“风车状”双核镉配合物[Cd2(3-PyOH)4(FBA)4]的合成、晶体结构及热稳定性

A dinuclear cadmium complex, [Cd₂(3-PyOH)₄(FBA)₄] (FBA^-=4-formylbenzoate monoanion, C₈H₅O₃, 3-PyOH=3-hydroxypyridine), was synthesized and characterized by the element analysis, IR, TG and single crystal X-ray diffraction. Each cadmium(II) ion is six-coordinated by four O atoms from three different FBA^- groups and two N atoms from two different 3-PyOH ligands, giving a distorted octahedral geometry. The two cadmium(II) atoms are bridged by two FBA- groups, with the Cd…Cd distances being 0.392 8(6) nm. In addition, there are two kinds of π-π stacking interactions between the two adjacent parallel 3-PyOH ligands in the title complex, with the Cg…Cg (Cg is the centroid of the above rings) distances of 0.361 0(5) and 0.385 2(6) nm, respectively. A two-dimensional supramolecular layer structure is constructed by intermolecular hydrogen bonds between the carboxyl O atoms of the FBA^- groups and the 3-PyOH ligands in ab plane. CCDC: 619649.     

配合物Zn(C3H4N2)2(C8H6O2Br)2的水热合成、晶体结构及性质

在140℃下,以3-溴-4-甲基苯甲酸和咪唑为配体,通过水热法在甲醇/水混合溶剂中反应24 h合成了锌(Ⅱ)配合物Zn(C3H4N2)2(C8H6O2Br)2。通过元素分析、红外光谱、热重分析和X射线粉末衍射对配合物进行了结构表征,同时用X射线单晶衍射分析确定了其晶体结构。结果表明,其晶体属单斜晶系,空间群为C2/c,晶胞参数:a=13.257(3),b=9.765(2),c=20.494(4),β=107.79(3)°,V=2526.3(9)3,Dc=1.655g·cm-3,μ=4.170mm-1,F(000)=1248,Z=4,最终残差因子R1=0.0552,wR2=0.1378。配合物为单核结构,中心锌(Ⅱ)离子与来自2个3-溴-4-甲基苯甲酸根的2个O原子及2个咪唑分子的2个N原子配位,形成了畸变的四方锥几何体。晶体内,分子间则通过N—H…O氢键作用在ab面形成了层状结构。研究了配合物的发光性质。     

混合配体配合物[Cd2(phen)4(bmal)2]·3H2O的合成与晶体结构研究

A novel binucleus mixed-ligand[Cd₂(phen)₄(bmal)₂]·3H₂O (phen=phenanthroline; bmal=benzylmalonic acid radical) has been synthesized by the reaction of phen and bmal with cadmium(Ⅱ) salt. X-ray crystal structure analysis was carried out to determine the crystal structure of the title complex. The crystal of the title complex belongs to monoclinic system with space group P2₁/c, a=1.119 1(8) nm, b=2.480 5(17) nm, c=1.063 4(8) nm, β=142.042(12)°, Z=4, V=2.887(3) nm³, D_c=1.613 g·cm^-3, R₁=0.046 2, wR₂=0.115 6, F(000)=1 424. One carboxyl of bmal is coordinated to Cd(1) with monodentate form, the others are coordinated to Cd(2) with bidentate form. The complexes form a 1-D chain structure bridged by hydrogen bonds that formed by uncoordinated water and oxygen atom of carboxyl group in bmal, the 2-D network structure was formed by π-π interaction of neighbouring phen. CCDC: 257080.     

一维链状芴酸镉配位聚合物{[Cd(C14H9O3)2]·2H2O}n的合成、晶体结构与热稳定性研究

芴的9位上2个氢原子被羟基和羧基取代可生成9鄄羟基鄄芴鄄9鄄羧酸,它是α鄄羟基乙酸的衍生物,是一种具有生理活性的植物生长整形素[1]。由于芴酸含有羟基和羧基两种不同的氧配位原子,使其又可以作为一种潜在的构筑配位聚合物的组织基元。目前,有关芴酸与金属离子形成配合物的结     

苯丙烯酸桥联的双核镉配合物[Cd(cinnamato)2(Phen)]2的水热合成和晶体结构

A cadmium complex [Cd(cinnamato)₂(Phen)]₂ was synthesized by the reaction of cinnamic acid, phenanth-roline (phen), and Cd(ClO₄)₂·6H₂O. It crystallizes in triclinic, space group P1, with a=1.142 1(13) nm, b=1.157 6(13) nm, c=2.106 1(2) nm, α=80.307(2)°, β=77.334(2)°, γ=71.630(2)°, V=2.563 4(5) nm³, D_c=1.521 g·cm^-3, Z=2, M_r=586.90, μ=0.891 mm^-1, F(000)=1 184, the final R=0.031 7, wR=0.067 5. The crystal structure shows that the cadmium ion is coordinated with two nitrogen atoms from one phen molecule and five oxygen atoms respectively from three cinnamic acids, giving a pentagonal bipyramid coordination geometry. CCDC: 687380.     

