{sub 7}:Eu{sup 2+} were broad-banding, extending from 260 to 465 nm, which match the emission of UV-LEDs.

  1. Synthesis, crystal structures and spectral properties of 6'-phenyl-2,2'-bipyridine derivatives and their CdLI(2) complexes.

    Science.gov (United States)

    Zhao, Xuesong; Chen, Yanxin; Luo, Junshan; Wang, Hui; Li, Shengli; Zhou, Hongping; Wu, Jieying; Tian, Yupeng

    2014-04-05

    Two novel 6'-phenyl-2,2'-bipyridine ligands (L1, L2) and their CdL(1,2)I2 complexes (1, 2) were synthesized and characterized by elemental analysis, (1)H NMR, IR, MALDI-TOF spectroscopy, and single crystal X-ray diffraction analysis. The results reveal that the central cadmium(II) atom in the complexes was coordinated by two iodide ions and two nitrogen atoms from L1, L2, forming a distorted coordination geometry. The electronic absorption properties of them were investigated on the basis of theoretical calculations (TD-DFT). Copyright © 2013 Elsevier B.V. All rights reserved.

  2. Shear induced structures in crystallizing cocoa butter

    Science.gov (United States)

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

    2004-03-01

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

  3. Modular crystals as modulated structures

    DEFF Research Database (Denmark)

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

    2008-01-01

    The use of the superspace formalism is extended to the description and refinement of the homologous series of modular structures with two symmetry-related modules with different orientations. The lillianite homologous series has been taken as a study case. Starting from a commensurate modulated c...

  4. Hydrothermal synthesis and crystal structure of a europium(III) coordination polymer with 5-sulfoisophthalate trivalent anions and free 4, 4'-bipyridine molecules

    International Nuclear Information System (INIS)

    Lin Humao; Qing Caixiao; Qian Miao; Ping Xiaohong

    2005-01-01

    A novel europium(III) coordination polymer [Eu(Sip)(H 2 O) 5 ] n · nH 2 O · 1.5 n(Bipy) (I) (Sip is 5-sulfoisophthalate trivalent anion and Bipy is 4,4'-bipyridine) is hydrothermally synthesized and determined by the single crystal X-ray diffraction method. Polymer I crystallizes in the monoclinic system, space group C2/c with a = 30.7515(6), b = 10.9577(2), c = 17.5545(4) A, β = 112.040(1) deg, Z = 4. In I, each Eu 3+ ion is coordinated by four oxygen atoms from two carboxylate groups of two different Sip anions and five oxygen atoms from five coordinated water molecules to complete a deformed mono-cap square antiprism. Moreover, each Sip anion acts as a tetradentate ligand to connect two adjacent Eu 3+ ions through its two chelating carboxylate groups, resulting in one-dimensional linear chains. In addition, fifteen different kinds of hydrogen-bonding interactions link the chains, lattice water molecules, and free Bipy molecules to engender a complicated hydrogen-bonding network [ru

  5. Construction of a 2D Co(II) Coordination Polymer with (4,4)-Connected Topology: Synthesis, Crystal Structure, and Surface Photo-electric Property

    Energy Technology Data Exchange (ETDEWEB)

    Li, Jiaming [Qinzhou Univ., Qinzhou (China)

    2014-04-15

    A 2D grid-like (4, 4)-connected topology coordination polymer, [Co(BTA){sub 2}(H{sub 2}O){sub 2}]{sub n}, where HBTA = 2-(1H-benzotriazol-1-yl)acetic acid, has been synthesized by hydrothermal method and characterized by single crystal X-ray diffraction, IR spectroscopy, elemental analysis and surface photovoltage spectroscopy (SPS). X-ray diffraction analyses indicated that displays octahedral metal centers with secondary building units (SBUs) [Co(BTA){sub 2}(H{sub 2}O){sub 2}] bridged by the BTA. ligands. In the crystal, the 2D supramolecular architecture is further supported by O-H···O, O-H···N, C-H···O hydrogen bonds and π··π stacking interactions. The SPS of polymer 1 indicates that there are positive response bands in the range of 300.600 nm showing photo-electric conversion properties. There are good relationships between SPS and UV-Vis spectra.

  6. 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.

  7. [UO2(NH3)5]Br2·NH3: synthesis, crystal structure, and speciation in liquid ammonia solution by first-principles molecular dynamics simulations.

