双（N′-乙基-N-哌嗪基二硫代氨基甲酸锌）配合物[Zn2(S2CNC4H8NC2H5)4]的晶体结构和表征

The title compound has been prepared and characterized by elemental analyses, infrared and raman spectra, and thermal analyses. The crystal structure of Bis [di(N′-ethyl-N-piperazinly-carbodithioato-S,S′) Zinc(Ⅱ)] complexes, [Zn₂(S₂CNC₄H₈NC₂H₅)₄], was determined by X-ray diffraction methods. The compound crystallizes in Monoclinic system, space group P2₁/c, with lattice and some related parameters a=0.886(18), b=1.955(4), c=1.196(2) nm, β=106.03(3)°, V=1.991 3(7) nm³, Z=2, M_r=888.12, D_c=1.481 g·cm^-3, F(000)=928, R=0.054 3 and wR=0.227 6. In crystal structure of the binuclear zinc complexes is built up of centro-symmetric dimeric entities. The coordination sphere of zinc(Ⅱ) ions is best described as a distorted tetragonal-pyramid. The IR spectral data are in agreement with the structural data. The thermal analytical data indicate that it decomposed completely at the temperature of 652.5 ℃, leaving Zn. CCDC: 286177.     

配位聚合物{[Co(4,4′-bpy)(H2O)4](Fum)·4H2O}n的合成和晶体结构

The complex {[Co(4,4′-bpy)(H₂O)₄](Fum)·4H₂O}_n(where 4,4′-bpy = 4,4′-bipyridine and Fum = fumarate) was synthesized and characterized by X-ray diffraction. The complex consists of one-dimensional chains containing cobalt(Ⅱ) ions bridged by 4,4′-bpy molecules. The six-coordination of Co²⁺ is achieved by means of four water molecules. The fumarate is not coordinated to cobalt ion while it forms hydrogen bonds with coordinated and non-coordinated water molecules and extends the structure into three-dimensional hydrogen bonding network. CCDC: 190488.     

Co[(C6H11O)2PS2]2·2Py的合成和晶体结构

Oxidation process of Co[(C₆H₁₁O)₂PS₂]₂ and substitute-reduction reaction of Co[(C₆H₁₁O)₂PS₂]₃ with pyridine have been studied by spectrophotometric methods, respectively. The equilibrium constant was found to be K=0.63±0.02(mol·dm^-3)^-3. The crystal structure of Co[(C₆H₁₁O)₂PS₂]₂·2Py has been determined by X-ray diff- raction method. The crystal belongs to triclinic system, space group P1, with cell parameters: a=6.944(2)?,b=9.277(3)?,c=15.981(6)?,α=91.79(3)°,β=99.55(3)°,γ=94.44(3)°,V=1011.2(6)?³,Z=2,M_r=803.94,D_c=1.320Mg·m^-3,F(000)=425,μ=0.747mm^-1,final R=0.0700 and wR=0.1988 for 3626 re-flections with I≥2σ(I). The cobalt atom in the title complex has a octahedral geometry with four Co-S bonds and two Co-N bonds. The central atom P is tetrahedrally surrounded by two sulphur atoms and two oxygen atoms in the dicyclohexyldithiophosphate ligand. The six carbon atoms of cyclohexyl take the chair conformation.     

一个新的钴磷酸盐配合物Co(μ3-O3P)·H2O的合成与晶体结构

A new layered cobalt phosphate complex, Co( μ₃-O₃P)·H₂O, was prepared by the hydrothermal reaction. The crystal structure of the complex was determined by single-crystal X-ray diffraction. The results indicate that it contains two different infinite PO₃chains linked by CoO₆ octahedra with infinite 1-D tunnels. It crystallizes in the orthorhombic space group Pbcm with a=0.790 12(16) nm, b=0.900 25(18) nm, c=1.016 1(2) nm, β=90°, V=1.245 3nm³, Z=4. Refinement gave R₁=0.068 5, wR₂=0.175 1 for 2 133 unique observed reflections (I>2σ(I)). The title complex was also characterized by IR, TG-DTA and chemical analysis. CSD: 413934.     