[Ni(C6H4N2)(CHC6H4O)2]配合物晶体结构及性质

The complex has been synthesized and characterized by spectroscopic techniques and single-crystal X-ray analysis. The crystal is orthorhombic ， space group P2₁2₁2₁ with a=1.6620(3)nm， b=1.7300(4)nm， c=0.5450(1)nm and Z=4. In the crystal lattice， the molecules create a two-dimensional network structure through hydrogen bonds. The C-H…O intermolecular hydrogen bonds connect the title complex to form layer super-molecular plane structure perpendicular to the axis b， with the layers stacked by the Van der Waals interaction. CCDC： 195309.     

三核镍配合物Ni3(C14H8N3O5)2(C5H5N)4的合成、晶体结构和抗癌活性

The title complex Ni₃(C₁₄H₈N₃O₅)₂(C₅H₅N)₄ has been synthesized by the reaction of 2-hydroxy-N′-(4-nitrobenzoyl)benzohydraizide with nickel acetate in pyridine solution. Its molecular structure was characterized by elemental analysis, IR spectra and X-ray crystal structure determination. Crystal data for this compound: Mono-clinic, space group P2₁/c, M_r=1 089.00, a=0.249 27(5) nm, b=0.161 40(3) nm, c=0.121 81(2) nm, β=94.59(3)°, V=4.885 2(17) nm³, Z=4, D_c=1.481 Mg·m^-3, F(000)=2 232, R₁=0.049 7, wR₂=0.106 8 (observed reflections with I>2σ(I)) and R₁=0.105 1, wR₂=0.119 4 (all reflections), GOF=1.021. The complex was evaluated for their antitumor activi-ties against two kinds of cell lines (K562 and BGC) by MTT method. A preliminary bioactivity study indicates that the complex shows distinct antitumor activity. CCDC: 627252.     

配合物{CdI(phen)(H2O)[C8H11O2(COO)]}·H2O的水热合成、晶体结构及电化学性质

One Complex{CdI(phen)(H₂O)[C₈H₁₁O₂(COO)]}·H₂O with bicycle[2.2.1]hept-2-en-5,6-dicarboxylic acid [C₇H₈(COOH)₂], hydriodic acid and 1,10-phenanthroline(phen) has been synthesized by means of hydrothermal way and characterized. It crystallizes in the triclinic space group P1, with a=0.975 4(2) nm, b=0.990 0(2) nm, c=1.319 1(3) nm, α=89.146(4)°, β=69.800(3)°, γ=68.718(3)°, V=1.105 0(4) nm³, D_c=1.914 g·cm^-3, Z=2, F(000)=620, Final R₁=0.033 2, wR₂=0.085 7, GooF=1.092. The crystal structure shows that the cadmium ion is coordinated with two oxygen atoms from one C₇H₁₀(COOH)₂ molecule, two nitrogen atoms from the 1,10-phenanthroline, one oxygen atom from one water molecule and one iodine ion, respectively, forming a distorted octahedral coordination geometry. The cyclic voltametric behavior of the complex is also reported. CCDC: 648242.     

配合物{Cd(phen)[(C6H5)2C(OH)COO]2}2·H2O的合成、晶体结构及荧光性质

羧酸配合物在配位化学中占有重要地位.羧酸配合物有丰富的拓扑结构、较高的稳定性,在磁学、光学、催化、生物等诸多领域有广泛的应用前景,羧酸配合物引起了人们广泛的兴趣和极大的关注[1～3].近年来,我们用小位阻的羧酸配体合成了一些羧酸配合物[4～6],而对于大位阻的羧酸配体体系我们研究很少.二苯乙醇酸是一种大位阻的柔性芳香羧酸,文献报道的二苯乙醇酸配合物不多[7-9].     

新颖双核铜配合物[Cu2(C7H19N3O)2(C10H8N2)](ClO4)4·H2O的合成、晶体结构及表征

生物体内由金属离子构成的水解酶的活性中心结构和催化机理是物物无机化学领域研究的热点问题[1~4].     

