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π-π Stacking Force in the Solid structure of Mixed-Metal Complexes: Zn(phen)_2MS_4 (M=W, Mo)

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Chinese Journal of Structural Chemistry 2001年第6期20卷 481-485页

作者：王庆华郭国聪等 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences

The inter-diffusion of N,N-dimethylformamide solution of Zn(phen)2Cl2 and (NH4)2MS4 (M = W, Mo) in an H-shape tube produced crystals of Zn(phen)2WS4 1 and Zn(phen)2MoS4 2 (phen = 1,10-phenanthroline). The structures of isomorphous complexes 1 and 2 have been determined by X-ray single-crystal structure analyses. Four nitrogen atoms from the phenanthroline ligands and two sulfur atoms from the MS42- anion forming a distorted octahedron coordinate each zinc atom. Through p-p interactions of adjacent aromatic rings of the phenanthroline ligands, a quasi one-dimensional zigzag-stacking column is formed in each complex. Complex 1 crystallizes in monoclinic space group C2/c, with a = 10.447(8), b = 22.016(9), c = 12.824(8) ? b = 103.56(6)? V = 2867.7(8) 3, Z = 4, C24H16N4S4WZn, Mr=737.90, Dc = 1.71 g/cm3, F(000) = 1424, m = 5.25 mm-1, the final R = 0.054 and Rw = 0.075 for 2315 observations with I > 3s (I). Complex 2 crystallizes in monoclinic space group C2/c, with a = 10.410(6), b = 22.095(7), c = 12.830(6) ? b = 103.19(8)? V = 2873.1(5) 3, Z = 4, C24H16MoN4S4Zn, Mr=649.99, Dc = 1.50 g/cm3, F(000) = 1296, m = 1.58 mm-1, the final R = 0.072 and Rw = 0.100 for 1631 observations with I > 3s(I).

关键词： synthesis crystal structure p-p interaction zinc-molybdenum zinc-tungsten

Synthesis,structure and Fluorescent Property of a Novel 2-D Sheet Inorganic-organic Hybrid Cadmium Polymer [CdBr_2(bpdo)]_n

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Chinese Journal of Structural Chemistry 2007年第11期26卷 1345-1348页

作者：沈艺程尹培秀李兆基覃业燕姚元根 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of MatterThe Chinese Academy of Sciences

A novel 2-D sheet inorganic-organic hybrid cadmium polymer, [CdBr2（bpdo）]n （bpdo = N,N＇-O,O-4,4’-bipyridine） has been hydrothermally synthesized and characterized by elemental analysis, IR and single-crystal X-ray diffraction. The crystal crystallizes in monoclinic, space group C2/c, with a = 16.336（3）, b = 3,9904（5）, c = 18,479（3） ]A, β = 91.640（6）°, Mr = 460.40, V= 1204.1（3）A3, Z = 4, Dc = 2,540 g/cm^3, p = 8.439 mm^-1, F（000） = 864, R = 0.0314 and wR = 0.0733 for 1069 observed reflections （Ⅰ 〉 2σ（Ⅰ））. X-ray diffraction reveals that the title compound consists of the 2-D inorganic-organic hybrid sheet constructed from [CdBr2]n chains and bpdo bridges in the packing motif of …ABAB… The title compound exhibits intense blue photoltmainescence in the solid state at room temperature.

关键词： cadmium polymer bpdo crystal structure luminescence

A Chain structure Based on Homodinuclear Scandium Units: [Sc(μ-OH)(2,5-pydc)(H_2O)]_n

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Chinese Journal of Structural Chemistry 2008年第1期27卷 83-87页

作者：黄有桂江飞龙吴明燕高强魏纬洪茂椿 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter The Chinese Academy of Sciences

The reaction of pyridine-2,5-dicarboxylic acid with Sc2O3 under hydrothermal con- dition yields a new complex [Sc（μ-OH）（2,5-pydc）（H2O）]n 1 which has a chain structure based on homodinuclear scandium units. Crystal data for 1： space group P^-1, a = 6.7192（13）, b = 7.6131（13）, c = 8.9313（14） A, α = 95.976（6）, β = 101.663（6）, γ = 108.151（5）^o, V= 418.26（13） A^3, Z = 2, Dc = 1.946 g/cm^3, g = 0.889 mm^-1, F（000） = 248, C7H6NO6Sc, Mr = 245.09, the final R = 0.0429 and wR = 0.1086.

