配合物[Cu(CAM)(H2O)2]的水热合成与结构表征

A copper(II) complex [Cu(CAM)(H₂O)₂], (CAM=4-hydroxypyridine-2,6-dicarboxylic acid), has been hydr-othermally synthesized and characterized by elemental analysis, IR, and X-ray diffraction single crystal structure analysis. It belongs to triclinic system, with space group P1, a=0.783 3(3) nm, b=0.796 5(3) nm, c=0.798 6(3) nm, α=100.340(6)°, β=93.768(6)°, γ=109.348(5)°, V=0.458 3(3) nm³, Z=2. The copper(II) ion is 5-coordinated and exhi bits a distorted square pyramidal coordination environment. The two coordinated aqueous molecules and the oxygen atoms from the ligand generate the intermolecular hydrogen bonds, which result in the 2D supramolecular network. CCDC: 227156.     

配合物[Mn(phendione)(PDC)(H2O)2]·2H2O的合成与晶体结构

The title compound [Mn(phendione)(PDC)(H₂O)₂]·2H₂O (H₂PDC=pyridine-2，6-dicarboxylic acid) has been prepared in aqueous solution and characterized by single X-ray diffraction structure determination， elemental analysis， IR spectroscopy， and thermal analyses. The compound crystallizes in Monoclinic system， space group C2/c， a=1.017 51(11) nm， b=1.483 25(11) nm， c=1.461 21(13) nm， β=109.86(10)°， V=2.074 1(3) nm³， Z=4， F(000)=1 028， μ=0.701 mm^-1， D_c=1.609 g·cm^-3， R₁=0.028 9， wR₂=0.078 8 [I>2σ(I)]. Crystal structure reveals that complex consists of one-dimensional chain framework bridged by hydrogen bonds that formed by uncoordinated water and oxygen atom of carboxyl group in PDC^2-. Furthermore， the complexes form a three-dimensional super-molecular structure through hydrogen bonds. CCDC: 648570.     

异核配合物K2[Co(Dipc)2]·7H2O的合成、性质、结构和热分解动力学研究

A heteronuclear compound, K₂[Co(Dipc)₂]·7H₂O (Dipc=pyridine-2,6-dicarboxylic acid) has been synthe- sized and characterized by IR, elemental analysis, and X-ray diffraction. Crystal data: orthorhombic system with space group Pnna and unite cell parameters: a=2.0645(3)nm, b=1.3484(2)nm, c=0.8204(1)nm; V=2.2838(6)nm³, Z=4, D_cald=1.726 g·cm^-3, μ=1.193 mm^-1, F(000)=1212, Gof=1.045, Δρ=339～-348 e·nm^-3, the final R is 0.0295. In the molecule of the complex, Co(Ⅱ) ion is six-coordinate to form a dis-torted octahedron. The N atom and the carboxyl group of pyridine-2,6-dicarboxylic acid are coordinated with the central ions. One of the carboxyl groups of the pyridine-2,6-dicarboxylic acid connect K(Ⅰ) and Co(Ⅱ). The com- pound possesses approximate C₂ symmetry. The compounds form a three-dimensional network of infinite length connection with crystal waters, potassium ions and hydrogen bonds. The result of kinetics of thermal decomposition indicated that the compound decomposition takes place in two steps. CCDC: 207078.     

[Cu(HDPC)2]·(HOx)2·6H2O的合成及晶体结构

The new complex formulated [CU(HDPC)₂]·(HOx)₂·6H₂O(HDPC^- is pyridine-2,6-dicarb-oxylate,Hoxis 8-Hydroxyquindine) 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 C2/c. a=18.423(3)Å, b=10.384(2)Å,c=19.139(2)Å, α=γ=90°, β=111.050(10)°, V=3417.0(9)ų, Z=4, D_c=1.544Mg·m^-3, μ=0.722mm^-1. In the crystal Cu(Ⅱ) ion is six coordinated to form a distorted octahedron.     

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.     

Ni(Ⅱ)离子型配合物的合成与晶体结构

吡啶-2,6-二甲酸(H2DPC)在生物体内是具有生物活性的物质,通过研究过渡金属配合物的结构来了解其在生物体内的作用,已引起人们极大的兴趣[1,2]。而镍是生物必要的痕量元素。B.Sumner于1926年从刀豆种子中提取第一种晶体酶———脲酶,1975年确定其含有金属镍[3]。镍能促进体内铁     

一维梯子状配位聚合物[Na3Er(2，6-PDA)3]·11.5H2O的合成与晶体结构

A novel 1D Ladder-like coordination polymer [Na₃Er(2，6-PDA)₃]·11.5H₂O (2,6-H₂PDA is pyridine-2,6-dicarboxylic acid) 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=0.969 7(3) nm, b=1.914 6(6) nm, c=1.8031(6) nm, β=91.524(5)°, V=3.346 6(18) mm³, Z=4, D_c=1.863g·cm^-3, μ=2.645 mm^-1. The coordination geometry configuration of Er³⁺ center is tricapped trigonal prism. The structures of the title compound exhibit a novel 1D Ladder-like chain.     

