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Synthesis, Single-crystal Structure, and Optical and Magnetic Properties of CaEr_2S_4

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Chinese Journal of Structural Chemistry 2007年第8期26卷 973-979页

作者： ZENG Hui-Yi Mattausch Hansjtirgen zheng fa-kun DONG Zhen-Chao GUO Guo-Cong HUANG Jin-Shun State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter The Chinese Academy of Sciences Fuzhou Fujian 350002 China Max Planck Institute for Solid State Research Heisenbergstrasse 1 D-70569 Stuttgart Germany Hefei National Laboratory for Physical Sciences at Microscale University of Science and Technology of China Hefei Anhui 230026 China

Brown needle-like crystals of CaEr2S4 were isolated as the major product from a reaction of elements and binary sulfides by a two-step flux technique. CaEr2S4 crystallizes in the orthorhombic space group Pnma with a=12.845（4）, b=3.862（4）, c=13.001（2）（A）, V=645.0（7）（A）3,Z=4, F（000）=880,μ（MoKα）=27.794 mm^-1, the final R=0.0528 and wR=0.0562 for 1070observed reflections with I 〉 3σ（I）. The CaEr2S4 structure forms a three-dimensional framework that consists of interconnected tetra-octahedral Er4S18 fragments. Ca^2＋cations, in a monocapped trigonal prism geometry, are stuffed in two parallel rows into the one-dimensional channels along the b direction. CaEr2S4 is an infrared-transparent semiconductor with a band gap of 1.81 eV. Magnetic susceptibility measurements over 6～300 K indicate a Curie-Weiss paramagnetic behavior for the phase, with an effective magnetic moment of 9.64（1） μB per Er^3＋ ion.

关键词： rare-earth chalcogenides flux crystal growth crystal structure optical and magnetic properties

Synthesis and Crystal Structure of a New Copper(II) Complex with 4-Cyanobenzoic Acid

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Chinese Journal of Structural Chemistry 2005年第11期24卷 1281-1285页

作者： LI Yan WU A-Qing zheng fa-kun GUO Guo-Cong LU Can-Zhong HUANG Jin-Shun State Key Laboratory of Structural Chemistry Fujian Institute of Research on theStructure of Matter The Chinese Academy of Sciences Fuzhou Fujian 350002 China Graduate School The Chinese Academy of Sciences Beijing 100039 China

A new Cu（Ⅱ） complex [Cu（4-cba）（1,10-phen）（H2O）2]（NO3）（4-Hcba = 4-cyanobenzoic acid） has been synthesized by solvothermal reaction in an ethanol/water mixed solution at 100 ℃ and structurally characterized by single-crystal X-ray diffraction. Crystallographic data： C20H16CuN4O7, Mr= 487.91, triclinic, space group PI, a = 7.8420（2）, b = 9.1070（2）, c = 15.1140（6） A, a = 76.889（9）, β = 81.332（11）, γ = 74.844（ 11）°, V = 1009.89（5） A^3, Z = 2, Dc = 1.605 g/cm^3, F（000） = 498, μ = 1.134 mm^-1, the final R = 0.0379 and wR = 0.0865 for 2977 observed reflections with 1 〉 2σ（Ⅰ）. The Cu（Ⅱ） atom is coordinated by two terminal water molecules, one chelating 1,10-phen molecule and one monodentate 4-cba ligand to form a slightly distorted square pyramid. The title complex molecules are connected through hydrogen bonds and π-π stacking interactions to generate a 2D layered network. The thermogravimetric analysis of the title complex has also been discussed.

