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Chinese Journal of Structural Chemistry 2006年第7期25卷 830-836页

作者： LIU Hong-Sheng CHEN Yan-Hui PENG Jun SHI Zhen-Yu DONG Bao-Xia KONG Yu-Mei Institute of Polyoxometalate Chemistry Department of Chemistry Northeast Normal University Changchun Jilin 130024 China Department of Chemzstry Suihua University Suihua Heilongjiang 152061 China

A new compound [Cu（I）（phen）2]5[HV15O36（Cl）]0.65[H3V16O38（Cl）]0.35·2H2O 1 （phen = 1,10′-phenanthroline） has been prepared from the hydrothermal reaction of V2O5, CuCl, phen, H2C2O4·2H2O, THMAM （tris（hydroxymethyl）aminomethane） and H2O in the molar ratio of 3：1：1：0.5：2.5：1400. Compound 1 crystallizes in the space group P42212 of the tetragonal system with a = b = 21.5009（8）, c = 28.401（2） A, V= 13129.5（12） A^3 Z = 4, Dc = 1.800 g/cm^3, μ（MoKa） = 1.932 mm^-1, λ（MoKa） = 0.71073 A, F（000） = 7063.4, C120H81.20ClCu5N20O38.7V15.35, Mr = 3557.58, the final R = 0.0594 and wR= 0.1320 for 7761 observed reflections （I 〉 2σ（I））. Structure analysis shows that 1 exhibits a 3D channel framework formed by the supramolecular assembly of Cu complexes and polyoxovanadate clusters via intermolecular hydrogen bonding, and the channels contain Cu complexes. Other characterizations by elemental analysis, XPS, IR, XRD and thermal analysis are also described.

关键词： hydrothermal synthesis crystal structure polyoxovanadate supramolecular assembly

hydrothermal synthesis,Crystal Structure and Spectral Characterization of a New Copper Isopolytungstate: [Cu(phen)_3][W_6O_(19)]

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Chinese Journal of Structural Chemistry 2006年第7期25卷 837-843页

作者： MENG Fan-Xia LIU Kun CHEN Ya-Guang Institute of Polyoxometalate Chemistry Faculty of Chemistry Northeast Normal University Changchun 130024 China

An unusual inorganic-organic hybrid hexatungstate complex [Cu（phen）3][W6O19] 1 （C36H24 CuN6O19W6, Mr= 2011.20） was hydrothermally synthesized and characterized by singlecrystal X-ray diffraction, IR spectrum, UV-VIS spectrum and elemental analyses. This compound crystallizes in the monoclinic system, space group C2/c with a = 19.1005（11）, b = 11.2585（11）, c = 20.2867（15） A, β= 102.177（2）°, V= 4264.4 A^ 3, μ（MoKa） = 16.691 mm^-1, Dc = 3.133 g/cm^3, Z = 4, F（000） = 3628, the final R = 0.0338 and wR = 0.0798 for 4090 observed reflections with I 〉 2σ（I）. The result of structure determination shows that the crystal structure is constructed from [W6O19]^2- cluster anions and [Cu（phen）3]^2＋ complex fragments, which are held together into a three-dimensional network through hydrogen-bonding interactions.

关键词： hydrothermal synthesis tungstates polyoxometalates copper coordination complexes

hydrothermal synthesis and Crystal Structure of a New Hexa-cobalt-containing POM

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Chinese Journal of Structural Chemistry 2008年第8期27卷 943-948页

作者：傅春花郑寿添杨国昱 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter The Chinese Academy of SciencesFuzhou Fujian 350002 China

A new compound Na3H3[Co（en）3]2[Co4（H2O）2（PW9O34）2]·11H2O 1 （en = ethylenediamine） has been synthesized under hydrothermal conditions and characterized by IR, TGA, and single-crystal X-ray diffraction analysis. Crystal data： monoclinic, space group C21c, a = 26.336（5）, b = 18.135（2）, c = 22.751（4）A, β = 123.039（7）° and Z = 4. X-ray crystallographic study on compound 1 reveals that it includes a Weakley-type sandwich polyoxoanion [Co4（H2O）2（PW9O34）2]^10-, two complex ions [Co（en）3]^2＋, three Na^＋ ions （one Na（1） and two Na（2））, and eleven crystallographic water molecules. The sandwich polyoxoanions are linked by Na2 to form 2D layers parallel to the （100） plane, and these layers are further connected by Nal along the α-axis to generate a 3D structure.