甲酸桥联四核锰配合物[Mn4(O2CH)4(phen)8](ClO4)4·6H2O的水热合成和晶体结构

The title compound, [Mn₄(O₂CH)₄(phen)₈](ClO₄)₄·6H₂O(1), where phen=1,10-phenanthroline, was synthes-ized and its crystal structure was determined by X-ray diffraction structure analysis. The crystal is of monoclinic, space group P2/c with a=1.928 0(16) nm, b=1.297 0(11) nm, c=2.126 4(18) nm, V=5.242 2(8) nm³, Z=2, M_r=2 347.36, D_c=1.487 g·cm^-3, μ=0.659 mm^-1, F(000)=2 400, R_int=0.043 7, R=0.052 3, wR=0.118 6. The Mn atoms are octahed-rally coordinated by two O atoms of two ligands and four N atoms of two 1,10-phenanthroline molecules. The carboxyl group coordinates to Mn(Ⅱ) in the bridging bidentate mode. CCDC: 675520.     

双核Cd(Ⅱ)配合物[Cd2(C22H14N4)2Cl2(N3)2]2·H2O的合成与晶体结构

A dinuclear Cd(Ⅱ) complex [Cdz (N3)2LzCl2]2·H2O (1) [L=4'-(4-eyanophenyl)-2,2':6',2"-terpyridine]was synthesized by reaction of ligand L with CdCl2 and NaN3 using solvothermal method and its structure was determined by X-ray crystal structure analysis. The structure indicates that the complex crystallizes in monoclinic, space group C2/c with a=1.644 5(16) nm, b=1.441 9(12) nm, c=1.9181(18) nm,β=100.349(11)°. V=4474(7) nm3, Z=2, Dc=1.570Mg·m-3,μ=1.120 mm-l, F(000)=2 100, and final R1=0.039 3, wR2=0.0811. The result shows a Cd(Ⅱ) ion was sixcoordinated by a tridentate 4'-(4-cyanophenyl)-2,2' :6',2"-terpyridine ligand and one bridging nitrogen atom of the azide group in the basal position and an chloride atom and the other bridging nitrogen atom of the azide group in the axialone, to form a distorted octahedral-pyramidal geometry. CCDC: 673291.     

配合物[Mn(C13H8N2OBr)2(C5H5N)2]·3C5H5N的结构与磁性研究

The complex [Mn(C₁₃H₈N₂OBr)₂(C₅H₅N)₂]·3C₅H₅N has been synthesized and characterized by X-Ray diffraction, IR and variable temperature (～10 to ～278K) magnetic susceptibility. X-Ray diffraction result for the single crystal shows that the crystal belongs to monoclinic, space group P2₁/c, a=1.0969(3)nm, b=2.0903(5)nm, c=2.0481(6)nm, β=97.366(6), V=4.657(2)nm³, Z=4, D_c=1.47g·cm^-3。     

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.     

有机-无机复合物[H2(PW12O40){Zn(C10H8N2)2(H2O)}]·1.5[Zn(C10H8N2)3]·1.75H2O的合成、结构及性能

An organic-inorganic hybrid complex, [H₂(PW₁₂O₄₀){Zn(C₁₀H₈N₂)₂(H₂O)}]·1.5[Zn(C₁₀H₈N₂)₃]·1.75H₂O has been synthesized hydrothermally and structurally characterized by X-ray crystallography. The crystal belongs to monoclinic, space grounp C2/c, with a=4.709 4(2) nm, b=1.431 77(7) nm, c=2.621 07(1) nm, β=90.125(4)°, V=17.673 4(2) nm³, Z=8, D_c=3.087 Mg·m^-3, F(000)=14 884, μ(Mo Kα)=16.327 mm^-1. The structure was refined to R₁=0.068 7 and wR₂=0.158 0 for 20 128 observed reflections with I>2σ(I). Single crystal structure shows that the title compound is constructed from [PW₁₂O₄₀]^3- cluster anion and [Zn(C₁₀H₈N₂)₂(H₂O)]²⁺ metal-organic complex cation, in which metal Zn(Ⅱ) cation are coordinately bonded to the terminal oxygen of Keggin polyanions. The title compound exhibits good catalytic activity for oxidation of benzaldehyde to benzoic acid. CCDC: 624772.     