N′-乙基-N-哌嗪基二硫代氨基甲酸铜(Ⅱ)配合物Cu(S2CNC4H8NC2H5)2的晶体结构及谱学研究

合成了标题化合物Cu(S₂CNC₄H₈NC₂H₅)₂,得到深棕色柱状晶体。晶体属三斜晶系,空间群为P1。中心Cu(Ⅱ)离子分别与来 自2个N′-乙基-N-哌嗪基二硫代氨基甲酸的4个硫原子配位,形成略微扭曲的平面四方配位构型。4个Cu-S键的键长范围0.220 10(11)～0.220 34(13) nm;Cu-S键的FT-Raman伸缩振动峰在134.921 cm^-1;ESR谱表明Cu(Ⅱ)离子处于对称中心;其局部配位构型属于D_2h群;热分析表明标题化合物在753.15 ℃时分解为金属Cu。     

桥联双核配合物[(DPC)2Co2(H2O)5]·2H2O的合成与晶体结构

The new complex formulated [(DPC)₂Co₂(H₂O)₅]·2H₂O (HDPC^- is pyridine-2,6-dicarboxylate) has been synthesized and the crystal structure was determined by X-ray diffraction. The crystal structure of the complex belongs to monoclinic system with space group P2₁/c, a=0.83850(10) nm, b=2.7386(4) nm, c=0.9610(2) nm, β=98.280 (10) °, V=2.1838(6) nm³, Z=4, D_c=1.746 g·cm^-3, μ=1.597 mm^-1. In the crystal the two Co²⁺ are in distorted octahedrons. The part of [Co(DPC)₂] possess an approximate D_2d symmetry, while the part of [OCo₍₂₎(OH₂)₅] has an approximate C₂ symmetry.     

[La(p-OHC6H4CH2COO)3(phen)]2·2H2O的合成和晶体结构

A complex of lanthanides formulated as [La(p-OHC6H4CH2COO)3(phen)]2 was prepared from the water/ethanol solution under normal temperturate with 8-hydroxyquinoline as the acidity eonditionor,the complex was characterized by elemental analysis,IR,1H NMR spectroscopy and X-ray crystal structure analysis.The crystal belongs to monoclinic crystal system,space group P21/n.The 1,10-phenanthroline and 4-hydroxyphenylacetic ligands coordinated to the center ion through O or N atoms.The structural feature of the complex were discussed.CCDC:25305.     

咪唑配合物[Co(C3H4N2)6](PhCHCHCOO)2的合成及晶体结构

The complex [Co(Im)6](Cin)2 (Im=imidazole,Cin=cinnamate) was prepared by reaction of Co(PhCHCHCOO)2 with imidazole in ethanol. It has been determined by single crystal X-ray analyses. The crystals are triclinic, space group P, with a=9.7601(3),b=10.5935(3),c=11.3269(2)(A),α =69.948(1),β =71.027(1),γ =62.803(1)°, and Z=1. The crystal structure of the title complex consists of monomeric [Co(Im)6]2+ cations and cinnamate anions in which the cobalt(Ⅱ) ion assumes a centrosymmetric octahedral geometry with the CoN6 chromophore. In the solid state, the complex forms a three dimensional network through N-H… O hydrogen bonds, the intermolecular hydrogen bonds connect the [Co(Im)6]2+ cations and cinnamate anions.The cinnamate anions are nearly planar.     

配合物[Co(phen)2(m-chlorobenzoic acid)2·(H2O)]·(H2O)2的水热合成、晶体结构电化学分析

The title complex has been synthesized with m-chlorobenzoic acid, 1,10-phenanthroline and cobalt perchlorate anhydrous in the solvent mixture of water and methanol. Crystal data for this complex: triclinic, space group P1, a=0.870 7(3) nm, b=1.284 4(4) nm, c=1.692 9(5) nm; α=75.430(5)°, β=77.562(5)°, γ=86.346(5)°, V=1.789 4(9) nm³, D_c=1.456 g·cm^-3, Z=2, F(000)=806. Final GooF=1.065, R₁=0.068 4, wR₂=0.127 5. The crystal stru-cture shows that the Cobaly ion is coordinated with four nitrogen atoms from two 1,10-phenanthroline molecules and two oxygen atoms from one m-chlorobenzoic acid molecule and one water molecule respectively, forming a distorted octahedral coordination geometry. The cyclic voltametric behavior of the complex is also reported. CCDC: 619087.     

铋配合物[Bi(S2CNC5H10)2(NO3)]·[1，10-Phen]·0.5H2O的合成及晶体结构

The bismuth complex with dithiopiperdylcarbamate [Bi(S₂CNC₅H₁₀)₂(NO₃)]·[1，10-Phen]·0.5H₂O was synthesized. The crystal and molecular structure were determined by X-ray single crystal diffraction. The crystal belongs to monoiclinic with space group C2/c, a=3.140(2) nm, b=1.176 4(9) nm, c=2.021 6(15) nm, β=103.081(12)°, V=5.713(7) nm³, Z=8, F(000)=3064, D_c=1.815 g·cm^-3, μ=6.502mm^-1. The final R₁=0.0332, wR₂=0.040 3. In the complex, the bismuth atom is eight-coordinated in a capped distorted pentagonal bipyramidal geometry. CCDC: 222655.     

