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Hydrothermal Synthesis, Crystal structure and Magnetic Property of a Novel Mixed Valence Decatungstate: [Cu(2,2′-bipy)_2]_2Na_2W_6~VW4^(VI)O_(30)·2H_2O

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Chinese Journal of Structural Chemistry 2008年第1期27卷 57-62页

作者：李涛海吕健高水英曹荣 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter The Chinese Academy of Sciences

A novel Cu（II）-2,2＇-bipy-supported （bipy = bipyridine） mixed valence decatungstate, [Cu（2,2＇-bipy）2]2Na2W6^VW4^VIO30·2H2O 1, has been synthesized and structurally characterized by X-ray analysis. The crystal of 1 is of triclinic, space group P1^- with a= 10.9393（10）, b = 12.0492（2）, c = 12.3783（2）A, a = 80.631（10）, β= 70.226（10）, γ= 72.329（9）^o, V = 1459.64（4）A^3, Z = 1, Dc = 3.582 g/cm^3, F（000） = 1404, R = 0.0553 and wR = 0.1242 for 4607 observed reflections （I 〉 2σ（I））. The EPR spectrum of 1 indicates that its unpaired electrons are placed in the dx2-y2 orbital of the ground state of Cun. Furthermore, compound 1 shows an antiferromagnetic interaction.

关键词： crystal structure decatungstate mixed valence magnetic property

A Novel Hybrid Solid Constructed from Tetramolybdate and Copper Complexes with Mixed Ligands: [{(Cu·phen)_2(tp)}{(Cu·phen·H_2O)_2(tp)}{Mo_4O_(14)}]

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Chinese Journal of Structural Chemistry 2007年第4期26卷 389-394页

作者：吴小园翟全国陈丽娟杨文斌卢灿忠 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter The Chinese Academy of Sciences

A novel copper molybdate with mixed ligands, [{（Cu·phen）e（tp）} {（Cu·phen·H2O）2（tp）} {Mo4O14}（phen = 1,10-phcnanthroline, tp = tercphthalate） 1, has been hydrothermally synthesized and structurally characterized. The crystal belongs to monoclinic system, space group P2l/c with a = 13.1711（7）, b = 19.6132（10）, c= 13.6910（7） A, β = 117.6870（10）°, V= 3131.8（3） A^3, Z= 2, C64H44Cu4MoaN8O24, Mr= 1946.99, D, = 2.065 g/cm^3, F（000） = 1920,μ（MoKa） = 2.198 mm ^1, R = 0.0810 and wR = 0.2012 for 4233 observed reflections （I 〉 2σ（I））. The structural analysis indicates that the title compound contains a discrete tetramolybdate cluster decorated with copper colnplcx fragments and tp ligands bridging the clusters into a wave-like layer. The hydrogen bonding between adjacent layers further extends the COlnpound into a 3-D framework.

关键词： polyoxometalate I,10-phenanthroline terephthalate,tetramolybdate cluster crystal structure

Self-assembly of Quasi-monocrystal CdCO_3 Nanorings

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Chinese Journal of Structural Chemistry 2007年第7期26卷 757-762页

作者：王朝明程遥王元生包峰 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter The Chinese Academy of Sciences

Hierarchical CdCO3 nanostructures with complex morphologies, such as tetragonal, pentagonal and hexagonal nanorings, can be prepared via self-assembly of nanocrystals in a solvothermal environment. XRD pattern indicated that the product is trigonal CdCO3 phase （PDF#850989） with cell constants a = 6.112 A and a = 47.4°. Based on our experimental results, a possible nanoring formation mechanism was proposed.

关键词： nanorings self-assembly solvothermal

Growth and Spectral Characteristics of Yb^(3+)-doped LiGd(MoO_4)_2 Crystal

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Chinese Journal of Structural Chemistry 2010年第6期29卷 853-860页

作者：黄新阳王国富 institute of research on the Functional Materials Jiangxi University of Finance and Economy institute of research on the structure of matter Chinese Academy of Sciences

The Yb3＋-doped LiGd（MoO4）2 crystal with the size up to Φ20×30 mm3 has been grown by Czochralski *** polarized room temperature absorption and emission spectra have been *** crystal exhibits a broad absorption band centered at 975 nm with an FWHM of 43 and 59 nm for π-and σ-polarization,respectively,and the corresponding maximal absorption cross-sections are 3.36 and 2.42×10-20 *** emission broadband has an FWHM of 47 and 54 nm for π-and σ-polarization,respectively,with the corresponding emission cross sections of 3.92 and 3.34 × 10-20 cm2 at 1020 *** measured fluorescence lifetime is 287 μs.