关键词： polyoxometalate Keggin cobalt hydrothermal synthesis crystal structure

hydrothermal synthesis,Crystal Structure and Magnetic Properties of a Cobalt(II) Coordination Polymer Assembled by 4-Sulfophthalate and 4,4'-Bipyridine

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Chinese Journal of Structural Chemistry 2006年第11期25卷 1369-1374页

作者： WANG Qing-Wei LI Xiu-Mei HAN Jing College of Chemistry. dilin Normal University Siping 136000 China Department of Chemistry. Tonghua Teachers College Tonghua 134002 China College of Chemistry Jilin University Changchun 130023 China

A novel metal-organic coordination polymer {[Co2（4-sphth）2（4,4＇-bpyh（H2O）4]- [Co（4,4＇-bpy）2（H2O）4]}, （4-sphth = 4-sulfophthalic acid, 4,4＇-bpy = 4,4＇-bipyridine） 1 has been hydrothermally synthesized and structurally characterized by single-crystal X-ray diffraction, elemental analyses, IR spectroscopy, and magnetic susceptibility measurements. The complex crystallizes in monoclinic, space group C2/c with a = 18.893（6）, b = 23.080（7）, c = 22.473（7） A, fl = 107.311 （4）°, V = 9356（5） A^3, C76H70Co3N12O22S2, Mr = 1744.35, De = 1.238 g/cm^3,μ（MoKα） = 0.640 mm^-1, F（000） = 3596, Z = 4, the final R = 0.0444 and wR = 0.0846 for 9178 observed reflections （I 〉 2σ（I））. It exhibits a novel three-dimensional supramolecular network formed by hydrogen-bonding and π-π interactions. Variable-temperature magnetic measure shows an overall anti-ferromagnetic behavior for compound 1.

关键词： hydrothermal synthesis supramolecular network magnetic properties

hydrothermal synthesis and characterization of nano-petal nickel hydroxide

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Rare Metals 2015年第9期34卷 667-672页

作者： Wen-Xiu He Yong-Qiang Zhang Qian-Qing Liang Wen-Quan Jiang Hai-Feng Sun School of Chemistry Engineering Inner Mongolia University of Science and Technology Analysis & Measurements Research Center General Rearch Institute for Non-Ferrous Metals

The current article reports a preparation method of nano-petal nickel hydroxide, which was synthesized using urea as a precipitator by hydrothermal method. Nickel hydroxide samples with different microstructural characteristics were prepared by changing molar ratio of nickel/urea and reaction time. The prepared nickel hydroxide samples were characterized using X-ray diffraction(XRD) and scanning electron micrography(SEM).Electrochemical performances of the samples were then determined under charging–discharging rate of 0.2C. The influences of different conditions of the hydrothermal synthesis method on microstructure parameters of nickel hydroxide were analyzed, while relationships between microstructural characteristics parameters of nickel hydroxide and the electrochemical performances of nickel electrode were also explored.

