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Synthesis and crystal structure of an ionic cluster {[Mo_3(μ_3-O)(μ-S)_3(dtp)_3(py)_3][CdI(dtp)_2]}

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chinese Journal of chemistry 1997年第4期15卷 296-303页

作者： LU,Shao-Fang HUANG,Jian-Quan HUANG,Xiao-Ying WU,Qiang-Jinstate key laboratory of structural chemistry,fujian institute of research on the structure of matter,chinese academy of sciences,fuzhou,fujian 350002,china state key laboratory of structural chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Fuzhou Fujian 350002 China [?]Invited professor at fuzhou University.

A new cluster compound {[Mo3(μ3-O)(μ-S)3(dtp)3(py)3][CdI(dtp)2]} (dtp=S2P(O-was obtained from the reaction of (Mo3OS3(dtp)4(H2O)] with a CdI2-Bu4NI *** molecular structure is composed of a cluster cation [Mo3OS3(dtp)3(py)3]+ and the complex anion [CdI(dtp)2]-Crystal data:Triclinic,space group P1 with cell parameters a=1.4672(7),b=1.5356(5),c=1.6806(5) nm,α=74.59(3),β=67.89(4),7=78.86(3)°,V=3.364(2) nm3,and Z=2,least-squares refinement of 8941 reflections gives a final agreement factor of R=0.052,Rw=0.065.

关键词： Molybdenum cadmium cluster synthesis crystal structure

A dinuclear molybdenum cluster containing i-mnt ligand: synthesis and crystal structure of [Mo_2S_4(i-mnt)_2] (Et_4N)_2

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chinese Journal of chemistry 1997年第5期15卷 417-424页

作者： SUN, Fu-Xia LU, Shao-Fang WU, Qiang-Jin HUANG, Xiao-Yingstate key laboratory of structural chemistry and fujian institute of research on the structure of matter, chinese academy of sciences, fuzhou, fujian 350002, china state key laboratory of structural chemistry and fujian institute of research on the structure of matter Chinese Academy of Sciences Fuzhou Fujian 350002 China

A dinuclear molybdenum(V) cluster compound (Et4N)2[Mo2S4(i-mnt)2] (i-mnt=l,l-dicyanoethylene-2,2-dithiol, (S2C=C(CN)2]2-) has been prepared by the ligand substitution reaction of Mo2S4(iso-pr2dtp)2 (iso-pr2dtp=S2P(OC3H7)2-) with K2(i-mnt) in the presence of Bt4NI. This cluster was characterized by inrrared spectrum, UV-Vis spectrum and single crystal structure analy-sis. The cluster anion [Mo2S4(i-mnt)2]2- possesses C, symmetry with a crystallographic mirror plane through two bridging S atoms. By the S....S supramolecular interactions between two adjacent cluster anions the [Mo2S4(i-mnt)2]2- anions are linked to form infinite chains along the b axis. Crystal data: monoclinic, space group C2/m, a=1.8748(6), b=1.5360(4), c=1.4322(5) nm, ,β=112.02(2)°, V=3.823(4) nm3, Z=4, Dc=1.50 g/cm3. The final R=0.038 and .RW=0.053 for 3015 observed unique reflections.

关键词： Dinuclear molybdenum cluster synthesis crystal structure IR and UV-Vis spectra S....S supramolecular interaction

Synthesis,X-Ray structure and Characterization of a Triruthenium Cluster Complex Ru3Ⅲ（μ3-O）(μ-CH3COO)6（py）2Cl with Four Steps One-electron Redox Processes

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chinese Chemical Letters 2003年第5期14卷 519-522页

作者： Jing Lin CHEN, Gang Qiang YIN, Zhong Ning CHEN* state key laboratory of structural chemistry, fujian institute of research on the structure of matter, fuzhou 350002 Stt. key Lab. of Struct. chemistry Fujian Inst. Res. Struct. of Matter Fuzhou 350002 China

The synthesis and crystal structure of oxo-centered carboxylate-bridge trinuclear ruthenium complex, Ru3O(CH3COO)6(py)2Cl (py = pyridine) (1), are reported herein. The complex 1 has been characterized by IR, cyclic voltammetry (CV), UV-Vis and X-ray crystal analysis. The complex 1 in 0.1 mol/L (n-C4H9)4NPF6-CH2Cl2 solution at room temperature shows four one- electron redox processes at E1/2 = -1.38, -1.20, -0.17 and 1.07 V vs. Ag/AgCl.