关键词： optical microscopy growth from melt molybdate solid state laser materials

Two Novel Zinc Compounds with in situ Formation of Dimethylamine Ligand

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Chinese Journal of Structural Chemistry 2008年第6期27卷 667-672页

作者：刘玺吴阿清郭国聪 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of MatterThe Chinese Academy of Sciences

The investigation of the supramolecular interactions between the zinc chloride salts and the crown ether in tetrahydrofuran （THF） with the diffusion of in situ formed DMA （DMA = dimethylamine） ligand leads to two novel zinc-DMA compounds, [（H3O）·（18C-6）][ZnCl3（DMA）] 1 and [（HDMA）·（18C-6）][ZnCl3（DMA）] 2 （18C-6 = 18-crown-6）, whose emissions fall into the blue-emission field. Crystal data for compound 1： monoclinic, space group P21/c, a = 8.753（1）, b = 14.538（2）, c = 19.969（3）A, β = 110.121（7）°, V = 2386.2（5）A^3, T = 293（2） K, Z = 4, Mr = 500.14, Dc= 1.392 g/cm^3,μ = 1.395 mm^-1, F（000） = 1048, S = 1.006, R = 0.0611 and wR = 0.1755 for 3676 observed reflections with I 〉 2σ（I） and 235 parameters. For 2： triclinic, space group P1^-, a = 9.2672（4）, b = 11.8778（2）, c = 13.3846（1） A, a = 67.09（1）, β = 75.54（2）, ）,γ = 81.32（2）°, V = 1311.74（6） A^3, T = 293（2） K, Z = 2, Mr = 527.21, Dc = 1.335 g/cm^3,μ = 1.271 mm^-1, F（000） = 556, S = 1.006, R = 0.0393 and wR = 0.1034 for 3839 observed reflections with I〉 2σ（I）.

关键词： zinc compound in situ crystal structure blue-emission

Growth,Band structure and Optical Properties of LiSrBO_3 Crystal

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Chinese Journal of Structural Chemistry 2007年第10期26卷 1165-1170页

作者：龚亚京吴东升程文旦张浩陈达贵张永春阚子规 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of MatterThe Chinese Academy of Sciences

The bulk crystal of LiSrBO3 （8.39 g） with a size of 21mm × 20mm × 15mm was grown by high temperature solution growth method. The relationship between growth habit and crystal structure was discussed. The transmission spectrum shows an UV absorption edge at about 300 nm. The melting temperature of this crystal was detemained to be 942 ℃ by DTA-TG measurement. The band structure of the LiSrBO3 crystal was studied by means of the first principle method. An indirect band gap was found to be about 4.0 eV, and a low dielectric constant was estimated to be about 1.9 in terms of theoretical results.

关键词： high temperature spectrum band structure

Syntheses and Crystal structures of Two New Iron-sulfur Carbonyl Complexes: [Fe_2(SC_6H_4Cl)_2(CO)_6]·0.5(Et_2O) and [Fe_3(SC_6H_4NH_2)_6(CO)_6]·2(MeOH)

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Chinese Journal of Structural Chemistry 2006年第3期25卷 326-332页

作者：马成丙陈昌能刘秋田 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter The Chinese Academy of Sciences