关键词： scandium pyridine-2,5-dicarboxylic acid homodinuclear chain

Synthesis and Crystal structure of a Model for the Active Sites of Fe-only Hydrogenases:[Fe_2(SCH_2)_2N(3-PhCF_3)(CO)_6]_2

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Chinese Journal of Structural Chemistry 2007年第1期26卷 113-117页

作者：程岚霞马成丙胡明强陈昌能刘秋田 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of MatterThe Chinese Academy of Sciences

A model compound for the active sites of Fe-only hydrogenases, [Fe2（SCH2）2N（3- PhCF3）（CO）6]2, has been synthesized and structurally characterized by single-crystal X-ray diffraction. It crystallizes in tetragonal, space group P43, with α = 12.6324（3）, b = 12.6324（3）, c = 24.0453（12） A, V = 3837.1（2） A^3, Z= 4, Fe4S4N2C30O12F6H16, Mr= 1062.09, Dc= 1.839 g/cm^3, μ（MoKα） = 1.791 mm^-1, F（000） = 2112, T= 293（2） K, Flack = 0.034（9）, R = 0.0282 and wR = 0.0685 for 8148 observed reflections with I 〉 20（I）. In the title compound, each Fet atom is coordinated by three terminal carbonyl C atoms （Fe-C： 1.783（3）- 1.816（3） A）, two bridging S atoms （Fe-S： 2.2609（7）-2.2757（8） A） and another Fe atom （Fe-Fe 2.5011（5） A）, adopting a distorted octahedral geometry with trans angles ranging from 152.45（11） to 157.77（10）°.

关键词： Fe-only hydrogenases crystal structure iroa-suifur duster

Synthesis and structure of a novel V_2Ag_2S_4 cubane-like cluster (Et_4N)_2[V_2Ag_2S_4(OC_4H_8dtc)_2(PhS)_2]

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Science China Chemistry 1995年第3期38卷 264-272页

作者：杨瑜刘秋田康北笙卢嘉锡 State Key Laboratory of structure Chemistry and Fujian institute of research on the structure of matter. Chinese Academy of Sciences Fuzhou 350002 China

A novel heterometallic V2Ag2S4 thiocubane cluster was isolated from an assembly reaction system including (NH4)3VS4, Ag(PPh3)2NO3, OC4H8dtcNa and PhSNa in DMF. The title compound crystallizes in monoclinic space group C2/c with a = 2.0448(3) nm, b= 1.5086(2) nm, c= 1.7923(2) nm, β=109.32(1)°. The structure of the title compound was solved by using 1 500 (I>3σ(I)) unique reflections and refined to R = 0.068. The structural features indicate the formal oxidation state of V(IV) + Ag (I), and partial charge transfer from Ag(I) to V(IV). The actions of reactants used in the reaction are discussed and a supposed formation process of the V2Ag2S4 cluster is suggested.

关键词： vanadium cluster silver cluster V-Ag-S cluster cubane-like cluster heterometallic cluster.

Synthesis and Characterization of [NH_3(CH_2)_2NH_2(CH_2)_2NH_3]BiCl_6

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Chinese Journal of Structural Chemistry 2006年第3期25卷 338-342页

作者：徐刚付明来蔡丽珍张章静郭国聪黄锦顺 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter The Chinese Academy of Sciences

The title compound （[NH3（CH2）2NH2（CH2）2NH3]BiCl6, Mr= 527.88） has been synthesized by diffusion method and its crystal structure was determined by X-ray diffraction method. It crystallizes in orthorhombic, space group P212121 with a = 6.8444（4）, b = 13.6329（10）, c = 15.6641（12）A°, V= 1461.60（18）A°^3, Z= 4, Dc = 2.399 g/cm^3, F（000） = 984,μ（MoKα） = 13.132 mm^-1 and T = 293（2） K. The final R = 0.0294 and wR = 0.0490 for 2325 observed reflections with I 〉 2σ（I）. Each bismuth atom in the present compound is coordinated by six chlorine atoms to furnish a slightly distorted octahedral geometry. It is worthy to note that each adjacent [BiCl6]^3- and [H3dien]^3＋ entities are linked by hydrogen bonds to form two right- and left-handed helical double-chains running along the b axis. These two helical double-chains are interlaced into quadruple-stranded braid to give rise to a three- dimensional network. The optical absorption spectrum of the compound reveals the appearance of a sharp optical gap of 3.30 eV.