七配位二聚体配合物{(PhCH2)2Sn·[2,6-(O2C)2C5H3N](CH3OH)}2的合成及结构

在三乙胺存在下利用三苄基氯化锡和2,6-吡啶二甲酸,以1:1摩尔比反应,合成了七配位二聚体{(PhCH2)2Sn[2,6-(O2C)2C5H3N](CH3OH)}2.通过元素分析、红外光谱和核磁共振氢谱对其结构进行了表征.用X射线单晶衍射法测定了该化合物的晶体结构.化合物为三斜晶系,P1空间群,晶胞参数a=0.9625(6)nm,b=1.0947(9)nm,c=1.996(3)nm,α=90.00(2)°,β=87.69(3)°,γ=90.00(3)°,Z=2,V=2.102(6)nm3,μ=1.248mm-1,F(000)=1000,R1=0.0476,wR2=0.0782.化合物中2个锡原子呈七配位畸变五角双锥构型.生物活性测试结果表明,该化合物具有较强的体外抗肿瘤活性.     

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.     

配合物[Co(Hdhpmy)(H2O)3]·3H2O的合成、晶体结构和荧光性质

用溶液法合成了钴的配合物[Co(Hdhpmy)(H₂O)₃]·3H₂O(H₃dhpmy=4,6-二羟基嘧啶-2-硫醇乙酸),对它进行了元素分析、红外光谱、荧光等表征,并用X-射线单晶衍射测定了配合物的单晶结构。标题配位聚合物晶体属正交晶系,Pca2₁空间群。弱的π-π相互作用将单分子连接成一维链状结构,而氢键使配合物形成三维网状结构。     

新颖一维配位聚合物[Ni(3，5-pdc)(H2O)4]·(H2O)的合成与晶体结构

The hydrothermal reaction of 3,5-pyridinedicarboxylic acid and NiCl₂·6H₂O results in a novel coordination polymer， [Ni(3,5-pdc)(H₂O)₄]·(H₂O). The crystal structure of the compound was determined by X-ray single crystal diffraction. The crystal belongs to monoclinic system with space group P2₁/n, a=1.136 1(3)nm, b=0.709 8(2) nm, c=1.459 7(4) nm, β=107.538(4)°， V=1.122 4(6) nm³, D_c=1.858 g·cm^-1, Z=4, F(000)=648, R₁=0.0264, wR₂=0.0665. CCDC: 224880.     

含二维水网的三维超分子[Ni(phen)2(H2O)2][Ni(PDC)2]•7H2O

在水溶液中合成了离子型配合物[Ni(phen)₂(H₂O)₂][Ni(PDC)₂]•7H₂O (H₂PDC＝吡啶-2,6-二甲酸, phen＝1,10-菲啰啉). 通过元素分析、红外光谱、单晶X射线衍射以及热重分析对配合物进行了表征. 晶体数据解析表明, 化合物属于三斜晶系, 空间群为P1, a＝1.0092(4) nm, b＝1.4599(6) nm, c＝1.4933(5) nm, α＝73.982(2)°, β＝78.652(2)°, γ＝75.184(3)°, V＝2.0256(13) nm³, Z＝2, F(000)＝1004, μ＝1.014 mm^－1, R₁＝0.0538, wR₂＝0.1493. 配合物中的结晶水分子形成一个(H₂O)₁₂水簇, (H₂O)₁₂水簇通过氢键连接为二维水网, 最终构成三维超分子网络.     

含二维水网的三维超分子[Ni(phen)2(H2O)2][Ni(PDC)2]•7H2O

在水溶液中合成了离子型配合物[Ni(phen)₂(H₂O)₂][Ni(PDC)₂]•7H₂O (H₂PDC＝吡啶-2,6-二甲酸, phen＝1,10-菲啰啉). 通过元素分析、红外光谱、单晶X射线衍射以及热重分析对配合物进行了表征. 晶体数据解析表明, 化合物属于三斜晶系, 空间群为P1, a＝1.0092(4) nm, b＝1.4599(6) nm, c＝1.4933(5) nm, α＝73.982(2)°, β＝78.652(2)°, γ＝75.184(3)°, V＝2.0256(13) nm³, Z＝2, F(000)＝1004, μ＝1.014 mm^－1, R₁＝0.0538, wR₂＝0.1493. 配合物中的结晶水分子形成一个(H₂O)₁₂水簇, (H₂O)₁₂水簇通过氢键连接为二维水网, 最终构成三维超分子网络.     