关键词： copper(Ⅱ) complex,4-cyanobenzoic acid crystal structure hydrogen bonds,π-π stacking

Synthesis and Crystal Structure of a New Lanthanum(III) 4-Cyanobenzoate Complex

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Chinese Journal of Structural Chemistry 2007年第5期26卷 575-579页

作者： LI Guo-Qing LI Yanb ZOU Wen-Qiang CHEN Qi-Yong zheng fa-kun GUO Guo-Cong Chemistry and Life Science School Quanzhou Normal University Quanzhou Fujian 362000 China State Key Laboratory of Structural Chemistry Fujian Institute of Research on theStructure of Matter The Chinese Academy of Sciences Fuzhou Fujian 350002 China Graduate School of the Chinese Academy of Sciences Beijing 100039 China

A new dinuclear La（Ⅲ） complex [La2（4-cba）4[H（4-cba）2]2（phen）2（H2O）4] （4-Hcba = 4-cyanobenzoic acid and phen = 1,10-phenanthroline） 1 has been synthesized by solvothermal reaction in an ethanol/water mixed solution at 100 ℃ and structurally characterized by singlecrystal X-ray diffraction. Crystallographic data： C88H58La2N12O20, Mr = 1881.28, triclinic P1, a = 7.518（3）, b = 17.033（6）, c = 17.551（6）A, α = 115.333（4）, β = 92.9910（10）, γ = 99.366（5）°, V = 1985.3（12）A^3, Z = 1, Dc = 1.574 g/cm^3, F（000） = 944 μ = 1.145 mm^–1, the final R = 0.0281 and wR = 0.0686 for 6708 reflections with Ⅰ 〉 2σ（I）. In 1, two nine-coordinated La（Ⅲ） ions are connected by two 4-cba ligands in a syn-syn bidentate coordination mode, and the other six 4-cba ligands terminate the La（Ⅲ） ions, resulting in an isolated dinuclear structure. Two different types of intramolecular hydrogen bonds, asymmetrical O-H…O and symmetrical O…H…O, exist in the crystal. The title complex molecules are connected through hydrogen bonds and weak π-π stacking interactions to generate a 2-D layered network. The thermogravimetric analysis of 1 has also been discussed.

关键词： lanthanum(Ⅲ) complex 4-cyanobenzoic acid crystal structure hydrogen bonds

Studies　on　the　V－Cu－S　Heterometallic　Cluster　Compounds（2）．Crystal　Structure　of［VS₄（CuPPh₃）₅Br₂］·0．5CH₂Cl₂

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Chinese Journal of Structural Chemistry 1994年第5期13卷 397-401页

作者： zheng fa-kun Yu Xiu-Fen(State Key Laboratory of Structural Chemistry,Fujian Institute of Research on the Structure of Matter,Chinese Academy of Sciences,Fuzhou,Fujian 350002)(Department of Chemistry,Fuzhou University,Fuzhou,Fujian,350002)

The title compound crystallizes in the monoclinic space group P21/n with cell dimensions a=13.068(3),b=22.378(8),c=31.188(10),β=92.09(2)°,V=9113.13,Mr=2010.7,Z=4,Dc=1.44 g/cm3,μ(MoKα)=28.8cm-1,F(000)=3828.R=0.102 and Rw=0.109 for 3863 unique reflections with I>2σ(I).The V atom in the compound retains the tetrahedral geometry of thefree VS43-with S-V-S angles ranging from 106.8(4) to 110.6(4)°.The coreVCu5Br2S4 of the compound can be regarded as a face-sharing distorted cubane-likegeometry with lack of an edge.

关键词： preparation crystal structure tetrathiovanadate vanadium cluster copper cluster

Synthesis and Crystal Structure of an Octa-nuclear V-Cu-S Cluster:[VS_3O(CuPBu_3)_2(CuSPBu_3)]_2

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Chinese Journal of Structural Chemistry 1997年第5期16卷 365-370页