关键词： hydrothermal synthesis Nano-petal Electrochemical

hydrothermal synthesis and Characterization of a Novel Organically-templated Tungsten Heteropolyacid with a Microporous Structure

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Chinese Journal of Structural Chemistry 2005年第4期24卷 429-435页

作者： LIUWei CHENHao-Hong YANGXin-Xin ZHAOJing-Tai StateKeyLaboratoryofHighPerformanceCeramicsandSuperfineMicrostructure ShanghaiInstituteofCeramicsTheChineseAcademyofSciencesShanghai200050China

A microporous organically-templated tungsten heteropolyacid, (C2N2H10)2 [H2P2W18O62]?8H2O, with a new type was hydrothermally synthesized by using ethylenediamine as the structure-directing agent. Its structure was determined by single-crystal X-ray diffraction analysis. Crystal data: monoclinic, space group P21/c, a = 14.633(4), b = 19.432(5), c = 26.776(5) ?, β = 117.849(11)o, V = 6732(3) ?3, Z = 4, Mr = 4615.48, Dc = 4.554 g/cm3, μ(MoKα) = 30.781 mm-1, F(000) = 7976, the final R = 0.0678 and wR = 0.1359. The crystal of the title compound is constructed by Dawson anions and organic dications forming a novel “hollow” channel system.

关键词： hydrothermal synthesis crystal structure tungsten heteropolyacids organically templated

hydrothermal synthesis and characterization of two novel inorganic-organic hybrid materials

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Journal of Zhejiang University-Science A(Applied Physics & Engineering) 2008年第1期9卷 143-148页

作者： Zeng-he LI Hai-dan BAI College of Science Beijing University of Chemical Technology Beijing 100029 China China National Chemical Information Center Beijing 100029 China

By using different organic ligands, two 3D inorganic-organic hybrid compounds Co（C4H4N2）（VO3）2 1 and Co（C12H12N2）（VO3）2 2 were synthesized by hydrothermal reaction and characterized by X-ray crystallography. Crystal data： 1. crystal system orthorhombic, space group Pnna, a=1 0.188（2） A, b=1 1.497（2） A, c=7.3975（15） A, V=866.5（3） A^3, Z=4, Dcalcd= 2.705 g/cm^3; 2. crystal system triclinic, space group P1^- （No. 2）, a=8.3190（17） A, b=8.4764（17） A, c=1 1.183（2） A, a=95.48（3）°, β=92.03（3）°, γ=107.24（3）°,V=748.0（3） A^3, Z=2, Dcalcd= 1.958 g/cm^3. The framework of compound 1 contains both {Co（C4H4N2）} and infinite metavanadate chains. Crystal structure of compound 2 is constructed with inorganic {CoV2O6} layers across-linked by organic 1,2-bis（4-pyridyl） ethane ligands. The two compounds are thermally stable to approximately 410 ℃ and 350 ℃, respectively. Their optical band gaps are determined to be 2.13 eV and 2.12 eV by UV-VIS-NIR diffuse reflectance spectra, which revealed their nature of semiconductor and optical absorption features.

关键词： Inorganic-organic hybrid materials hydrothermal synthesis Crystal structure Oxovanadium

hydrothermal synthesis,Crystal Structure and Electrochemical Properties of the Copper(II) Complex [Cu_4O_4(phen)_4(ClC_6H_4COO)_2(H_2O)_2]·(H_2O)_3

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Chinese Journal of Structural Chemistry 2006年第11期25卷 1331-1336页

作者： LI Wei LI Chang-Hong YANG Ying-Qun KUANG Yun-Fei Department of Chemistry and Materials Science Hengyang Normal University Hengyang 421008 China Department of Chemical Engineering Hunan Institute of Technology Hengyang 421008 China

The title complex of copper（Ⅱ） with m-chlorobenzoic acid, 1,10-phenanthroline （phen） and copper perchlorate has been synthesized and characterized in the solvent mixture of water and methanol. Crystal data for this complex： triclinic, space group PI^-, a = 1.06853（12）, b = 1.30740（16）, c = 1.49546（17） nm, α= 101.791（2）,β = 103.413（2）, γ = 105.815（2）°, V= 1.8736（4） nm^3, Mr = 904.67, Dc = 1.604 g/cm^3, Z = 2,/7（000） = 924,μ = 1.34 mm^-1, GOOF = 1.049, the final R = 0.0324 and wR = 0.0797. The structure analysis shows that a chair-like structure [Cu4O4] is defined by three quadrilaterals shaped by four copper and four oxygen atoms, and every copper ion is coordinated by three oxygen atoms from three wate： molecules and two nitrogen atoms from one 1,10-phenanthroline molecule, giving a distorted square-pyramidal coordination geometry. The CV analysis results indicate that the electron transfer in the electrode reaction is quasi-reversible.