双核铜配合物{Cu[μ-S2P(C2H5O)2](C10H8N2)}2的合成和晶体结构

Binuclear Copper (Ⅰ) Complex {Cu[μ-S₂P(C₂H₅O)₂](C₁₀H₈N₂)}₂ was synthesized and characterized by elemental analysis, IRand X-ray diffraction analysis.The crystal belongs to triclinic system, space group P1 with Z = 1, cell dimentions are a = 1.0613 (5), b = 1.0723 (3), c = 0.9397 (2) um, a = 111.11 (4), β = 115.57(6), γ = 85.28(2)°, V= 0.8583(6) nm³.The structure was refined to R = 0.039 and Rw = 0.042 for 2527 reflection with Ⅰ≥3σ(Ⅰ).The complex exists as a centrosymmetric dimer with a Cu-S-P-S-Cu-S-P-Schair eight-membered ring in which Cu atoms are bridged by di-μ-S-P-Sgroups.     

[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。     

一维链状镉(Ⅱ)配位聚合物{[Cd(PAc)2(4，4′-bipy)(H2O)]·4H2O}n的合成、晶体结构及热稳定性研究

A novel one-dimensional coordination polymer, {[Cd(PAc)₂(4,4-bipy)(H₂O)]·4H₂O}_n (HPAc=phenyl acetic acid, 4,4′-bipy=4,4′-bipyridine) was synthesized and characterized by element analysis, IR, TG and X-ray single diffraction crystal structure determination. It crystallizes in the monoclinic space group C2/c with a=2.088 5(4) nm, b=0.839 05(17) nm, c=1.683 5(3) nm, β=105.45(3)° and V=2.843 5(10) nm³, Z=4, M_r=628.94, F(000)=1 288, μ=0.820 mm^-1, R=0.019 9, wR=0.056 5. Each cadmium(Ⅱ) atom is seven-coordinated by four oxygen atoms from two different phenyl acetate groups and two nitrogen atoms from two 4,4′-pyridine ligands and one water molecule, forming a distorted pentagonal bipyramid coordination geometry. Adjacent cadmium(Ⅱ) atoms are bridged by 4,4′-pyridine ligand, constructing a infinite chain along the diagonal direction of ac plane. The Cd…Cd separation within the polymer is 1.164 6(4) nm. The three-dimensional supramolecular structures of the title complexes are constructed by hydrogen bonding interactions and π-π stacking interactions between the benzene rings of HPAc and 4,4′-bipy. CCDC: 616697.     

有机锡配合物{[(n-C8H17)2Sn(O2CCH2CS2NC4H8O)]2O}2的合成，表征及晶体结构

The title complex {[(n-C₈H₁₇)₂Sn(O₂CCH₂CS₂NC₄H₈O)]₂O}₂ has been synthesized by the reaction of (morpholinylthiocarbamoylthio)acetic acid with the di-n-octyltin oxide in 1∶1 molar ratio. The complex was characterized by elemental analysis, IR and ¹H NMR. The crystal and molecular structure of complex was determined by X-ray single crystal diffraction. The crystal belongs to triclinic system with space group P1 and unit cell dimensions: a=1.201 5(9) nm, b=1.481 8(11) nm, c=1.894 1(14) nm, α=72.485(10)°, β=88.586(10)°, γ=66.893(9)°, and Z=1, μ=1.034 mm^-1, V=2.941(4) nm³, D_c=1.295 g·cm^-3, F(000)=1 196, R₁=0.058 8, wR₂=0.155 8. The complex is a centrosymmetric structure with a four-membered central endo-cyclic Sn₂O₂ unit in which two bridged oxygen atoms both connect with an exo-cyclic tin atom. The endo-cyclic tin atoms and the exo-cyclic tin atom are all five-coordinate and have coordination geometry of distorted trigonal bipyramid with an additional weak coordination carboxylate oxygen. Four carboxylate ligands are divided into two types. And two of them are monodentate and connecting to each of exo-cyclic tin atoms by using one oxygen atom, whereas the others bridge to each pair of exo-and endo-cyclic tin atoms utilizing one oxygen atom. CCDC: 277048.     

三氯化锑和二氧杂环己烷配合物[SbCl3·{(CH2)4O2}1.5]的合成与晶体结构

New solid complex of the antimony trichloride and dioxane was obtained th rough a reaction of the dioxane and the absolute methanol solution of the antimony trichloride.The formula of the complex is[SbCl₃·{(CH₂)₄O₂}_1.5].The crystal structure of the complex belongs to cubic system,space group I-43d,a=17.1417(5)Å,Z =16.The trivalent antimony ion n ot only bonds directly to three chlorine anions,but also is coordinated by three oxygen atoms of th e dioxane molecules.Two oxygen atoms in a dioxane molecule will coordinate to different antimony ions,respectively.