关键词： bismuthate halide hybrid inorganic-organic

Syntheses and Crystal structures of Two Cyano-bridged Bimetallic Complexes [Ln(DMSO)_2(H_2O)(μ-CN)_4Fe(CN)_2] (Ln = Ce and Eu, DMSO = Dimethylsulfoxide) with Layered structure

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Chinese Journal of Structural Chemistry 2008年第6期27卷 753-756页

作者：赵振乾蔡丽珍陈文通郭国聪黄锦顺 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of MatterThe Chinese Academy of Sciences

Two new bimetallic cyano-bridged complexes [Ln（DMSO）2（H2O）（μ-CN）4Fe（CN）2] （Ln = Ce 1, Eu 2） have been prepared by the grinding reaction method and structurally characterized by X-ray single-crystal structure analysis. Crystallographic data for 1： C10H14CeFeN6O3S2, Mr = 526.36, monoclinic, P2/n, a = 7.852（4）, b = 10.729（5）, c = 11.181（5）A,β = 96.992（8）°, V = 935.0（7） A^3, Z = 2, Dc = 1.870 g/cm^3,/1 = 3.421 mm^-1, F（000） = 512, R = 0.0363 and wR = 0.0971; and those for 2： C10H14EuFeN6O3S2, Mr = 538.20, monoclinic, P21n, a = 7.739（5）, b = 10.668（7）, c = 11.008（7） A,β = 96.943（3）°, V = 902.1（11） A^3, Z = 2, Dc = 1.981 g/cm^3,/1 = 4.499 mm^-1, F（000） = 522, R = 0.0345 and wR = 0.0855. In each complex the lanthanide ion is seven-coordinated in a pentagonal bipyramidal arrangement, and the Fe（Ⅲ） ion is in a nearly regular octahedral environment. The title complexes can be described as two- dimensional （2-D） stair-like structures, which are further connected by hydrogen bonds to form three-dimensional （3-D） frameworks.

关键词： crystal structure cyano-bridged bimetallic complex grinding reaction method

Synthesis and Crystal structure of [K(2,2,2-crypt)]_2HP_(11)

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Chinese Journal of Structural Chemistry 2008年第1期27卷 75-77页

作者：叶雅真徐立 State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter The Chinese Academy of Sciences

[K（2,2,2-crypt]2HP11 has been prepared from the reaction of K3P11 with the mixed ethylenediamine/2,2,2-crypt solution. The crystal structure was determined by singlecrystal X-ray diffraction. The crystal is of tdgonal system, space group P^-3c1 with a = 12.068（2）, b = 12.068（2）, c = 22.319（6）A, V = 2815.0（10）A^3, Dc = 1.384 g/cm^3, C36h73K2N4O12P11, Mr = 1172.85, F（000） = 1232,μ = 0.536 mm^-1, Z= 2, R = 0.0678 and wR = 0.2211 for 1763 observed reflections （I 〉 2σ（I））. In this compound, the P11 cluster has ideal 32-D3 symmetry, and the three-fold axis, corresponds to the crystallographic c axis. The （HP11）^2- anions are stable due to the completely sequestered alkali metal cations through only ion-ion interactions.

关键词： phosphorus hydrogen polyphosphide crystal structure

Triply-bridged Dicopper(Ⅰ)Complex of Bis(diphenylphosphino)acetylene with a Helical Coordination Cage

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Chinese Journal of Structural Chemistry 2002年第6期21卷 605-608页

作者： HAN Lei ZHANG Li-Yi CHEN Zhong-Ning HONG Mao-Chun(State Key Laboratory of Structural Chemistry, Fujian institute of research on the structure of matter, The Chinese Academy of Sciences, Fuzhou, Fujian 350002, China) State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter The Chinese Academy of Sciences

Self-organization of copper (I) ion with bridging ligand bis(diphenylphosphino)-acetylene resulted in the isolation of a dinuclear copper ( I ) complex [Cu2(μ-Ph2PC≡ CPPh2)3(MeCN)2](ClO4)2·Et2O. Structural analysis indicated the existence of a helical coordination cage, in which two copper (I) atoms are bridged triply by the linear diphosphine Ph2PC≡CPPh2 with the CuACu separation of 6.231 A. The copper (I) atom is in an approximately tetrahedral environment with a NP3 coordination chromophore. The complex crystallizes in the triclinic, space group P 1 with a = 13.8456(2), b = 16.6010(1), c = 18.9215(3) A, α = 98.289(1), β = 91.232(1), γ = 106.496(1)°, V = 4117.60(9) A3, Z = 2, C86H82Cl2N2O9P6Cu2, Mr= 1659.37, Dc= 1.338 g/cm3, F(000) = 1708, μ = 0.754 mm-1, the final R = 0.0688 and wR = 0.1940 for 11692 reflections with I>2σ(I).

关键词： bis(diphenylphosphino)acetylene cage copper crystal structure helicity