New Supramolecular Complex Assembled through Hydrogen Bonds. Crystal Structure of Co(PMBP-tsc)_2 ·2DMF·2H_2O

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Crystal Structure of [Co2(μ-dmg)2(μ-dmg H)(dmg H)(Pø3)] 1/2 dmg H2 · 1/2 CH3OH: A Crystal Containing Various Forms of dmg Ligand

The crystal structure of [Co₂(μ-dmg)₂(μ-dmg H)(dmg H)(Pø₃)] · 1/2 dmg H₂ · 1/2 CH₃OH has been determined by single crystal X-ray diffraction. The title complex crystallizes in triclinic space group P&1bar; with a=10.859(3), b=13.299(3), c=15.247(3)Å, α=98.52(2), β=99.26(2), γ=97.80(2)° and Z=2. The agreement indices are R(F)=0.062 and R_w(F)=0.085 for 5231 observations and 515 variables. Both cobalt atoms have an oxidation state of 3+ and are both six-coordinated; one Co(III) atom is bonded to a phosphorous atom of triphenylphosphine, four nitrogen atoms of two planar ligands, dmg^2? and dmgH^?, and one oxygen atom of another dmg^2? ligand. The other Co(III) atom is coordinated by four nitrogen atoms of two cis nonplanar ligands, dmg^2?, dmgH^?, and two oxygen atoms of the other dmg^2? and dmgH^? ligands. There are three N-O bridged ligands namely two dmg^2? and one dmgH^? between two Co(III) atoms. A free molecule of dmgH₂ and a molecule of CH₃OH are also found in the crystal lattice. The structure interestingly demonstrates the possible various forms of dmg, not only on their charge but also in different conformations upon coordination.     

混合价双核锰[Mn2(cyclen)2(μ-O)2](ClO4)3·4H2O的晶体结构和表征

The mixed-valence manganese(Ⅲ/Ⅳ) complex [Mn2(cyclen)2(μ-O)2](ClO4)3-4H2O (1) (cyclen=1,4,7,10-tetraazacyclododecan) with chemical formula C16H48Cl3Mn2N8O18 has been synthesized and characterized by single crystal X-ray diffraction analysis, elemental analysis, IR and electronic spectra. The results showed that the manganese(Ⅲ/Ⅳ) ions were six-coordinated by four nitrogen atoms from cyclen and two oxygen atoms from the oxygen bridge, forming a distorted octahedron geometry. There were two very strong peaks in the range of 400-700 nm in electronic spectrum, which was similar to Mn catalase and Mn ribonucleotide reductase extracted from organisms.Electrochemical study indicated that the complex underwent a quasi-reversible one-electron reduction and oxidation at E1/2=0.827 V in acetonitrile.     

[ZnL2Cl2]·2H2O (L = N’-苯甲酰基异烟酰肼)的合成、晶体结构及其表征

标题化合物中，锌（Ⅱ）为四配位畸变的四面体构型。通过相邻分子之间的氢键把配合物连接成三维网络结构，而且，配合物中吡啶环与苯环之间存在着面-面的π–π相互作用。配体与配合物均可发出蓝色荧光，其固态时的最大发射峰为480 nm。     

吗啉二硫代氨基甲酸铁（III）配合物Fe(S_2CNC_4H_8O)_3的合成、表征及晶体结构

合成了标题化合物Fe(S_2CNC_4H_8O)_3，得到黑色柱状晶体。晶体属三斜晶系 ，空间群为P－1，晶胞参数a=0.9300(2)nm，b=1.0490(2)nm，c=1.3710(3)nm， a=100.60(3)，γ=106.60(3)，V=1.2445(4) nm~3，M_r=542.58，Z＝2。中心Fe原 子分别来自三个吗啉二硫代氨基甲酸的六个硫原子配位形成八面体构型，由于四元 螯合环的环张力，导致该八面体严重变形，六个Fe-S键的键长范围在0.2423(5)～ 0.2458(2)nm。热分析表明标题化合物在791.80 ℃完成分解。     