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.     

配合物[Cu(H2biim)2]Br2的合成和晶体结构

The complex [Cu(H₂biim)₂]Br₂ (H₂biim=2,2′-biimdazole) has been synthesized and structurally charac-terized. It crystallizes in the Monoclinic system, space group C2/c with a=1.422 5(4) nm, b=0.931 2(2) nm, c=1.343 1(3) nm, β=116.227(4)°, V=1.595 9(7) nm^-3, R₁=0.060 2, wR₂=0.152 8 and Z=4. The copper ion has a sligh-tly distorted square planar coordination configuration with four nitrogen atoms from two H₂biim ligands. The complex has a one-dimensional chain structure, which is formed by hydrogen bonds and semi-coordinate bonds. CCDC: 624679.     

配合物[Sm(o-MOBA)3(phen)·H2O]2·4H2O的合成与晶体结构

The title complex [Sm(o-MOBA)₃(phen)·H₂O]₂·4H₂O has been synthesized by the reaction of SmCl₃·6H₂O with o-methoxybenzoic acid and 1,10-phenanthroline in 1∶3∶1 molar ratio. The crystal structure was determined by X-ray single crystal diffraction. The crystal belongs to triclinic system, space group P1 with a=1.203(10) nm, b=1.293(10) nm, c=1.306(11) nm, α=64.50(10)°, β=81.93(10)°, γ=74.81(10)°. The molecular structure shows that the Sm³⁺ ion coordinates to nine atoms. The carboxylate groups are bonded to the samarium ion in three modes: monodentate, bidentate chelating, tridentate chelating-bridging. CCDC: 603740.     

一个双核镍配合物[Ni2(Htda)2(H2O)6]·4H2O的合成、晶体结构和性质

双核金属配合物对于生物化学和磁化学都是非常重要的。在本文中,1,2,3-三氮唑-4,5-二羧酸(H₃tda)配体和硝酸镍在常温常压下反应得到了1个三氮唑桥联的双核镍配合物[Ni₂(Htda)₂(H₂O)₆]·4H₂O (1),并通过元素分析、红外光谱、X-射线单晶衍射、热重分析以及超导量子干涉仪(SQUID)对其晶体结构和磁、热性质进行了表征。晶体数据表明该配合物属三斜晶系,空间群为P1。在配合物1中,2个1,2,3-三氮唑-4,5-二羧酸配体利用2个相邻的氮原子桥联2个金属镍离子形成一个双桥的双核镍配合物。这些双核镍单元又通过体系中存在的大量的氢键相互作用形成了三维超分子骨架。磁性分析显示双核镍单元内镍镍之间存在反铁磁相互作用。     

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.     

双核镍配合物[Ni2(p-PhDTA)(2,2′-bipy)2(H2O)2]·4H2O的合成与晶体结构

A novel dinuclear complex of [Ni₂(p-PhDTA)(2,2′-bipy)₂(H₂O)₂]·4H₂O (p-PhDTA^2-=para-phenylenediamine-N,N,N′,N′-tetraacetate)has been synthesized. The complex was characterized by elemental analysis, IR spectra, thermo-analysis and X-ray diffraction. The crystal belongs to triclinic, space group P1 with a=0.976 3(7)nm, b=0.989 41(7) nm, c=1.084 29(8) nm, α=65.661 0(10)°, β=75.234 0(10)°, γ=85.616 0(10)°, Z=2, V=0.925 44(12) nm³, D_c=1.568 g·cm^-3, R₁=0.031 5, wR₂=0.081 4. In the complex, the central Ni(Ⅱ) ion is coordinated in a distorted octahedral geometry, defined by two carboxyl O atoms and one N atom from same p-PhDTA^2- group, two N atoms from 2,2′-bipyridine ligand and one water molecule. The two nickel (Ⅱ) ions are linked by p-PhDTA^2- group into a dinuclear structure and extensive hydrogen bonds link the complex into a 2D supramolecular network. CCDC: 294084.     

吡啶-2，3，5，6-四甲酸镉配合物[Cd(H2PTA)(H2O)3]·3H2O的合成与晶体结构

吡啶羧酸是一类非常有趣、灵活多变的配体,它能与过渡金属离子和稀土金属离子配位形成稳定的配合物,而且配位方式不拘一格.