    Science.gov (United States)

    Woidy, Patrick; Bühl, Michael; Kraus, Florian

    2015-04-28

    Pentaammine dioxido uranium(VI) dibromide ammonia (1/1), [UO2(NH3)5]Br2·NH3, was synthesized in the form of yellow crystals by the reaction of uranyl bromide, UO2Br2, with dry liquid ammonia. The compound crystallizes orthorhombic in space group Cmcm and is isotypic to [UO2(NH3)5]Cl2·NH3 with a = 13.2499(2), b = 10.5536(1), c = 8.9126(1) Å, V = 1246.29(3) Å(3) and Z = 4 at 123 K. The UO2(2+) cation is coordinated by five ammine ligands and the coordination polyhedron can be best described as pentagonal bipyramid. Car-Parrinello molecular dynamics simulations are reported for [UO2(NH3)5](2+) in the gas phase and in liquid NH3 solution (using the BLYP density functional). According to free-energy simulations, solvation by ammonia has only a small effect on the uranyl-NH3 bond strength.

  8. Synthesis and crystal structure of a new N-(2,6-dichlorobenzoyl)-N',N''-bis(pyrrolidinyl)-phosphoric triamide as a carrier and competitive bulk liquid membrane transport of six metal cations

    Czech Academy of Sciences Publication Activity Database

    Khoshnood, R.S.; Pourayoubi, M.; Kasraee, F.; Toghraee, M.; Dušek, Michal; Bereciartua, P.J.

    2014-01-01

    Roč. 88, č. 12 (2014), s. 2146-2156 ISSN 0036-0244 Institutional support: RVO:68378271 Keywords : organic membrane * ionic transport * crystal structure Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.562, year: 2014

  9. 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.

  10. The crystal structure of thiourea nitrate

    NARCIS (Netherlands)

    Feil, D.; Song Loong, W.

    1968-01-01

    The structure of thiourea nitrate has been determined by three-dimensional X-ray methods. Both Cu Ke and Mo K~ data were obtained with a single-crystal diffractometer and the final R values are 4.9% and 5.5% respectively. The space group is P211m and there are two molecules in the unit cell. All

  11. Crystal structure from one-electron theory

    DEFF Research Database (Denmark)

    Skriver, H. L.

    1985-01-01

    by the 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...

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

    International Nuclear Information System (INIS)

    Serna, Pedro Vera; Campos, Cecilio Garcia; De Jesus, Felix Sanchez; Miro, Ana Maria Bolarin; Loran, Jose Antonio Juanico; Longwell, Jeffrey

    2016-01-01

    Neodymium orthoferrite NdFeO 3 was obtained at room temperature by mechanosynthesis with a stoichiometric ratio of Nd2O 3 and Fe 2 O 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 3 was detected after a few hours of milling, indicating that the milling imparted mechanical energy to the system. (author)

  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. Transition metal complexes with thiosemicarbazide-based ligands. Part 45. Synthesis, crystal and molecular structure of [2,6-diacetylpyridine bis(S-methylisothiosemicarbazonato]diazide-iron(III

    Directory of Open Access Journals (Sweden)

    REFIK FAZLIC

    2003-05-01

    Full Text Available The template reaction of a warm methanolic solution of FeCl3.6H2O, S-methylisothiosemicarbazidehydroiodide and 2,6-diacetylpyridine in the presence of LiOAc and NaN3 yielded the high-spin complex [Fe(HL(N32], were HL is the monoanion of the ligand 2,6-diacetylpyridine bis(S-methylisothiosemicarbazone. X-Ray analysis of the complex showed its pentagonal-bipyramidal configuration, with pentadenate (N5 HL in the equatorial plane and two monodentate azide groups in the axial positions. Crystal data are: monoclinic, P21/c, a = 1.0263(2, b = 1.2525(2, c = 1.6660(3 nm, b = 98.94°, V = 2.1154 nm3, Z = 4, rx = 1.499 g cm-3, r0 = 1.48 g cm-3, F(000 = 984, m = 9.40 cm-3.

  15. SYNTHESIS, CRYSTAL STRUCTURE AND LUMINESCENT PROPERTY OF A DINUCLEAR Tb(II COMPLEX WITH HOMOPHTHALIC ACID AND 2,2’-BIPYRIDYL

    Directory of Open Access Journals (Sweden)

    LI-HUA WANG

    2015-07-01

    Full Text Available A novel dinuclear Tb(III complex, [Tb(bpy2L2] (bpy = 2,2’-bipyridine, H2L = homophthalic acid, has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction. The Tb(III complex is monoclinic, space group P21/c with a = 9.368(2 Å, b = 15.948(4 Å, c = 12.216(3 Å, β = 103.023(4º, V= 1778.2(7 Å3, Z = 2, Dc = 1.910 mg·m-3, μ = 4.011 mm-1, F(000 = 996, and final R1 = 0.0602, ωR2 = 0.2192. The result shows that the Tb(III center is seven-coordination with a N2O5 distorted pengonal bipyramidal geometry. The luminescent property of Tb(III complex was investigated.