Two new iron-sulfur carbonyl complexes, [Fe2（SC6H4Cl）2（CO）6]·0.5（Et2O） 1 and [Fe3（SC6H4NH2）6（CO）6]·2（MeOH） 2, have been prepared and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. Crystal data for 1： monoclinic, C2/c, a = 18.4439（8）, b = 11.0999（5）, c = 25.1830（10）A°, β = 97.0370（10）°, V = 5116.8（4） A°^3, Z = 8, C20H13Cl2Fe2O6.50S2, Mr = 604.02, Dc = 1.568 g/cm^3, μ = 1.540 mm^-1, F（000） = 2424, the final R = 0.0545 and wR = 0.1454 for 3443 observed reflections with I 〉 2σ（I）; 2： monoclinic, P21/n, a = 12.350, b = 26.3050（11）, c = 16.057A°, β = 97.891 （3）°, V = 5166.9（2）A°^3, Z = 4, C44H44Fe3N6O8S6, Mr = 1144.76, Dc = 1.472 g/cm^3, μ = 1.128 mm^-1, F（000） = 2352, the final R = 0.0442 and wR = 0.1197 for 7978 observed reflections with I 〉 2σ（I）. Complex 1 contains one iron dimer, in which two tricarbonyliron（Ⅰ） fragments are bridged together by two 4-chlorophenylthiolate ligands, whereas complex 2 contains a linear tri-iron cluster, in which two terminal tricarbonyliron（Ⅱ） fragments and the central Fe（Ⅱ） atom are linked together by six 4-aminophenylthiolate bridging ligands.

关键词： iron-sulfur carbonyl complex thiophenol synthesis crystal structure

Growth Units and Formation Mechanisms of the Crystals Under Hydrothermal Conditions

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Science China Chemistry 1994年第11期37卷 1288-1297页

作者：仲维卓刘光照施尔畏华素坤唐鼎元赵庆兰 Shanghai institute of Ceramics Academia SinicaShanghai 200050PRC Fujian institute of research of the structure of matter Academia SinicaFuzhou 350002PRC Fujian institute of research on the structure of matter Academia SinicaFuzhou 350002PRC

The growth units and formation mechanisms of quartz(SiO_2)and barium titanate (BaTiO_3)crystals under hydrothermal conditions have been investigated by means of cataphoretic experi- *** is proposed that the growth units of the crystals in hydrothermal solutions have the structures of coordinative polyhedra of anions,which correspond to those of coordinative polyhedra in the crystals. The relationship between crystal morphology and physico-chemical conditions has been explained accord- ing to the modes of incorporation of the coordinative polyhedra of anions on the various faces of crystals. The dimensions of the growth units vary with the change of the growth *** incorporation rates on the various faces of the growth units with varied dimensions must be different,which leads to a satis- factory explanation for the variety of the crystal morphology.

关键词： growth unit coordinative polyhedra of anion crystallization habit

Syntheses, Crystal structures and Magnetism of Two New Coordination Polymers [Ni(bix)_2Cl_2]_n and [Co(bix)Cl_2]_n

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Chinese Journal of Structural Chemistry 2007年第6期26卷 711-716页

作者：周慧杜少武 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter The Chinese Academy of Sciences

The self-assembly reactions of M^ⅡCl2 （M = Ni, Co） with the flexible bix ligand [bix = 1,4-bis（imidazole-1-ylmethyl）benzene] yielded a 2D network [N^Ⅲ（bix）2Cl2]n 1 and a 1D chain [Co^Ⅱ（bix）Cl2]n 2. Their crystal structures have been determined by X-ray single-crystal diffraction analysis. Complex 1 characters a two-dimensional grid-type structure and crystallizes in monoclinic, space group P21/c with a = 7.7231（7）, b = 12.7787（9）, c = 13.9374（13）A, β = 105.419（4）°, C28H28Cl2N8Ni, Mr = 606.19, Ζ = 2, V = 1326.0（2）A^3, Dc = 1.518 g/cm^3, μ = 0.969 mm^-1, F（000） = 628, R = 0.0429 and wR = 0.0783 for 2503 observed reflections （Ⅰ〉 2σ（Ⅰ））. Compound 2 is a one-dimensional chain and crystallizes in orthorhombic, space group Pbca with a = 11.3696（6）, b = 10.2128（6）, c = 14.4943（9）（A）, C14H14Cl2CoN4, Mr = 368.12, Z = 4, V = 1683.01（17）A^3, Dc = 1.453 g/cm^3, μ = 1.334 mm^-1, F（000） = 748, R = 0.0317 and wR = 0.0800 for 1778 observed reflections （Ⅰ〉 2σ（Ⅰ））. Magnetic properties of the title complexes were also investigated.

关键词： bix magnetic property non-rigid ligand crystal structure