关键词： Crystal structure ruthenium carboxylate electrochemistry.

structure of the Heterobimetallic Linear-Chain Polymeric Complex [NH_4]_n [WAgS_4]_n and Influence of Cationic Valence state on Configurations of Polymeric W/Ag/S Complexes

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chinese Journal of structural chemistry 1997年第4期16卷 253-257页

作者： HUANG Qun WU Xin-Tao LU Jia-Xi(state key laboratory of structural chemistry, fujian institute of research onthe structure of matter, the chinese academy of sciences, fuzhou 350002) 中科院福建物质结构所结构化学国家重点实验室福建福州

The title complex [NH4]n [WAgS4]n crystallizes in the tetragonalspace group I4 with crystallographic parameters: a = b = 7. 994 (2 ), c = 5. 855 (2 ):A,V = 373. g(2) A3, Z=2, Dc= 3. 89 g/cm3, F(000) = 392, μ= 19. 27 mm-l , A(MoKα) = 0. 71069, Mr = 438. 01, and the convergence factors R = 0. 045, Rw =0. 055 for 341 observed reflections (I>3σ(I)). The anion structure can be viewed as apolymeric single chain consisting of unlimited extended rhombic fragruents of -AgS2W-which are alternately perpendicular to each other. Additionally, influence of di- and tri-valent complex cations on the assembIy of WS2-4 and Ag+ is briefly discussed.

关键词： tungsten complex silver complex polymeric linear-chain complex crystal structure

Zinc-containing chainlike polymer {Cs_2[Zn(S_2C=C(CN)_2)_2]}_n,the second example of bridging [S_2C=C(CN)_2]

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chinese Journal of chemistry 1997年第2期15卷 188-192页

作者： ZHU,Yong-Bao LU,Shao-Fang HUANG,Xiao-Ying WU,Qiang-Jin ZHANG,Yu-Dongstate key laboratory of structural chemistry,fujian institute of research on the structure of matter,chinese academy of sciences,fuzhou,fujian 350002,china state key laboratory of structural chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Fuzhou Fujian 950002 China [*]state key laboratory of structural chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences Fuzhou Fujian 950002 China

The title compound {Cs2[Zn(S2C=C(CN)2)2]}n(2),Catena-poly {dicesium [bis(l,l-dicyanoethene-2,2-dithiolato-S,S':N)-Zinc(Ⅱ)]},is the second example of bridging [S2C=C(CN)2] (hereafter referred to as i-mnt) for metal-containing *** crystallizes in the non-centrosymmetric space group Ia (***,No.9).There are two coordination modes of i-mnt in this compound:μ-η1-η1-i-mnt,bridging two Zn moieties with two S atoms and terminal i-mnt.A characteristic feature of the structure is the infinite-Zn(η2-i-mnt)(η1-η1-i-mnt)-Zn(η1-η1-i-mnt)(η2-i-mnt)-wave-like *** atoms are located between the chains to form three-dimensional network-like *** efficient second harmonic generation from the crystal has been observed on the irradiation with the 1064 nm output of a Nd:YAG laser.

关键词： Zinc-containing polymer synthesis crystal structure

Synthesis and Crystal structure of an Ion- pair Compound: [HL]2[Ni（CN）4]·4H2O (L = 4-（2- Hydroxyphenyl）-1,5, 9-triazacyclododecan-2-one)

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chinese Journal of structural chemistry 2004年第4期23卷 361-365+352页

作者： LI Jian-Ronga, b XIE Ya-Bob CAI Li-Zhena GUO Guo-Conga② BU Xian-Heb② HUANG Jin-Shuna a (state key laboratory of structural chemistry, fujian institute of research on the structure of matter, The chinese academy of sciences, fuzhou, fujian 350002, china. b (Department of chemistry, Nankai University, Tianjin 300071, china. 中科院福建物质结构所 State Key Laboratory of Structural ChemistryCAS 福建 Fuzhou 350002 Department of chemistry Nankai University 天津 300071

An ion-pair compound, [HL]2[Ni(CN)4]4H2O 1 has been obtained as an unexpected product when we attempt to prepare a heterometallic cyano-bridged complex by the reaction of GdCl3nH2O, K2Ni(CN)4 and L (L=4-(2-hydroxyphenyl)-1,5,9-triazacyclododecan-2-one) in aqueous solution, and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P21/n with a = 12.380(1), b = 9.9637(8), c = 17.087(1) ? ?= 105.947(2)? V = 2026.6(3) ?, Rint = 0.0509, Z = 2, Dc = 1.297 g/cm3, C34H56O8N10Ni, Mr = 791.60, F(000) = 844, m(MoKa) = 0.538 mm1, S = 1.030, the final R = 0.0644 and wR = 0.1299 for 2023 observed reflections with I ≥ 2(I). The title compound 1 contains one anion of [Ni(CN)4]2, two cations of [HL]+ and four packing water molecules, which are held together by the NH···O and OH···O hydrogen bonds to form a three- dimensional framework.