  16. 1.2.2.Synthesis, crystal structure and in vitro anti-tumor activity of dibutyltin complex of 2,4-dichloro-5-fluorobenzoic acid

    Directory of Open Access Journals (Sweden)

    Ming Li, Liqin Wang, Zhenlei Zhang, Yue Xin, Laijin Tian*

    2014-04-01

    Full Text Available The dibutyltin complex of 2,4-dichloro-5- fluorobenzoic acid, [(2,4-Cl2 -5-FC6 H2 C(OOSnBu2 2 O]2 (Bu = CH2 CH2 CH2 CH3 (1 , has been synthesized and characterized by elemental analysis, FT-IR, 119 Sn NMR spectroscopy, and Xray single crystal diffraction. Compound 1 is a centrosymmetric dimmer with two distinct types of carboxylate moieties and tin atoms with distorted trigonal bipyramidal geometries. The in vitro  anti-tumor activity of 1 against two human tumor cell lines was found to be higher than that for cis-platin [cis diaminedichloroplatinum( II] used clinically. Supporting information : FT-IR, 119 Sn NMR, X-Ray, Proliferation inhibitory rate, Cif file.

  17. Synthesis and crystal structure of a new pyridinium bromide salt: 4-methyl-1-(3-phen-oxy-prop-yl)pyridinium bromide.

    Science.gov (United States)

    Said, Musa A; Aouad, Mohamed R; Hughes, David L; Almehmadi, Meshal A; Messali, Mouslim

    2017-12-01

    In the cation of the title mol-ecular salt, C 15 H 18 NO + ·Br - , the pyridinium and phenyl rings are inclined to one another by 11.80 (8)°. In the crystal, the Br - anion is linked to the cation by a C-H⋯Br hydrogen bond. The cations stack along the b -axis direction and are linked by further C-H⋯Br inter-actions, and offset π-π inter-actions [inter-centroid distances = 3.5733 (19) and 3.8457 (19) Å], forming slabs parallel to the ab plane. The effects of the C-H⋯ X - inter-action on the NMR signals of the ortho- and meta- pyridinium protons in a series of related ionic liquids, viz . 4-methyl-1-(4-phen-oxy-but-yl)pyridin-1-ium salts, are reported and discussed.

  18. Synthesis, spectral characterization and catalytic activity of Co(II) complexes of drugs: Crystal structure of Co(II)-trimethoprim complex

    Science.gov (United States)

    Madhupriya, Selvaraj; Elango, Kuppanagounder P.

    2014-01-01

    New Co(II) complexes with drugs such as trimethoprim (TMP), cimetidine (CTD), niacinamide (NAM) and ofloxacin (OFL) as ligands were synthesized. The complexes were characterized by analytical analysis, various spectral techniques such as FT-IR, UV-Vis, magnetic measurements and molar conductivity. The magnetic susceptibility results coupled with the electronic spectra suggested a tetrahedral geometry for the complexes. The coordination mode of trimethoprim ligand and geometry of the complex were confirmed by single crystal X-ray studies. In this complex the metal ion possesses a tetrahedral geometry with two nitrogen atom from two TMP ligands and two chloride ions coordinated to it. The catalytic activity of the complexes in aryl-aryl coupling reaction was screened and the results indicated that among the four complexes [Co(OFL)Cl(H2O)] exhibited excellent catalytic activity.

  19. Synthesis and crystal structure of Mg0.5NbO2: An ion-exchange reaction with Mg2+ between trigonal [NbO2]- layers

    Science.gov (United States)

    Miura, Akira; Takei, Takahiro; Kumada, Nobuhiro

    2013-01-01

    A new layered niobate, Mg0.5NbO2, was synthesized from LiNbO2 through a cation-exchange reaction with Mg2+ at 450-550 °C. This is the first example of a topotactic reaction with an aliovalent cation between trigonal [NbO2]- layers. It is proposed to be isostructural with LiNbO2 (space group; P63/mmc) with lattice parameters of a=2.9052(6) Å, c=10.625(15) Å. The lattice parameters and formation energy of Mg0.5NbO2 crystallized in LiNbO2 form and other layered CaNb2O4 one were calculated by density functional theory.

  20. Synthesis and crystal structure of 4-fluorobenzylammonium dihydrogen phosphate, [FC6H4CH2NH3]H2PO4

    Directory of Open Access Journals (Sweden)

    Ali Rayes

    2016-12-01

    Full Text Available The asymmetric unit of the title salt, [p-FC6H4CH2NH3]+·H2PO4−, contains one 4-fluorobenzylammonium cation and one dihydrogen phosphate anion. In the crystal, the H2PO4− anions are linked by O—H...O hydrogen bonds to build corrugated layers extending parallel to the ab plane. The FC6H4CH2NH3+ cations lie between these anionic layers to maximize the electrostatic interactions and are linked to the H2PO4− anions through N—H...O hydrogen bonds, forming a three-dimensional supramolecular network. Two hydrogen atoms belonging to the dihydrogen phosphate anion are statistically occupied due to disorder along the OH...HO direction.