作者： zheng fa-kun CUI Yong CHENG Wen-Dan HUANG Jin-Shun(State Key Laborory of Stractural Chemistry, Fujian Institute of Research onthe Stracture of Matter, the Chinese Academy of Scicnces, Fuzhozt, Fujian 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 compound has been synthesized by reaction of (NH4)3VS4,CuCl, and PBu3 in CH2Cl2 and its structure was determined by single crystal X-raydiffraction. Crystallographic data: C72 H162 Cu6O2P6S8V2, Mr= 1985. 57, monoclinicspace group C2/c, a= 17. 864(3), b= 25. 946(8), c= 24.071 (7),β= 112. 79(2)°,V = 10285. 9, Z= 4, Dc= 1. 28 g/cm3, F(000) = 4192, μ(MoKa) = 16. 7 cm-1,the final R=0.065 and Rw =0.074 for 4051 unique reflections with I> 3σ(I). Thestructure can be described as a metal-sulfur dodecahedral cage fused by two incompletecubane-like VS3Cu3 units connected by Cu - S bonds. The Cu - S bonds within theasymmetric VS3Cu3 unit are slightly shorter than those linking the two centrosymmetrically related VS3Cu3 units. The six copper and two vanadium atoms display asomewhat distorted cubane array with a μ4-S atom on each face of the metal cubane.

关键词： synthesis crystal structure vanadium cluster copper cluster

A　Novel　Cluster［V2（AgPPh3）6S6O2］·2CH2Cl2　Containinga　Cubane－like　Array　of　Six　Silver　and　Two　Vanadium　Atoms

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Chinese Journal of Structural Chemistry 1996年第2期15卷 102-105页

作者： zheng fa-kun Huang Jin-Shun Huang Xiao-Yin Zhang Qian-Er (State Key Laboratory of Structure Chemaxtry,Fujian instuute of Research on the Structure of Matter,Chinese Academy of Scicnces,Fuzhou,350002) State Key Lab. of Struct. Chemistry Fujian Inst. Res. Struct. of Matter Chinese Academy of Sciences Fuzhou 350002

ＡＮｏｖｅｌＣｌｕｓｔｅｒ［Ｖ２（ＡｇＰＰｈ３）６Ｓ６Ｏ２］·２ＣＨ２Ｃｌ２ＣｏｎｔａｉｎｉｎｇａＣｕｂａｎｅ－ｌｉｋｅＡｒｒａｙｏｆＳｉｘＳｉｌｖｅｒａｎｄＴｗｏＶａｎａｄｉｕｍＡｔｏｍｓ￥ＺｈｅｎｇＦａ－Ｋｕｎ；... 详细信息

ＡＮｏｖｅｌＣｌｕｓｔｅｒ［Ｖ２（ＡｇＰＰｈ３）６Ｓ６Ｏ２］·２ＣＨ２Ｃｌ２ＣｏｎｔａｉｎｉｎｇａＣｕｂａｎｅ－ｌｉｋｅＡｒｒａｙｏｆＳｉｘＳｉｌｖｅｒａｎｄＴｗｏＶａｎａｄｉｕｍＡｔｏｍｓ￥ＺｈｅｎｇＦａ－Ｋｕｎ；ＨｕａｎｇＪｉｎ－Ｓｈｕｎ?..

关键词： preparation crystal structure tetrathiovanadate vanadium cluster silver cluster

Structural Studies of [V_2S_6O_2(CuPPh_3)_4(CuMeCN)_2]·2CH_2Cl_2·2PrOH

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Chinese Journal of Structural Chemistry 1996年第5期15卷 353-357页

作者： ZHANG Han-Hui YU Xiu-Fen YANG Rong-Sheng zheng fa-kun HUANG Liao-Yuan ZHUO Ru-Peng(Department of Chemistry, Fuzhou University, Fuzhou, Fujian,350002)(State Key Laboratory of Structural Chemistry, Fuzhou, Fujian, 350002) 福州大学化学系结构化学国家重点实验室福建福州