关键词： tetracyanonickelate anion macrocyclic triamine cation crystal structure

structure of Barium Tetrafluorborate Ba_2(BF_4)_4

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chinese Journal of structural chemistry 1998年第4期17卷 245-248页

作者： LIN Qi-Sheng CHENG Wen-Dan CHEN Jiu-Tong HUANG Jin-Shun(state key laboratory of structural chemistry, fujian institute of research onthe structure of matter, the chinese academy of sciences, fuzhou 350002, china. 中科院福建物质结构所福建福州

The title compound Ba2 (BF4)4 crystallizes in the monoclinic spacegroup P21/n with crystallographic parameters: a = 8. 339 (3), b = 16. 530 (7), c =10. 212(4) A, V=1348. 7 A3, β= 106. 64(3)°, Z=4, Dc=3. 06 g/cm3, F(000)=1104, μ=5. 98 mm-1, (MoKa) =0. 71069, M= 621. 90. Least-squares refinementaffords the final residuals R=0. 0639 and Rw=0. 0676 for 2841 observed reflections (I>3(I)). The structure consists of columns of BF4 groups, which parallel to the b direction. All columns are linked together through Ba…F bonds, Both the two crystallographically different barium atoms are nine-coordinated by a distorted tri-capped prismof fluorine atoms from the nearest six BF4 tetrahedrons. There are two types of fluorineatoms, one connecting one barium atom and the other connecting two barium *** BF4 tetrahedron is connected to three barium atoms, so it (tetrahedron) can beviewed as unidentate ligand and bidentate ligand at the same time.

关键词： crystal structure barium tetrafluorborate

Synthesis and structure of Tungsten Carbonyl Compound with 2-Mercapto Pyrimidine [Et_4N] [W (CO)_4(SC_4H_3,N_2) ]

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chinese Journal of structural chemistry 1998年第5期17卷 334-336页

作者： PAN Guo-Hua ZHUANG Bo-Tao HUANG Liang-Ren (state key laboratory of structural chemistry, fujian institute of research on the structureof matter, the chinese academy of sciences, fuzhou, fujian 350002, china. state key Lab. of Struct. chemistry Fujian Inst. Res. Struct. of Matter Chinese Academy of Sciences Fuzhou Fujian 350002 China

Reaction of W (CO)6 with HSC3H3N2, Et3N and Et4NCl. H2O inCH3CN afforded a mononuclear compound (Et4N] [W(CO)4 (SC4H3N2)]. The crystalstructure was determined by X-ray diffraction. The crystallographic data: C16H23-N3O4SW, Mr = 537- 29, monoclinic, C2/c, a = 19. 3l7 (l0), b = 13. 75l (8), c=16. 350(8) A, β= l09. 93°, V= 4082. 7 A3, Z= 8, D.= 1. 75 g/cm', F(000) =2096, μ= 59. 0 cm-1, Final R=0. O29 and Rw= O. 036 for 2769 reflections with I>3σ(I). The X-ray structure analysis revealed that the center W atom is coordinated by Sand N atoms from 2-mercapto pyrimidine ligand and four C atoms from carbonyl,which displays a distorted octahedral geometry.

关键词： synthesis structure tungsten complex 2-mercaptpo pyrimidine

Synthesis and Crystal structure of Er_2Si_2O_7

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chinese Journal of structural chemistry 1998年第1期17卷 24-26页

作者： CHI Li-Sheng CHEN Hua-Yang ZHUANG Hong-Hui HUANG Jin-Shun(state key laboratory of structural chemistry, fujian institute of research onthe structure of matter, the chinese academy of sciences, fujian fuzhou 350002) state key Lab. of Struct. chemistry Fujian Inst. Res. Struct. of Matter Chinese Academy of Sciences Fujian Fuzhou 350002 China

The title compound crystallizes in monoclinic system, space group C2/m with cell dimensions of a=6. 843(2), b=8. 939(2), c=4. 720(1) A, β=101. 77(2), V=282. 7A3, Z=2, Mr=502. 69, Dc=5' 91 g·cm-3, u(MoKa)=303. 0cm-1, F(000) ~ 440. The structure solution and refinement are based on 869 uniqueobserved reflections with I≥3(I) and the final discrepancy factors converged at R=0. 034, Rw= 0. 042. The structure is considered to be the oxygen atoms packed innearly hexagonal arrangement with rare earth atoms in the octahedral and silicon atomsin tetrahedral holes in alternately parallel layers.

关键词： solid state synthesis crystal structure thortveitite