关键词： copper(Ⅱ) complex hydrothermal synthesis electrochemical property

hydrothermal synthesis and structural studies of a new coordination polymer of lanthanum(Ⅲ) with benzene-1,2,4,5-tetracarboxylic acid and 4,4′-bipyridine

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Journal of Rare Earths 2009年第3期27卷 357-362页

作者： Masoumeh Tabatabaee Mahboubeh A. Sharif Fatemeh Vakili Saina Saheli Department of Chemistry Islamic Azad University Yazd Branch Department of Chemistry Islamic Azad University Qom Branch

A new lanthanum complex formulated as {（bpyH2）[La（btc）（H2O）4（NO3）]·2H2O}n （1）（btcH4=benzene-1,2,4,5-tetracarboxylic acid; bpy=4,4＇-bipyridine） was hydrothermally synthesized. The complex was characterized by FT-IR spectroscopy, elemental analysis and X-ray diffraction. X-ray crystal structural analysis revealed that the compound belonged to the monoclinic space group C2/c with cell parameters a= 1.42806（7） nm, b=1.10258（5） nm, c=1.60333（8） nm and β=101.9400（10）°. The complex was polymeric with La^III atoms linked by four O atoms from two carboxylate groups of one benzene-1,2,4,5-tetracarboxylate. The LaIn atom was ten coordinated in a distorted tetracapped trigonal prism. In the crystal structure, a wide range of noncovalent interactions consisting of hydrogen bonding （of the types of O-H…O, N-H…O and C-H…O） and ion pairing interactions connected the various components into a supramolecular structure.

关键词： lanthanum(III) complex hydrothermal synthesis coordination polymer hydrogen bonding benzene-1,2,4,5-tetracarboxylic acid rare earths

hydrothermal synthesis of vanadium oxide nanotubes by a facile route

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Rare Metals 2006年第Z1期25卷 88-93页

作者： HUANG Chunming LIU Xueqin KONG Lingbin ZHOU Haijia LIU Yaqiang QIU Jiawen WANG Yinyue Department of Physics Lanzhou University Lanzhou 730000 China Department of Physics Lanzhou University Lanzhou 730000 China Lanzhou Institute of Physics Lanzhou 730000 China State Key Laboratory of Gansu Advanced Non-Ferrous Metal Materials Lanzhou University of Technology Lanzhou 730050 China Department of Physics Lanzhou University Lanzhou 730000 China Department of Physics Lanzhou University Lanzhou 730000 China Lanzhou Institute of Physics Lanzhou 730000 China Department of Physics Lanzhou University Lanzhou 730000 China

Vanadium oxide nanotubes were synthesized by hydrothermal treatment from V2O5·nH2O sols as precursor and dodecylamine as structure-directing template. The morphology and structure of the nanotubes were characterized by SEM, TEM, XRD, TG-DTA and FTIR. The experimental results reveal that the duration of the hydrothermal treatment is of importance for obtaining VOx-NTs which have a layered structure. TG-DTA study indicates that V5+ cations in nanotubes are partially reduced to V4+ cations. The results from FTIR spectra indicate the difference in V-O vibrations between before and after hydrothermal treatment. From the results, it suggests that during hydrothermal treatment, the rearrangement of the vanadium oxide structure leads to the formation of VOx nanotubes from lamellar structure because of the presence of V4+ species.

关键词： vanadium oxide nanotubes hydrothermal synthesis V2O5 sols