[Gd(C10H9N2O4)(C10H8N2O4)(H2O)3]2·phen·4H2O的晶体结构和生物活性

在水乙醇混合溶剂中，首次得到了2-羰基丙酸水杨酰腙、1，10-菲啰啉与硝酸钆形成的配合物[Gd(C₁₀H₉N₂O₄)(C₁₀H₈N₂O₄)(H₂O)₃]₂·phen·4H₂O，并测试了其单晶结构。该配合物属三斜晶系，空间群为P-1。每个配合物分子中有两个九配位的钆的结构单元，每个钆离子与两个三齿配体2-羰基丙酸水杨酰腙（分别以负一价和负二价形式）和三个水分子配位。每个钆单元在空间呈扭曲的单帽四方反棱柱。同时还有一个游离的1，10-菲啰啉存在于晶格中，通过氢键与配位水作用。生物活性试验表明该配合物对三种病原菌有一定的抑菌活性。     

富氮配合物[Co(DAT)6](PA)2∙4H2O的制备、晶体结构和热分析

以1,5-二氨基四唑（DAT）为配体,苦味酸根（PA）为外阴离子制备得到了一种新的配合物[Co(DAT)6](PA)2∙4H2O,并通过X射线单晶衍射分析、元素分析和FT-IR分析技术对其进行了结构表征。中心钴（II）离子与六个DAT分子的六个N原子配位,形成一个六配位、略微畸变的八面体结构。配离子位于两个苯环互相平行的PA离子之间。在[Co(DAT)6](PA)2∙4H2O的分子单元中,配离子和PA离子通过静电引力连接;分子单元间通过分子间氢键连接形成配合物的晶体结构,DAT配体分子对于晶体结构的形成起到了重要作用。采用TG-DTG、DSC和FT-IR分析技术对目标化合物的热分解过程进行了研究,并采用Kissinger法和Ozawa-Doyle法对目标配合物第一放热分解过程的非等温反应动力学进行了计算。     

Synthesis and Crystal Structure of Complex: [Co(cdm)_2(H_2O)_4].2H_2O (cdm=Carbamyldicyanomethanide Anion)

1 INTRODUCTION Crystal engineering and the design of solid-state architectures have recently become areas of increasing interest[1, 2]. Such crystal engineering may afford new materials with useful properties such as catalytic activity, micro-porosity, nonlinear optical activity, cooperative magnetic behavior and so on. Polynitrile-ligand is one of the ideal multi-functional ligands for crystal engineering and many complexes with polynitriles as ligands have been found to show the spe…     

3-羧基苯氧乙酸钴配合物[Co(m-CPOAH)2(H2O)4]的合成与晶体结构

合成了一个新的配合物 [Co(m-CPOAH)2(H2O)4](m-CPOAH- = 3-羧基苯氧乙酸根), 并对其进行了元素分析、红外和单晶X-射线的表征。结果表明:配合物晶体属三斜晶系, 空间群为P, 晶胞参数为a = 4.9701(10), b = 5.8701(12), c = 18.272(4) , a = 97.50(3), b = 94.76(3), g = 98.34(3), V = 520.11(18) 3, Z = 1, Mr = 521.29, Dc = 1.664 g/cm3, m = 0.901 mm-1, F(000) = 269, 最终R = 0.0415, wR = 0.0787。2个不同配体的氧乙酸上的羧基氧原子和4个配位水分子与钴原子配位, Co(Ⅱ)原子为六配位八面体构型, 且由分子间氢键形成了三维超分子氢键网络结构。     

Synthesis and Crystal Structure of the Binuclear Complex [Pr2(C10H8N2O4)2(C10H9N2O4)2(H2O)4]·3H2O·C6H6

The binuclear praseodymium(III) complex with N‐(1‐carboxyethylidene)‐salicylhydrazide (C₁₀H₁₀N₂O₄, H₂L) was prepared in H₂O‐C₂H₅OH mixed solution, and the crystal structure of [Pr₂L₂(HL)₂(H₂O)₄]·3H₂O·C₆H₆ was determined by X‐ray single crystal diffraction. The crystal complex crystallizes in the triclinic system with space group P‐1, and in the structure each Pr atom is 9‐coordinated by carboxyl O and acyl O and azomethine N atoms of two tridentate ligands to form two stable five‐membered rings sharing one side in keto‐mode and two water molecules. The coordination polyhedron around Pr³⁺ was described as a monocapped square antiprism geometry. In an individual molecule, four tridentate ligands were coordinated by two negative univalent (HL) and two bivalent forms (L) respectively. Two negative univalent ligands were coordinated via μ₂‐bridging mode.