The title V-Cu-S heterometallic cluster compound C84 H86Cl4Cu6N2O4P4S6V2, crystallizes in the monoclinic space group P21/n with a=16.381(5), b=17.114(3),c=16.749(6) A,β=107. 04(3)°,V=4490(2)A3, Mr=2128.84,Z=2,Dc=1. 57 g/cm3,μ= 19. 6 cm-1,F(000)=2160. Final R=0.074(Rw=0.082) for 2662 unique reflections with I≥3σ(I). The V atom in the compound retains the tetrahedral geometry of the VS3O with S-V-S or S-V-O angles of 108.6(6)～110.3 (6)°.The cluster core [V2Cu6S6O2] of the compound can be regarded as two cluster cores [VCu3S3O] bonded by bondings of the Cu-Cu'(distances of 2.774(3)～2.707(5) A) and Cu-S (distances of 2.463(7)～2.396(9) A) with centrosymmetric. Atoms of the cluster core V2Cu6 form a distorted cube with the Cu Cu'or the V-Cu distances of 2. 774(3)～2. 707(5) A.

关键词： crystal structure vanadium cluster copper cluster

Synthesis and Crystal Structure of a Hepta-nuclear V-Cu-S Cluster:[VS_4Cu_6(Py)_8Br_3]

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Chinese Journal of Structural Chemistry 1997年第5期16卷 392-396页

作者： zheng fa-kun ZHANG Han-Hui ZHUO Ru-Peng WU Yong-Sheng YU Xiu-Fen HUANG Jin-Shun(State Key Labortory of Structural Chemistry, Fujian Institute of Researchon the Structure of Matter, the Chinese Academy of Sciences, Fuzhou, Fujian 350002)(Chemistry Depa 中科院福建物质结构所福建福州福州大学化学系福建福州

The title compound has been synthesized by the reaction of(NH4)3VS4, CuBr and NMe4Br in pyridine and its structure was determined by singlecrystal X-ray diffraction. Crystallographic data: C40H40Br3Cu6N8S4V, M4= 1432. 95,orthorhombic space group Fdd2, a= 29. 9519 (2), b=13. 4719 (2), c= 25. 8612 (4)A, V= 10435. 2 (4), Z= 8, Dc= 1.824 g/cm3, F(000)= 5616,μ(MoKa) =50.64 cm-1, the final R =0.091 and wR =0. 206 for those 3401 unique reflectionshaving . The crystal structure determination shows that the cluster consists of a tetrahedral VS4 core encapsulated by a distorted octahedral array of six copperatoms which have two different coordination geometries, trigonal and tetrahedral.

关键词： synthesis crystal structure vanadium cluster copper cluster

Synthesis and Structure of [Cu2（μ-NO2）(aepy)4]（ClO4）3 (aepy = 2-（2-Aminoethyl）pyridine)

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Chinese Journal of Structural Chemistry 2002年第5期 485-488页

作者： LIU Jia-Cheng GUO Guo-Cong LIN Shan-Huo zheng fa-kun MA Hong-Wei ZHOU Guo-Wei HUANG Jin-Shun (State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, The Chinese Academy of Sciences, Fuzhou, Fujian 35

The title compound [Cu2(m-NO2)(aepy)4](ClO4)3 (Cu2C28H40N9Cl3O14, Mr = 960.12, aepy = 2-(2-aminoethyl)pyridine) was synthesized and its crystal structure was determined by X-ray diffraction method. It crystallizes in monoclinic, space group C2/c with cell parameters: a = 21.958(3), b = 12.205(2), c = 15.180(3) ? b = 106.06(1), V = 3909.5(12) ?, Z = 4, Dc = 1.631 g/cm3, F(000) = 1968 and m(MoKa) = 1.368 mm-1. The structure was solved by direct methods and refined by full-matrix least-squares techniques. The final R = 0.0734 and wR = 0.1954 for 1606 observed reflections with I ≥2.0s(I). The crystal structure revealed that the [Cu2(m-NO2)(aepy)4]3+ cation consists of two square-based pyramidal copper (Ⅱ) atoms bridged by one nitrate anion. The distance between the two copper atoms (Cu(1)…Cu(1A)) is 5.373 (2) ?

关键词： synthesis copper 2-(2-aminoethyl)pyridine crystal structure