Synthesis and Crystal Structure of a Copper(Ⅱ) Complex with 2,4-Dihydroxybenzylidene Benzoylhydrazone Ligand

A new copper(Ⅱ) complex with formula CuL(py), where L2- is the dianion of 2,4-dihydroxybenzylidene benzoylhydrazone, has been synthesized and characterized by IR spectra and single-crystal X-ray diffraction method. The crystal belongs to monoclinic, space group P21/c with a = 0.9630(4), b = 1.4808(6), c = 1.2320(5) nm, β= 104.969(6)°, V= 1.6973(11)nm3, Z = 4, Dc = 1.553 g/cm3, μ(MoKa) = 1.311 mm-1, F(000) = 812, R = 0.0694 and wR = 0.1727 for 1511 observed reflections (I ＞ 2σ(Ⅰ)). The crystal structure analysis indicates that the copper(Ⅱ) ion lies in a distorted square-planar environment composed of two oxygen atoms, one nitrogen atom from the tridentate acylhydrazone Schiff base ligand L2- and one nitrogen atom teractions to form dimers, which are further linked to generate a two-dimensional layer structure via interdimeric hydrogen bonds.     

铜配合物[CuL_2Cl_2]·4H_2O的合成和晶体结构(L=3-乙基-4-对甲氧苯基-5-(2-吡啶基)-1,2,4-三氮唑)

A new copper(Ⅱ)complex,[CuL_2Cl_2]·4H_2O,[L=3-ethyl-4-(p-methoxyphenyl)-5-(2-pyridyl)-1,2,4-triazole],was synthesized and characterized by X-ray crystallography and infrared spectroscopy.The complex crystallizes in triclinic system with space group P(1),α=0.843 9(7)nm,b=0.965 5(8)nm,c=1.093 6(8)nm,α=84.026(19)°,β=82.33(2)°,γ=89.167(19)°,V=0.878 3(12)nm~3,Z=1 with final R=0.033 8.The copper atom lies in a distorted octahedral environment with two bidentate chelating ligands(L)in the equatorial plane and two Cl~- ions in the axial positions.The ligand L coordinates via one triazole nitrogen and one pyridine nitrogen atom.The molecules are stabilized by intermolecular hydrogen bonds in the crystal lattice.CCDC:705817.     

Syntheses and Crystal Structures of Mono-and Binuclear Copper(Ⅱ) Mixed-ligand Complexes Involving Schiff Base

1 INTRODUCTION The chemistry of copper compounds has been extensively investigated and the relationship be- tween structure and reactivity, ranging from indus- trial catalysis to biochemistry activity, is of major importance. For binuclear copper(II) complexes equa- torially bridged by pair of hydroxide[1] or alkoxide[2, 3] groups, satisfactory linear correlation is found be- tween the Cu–O–Cu bridging angle and spin coupling between the metal centers. However, for binuclear copper(I…     

Synthesis and Crystal Structure of Dicyanamide(5,7,7,12,14,14-Hexamethyl-1,4,8,11-tetraazacyclotetradecane) Copper(II) Percholatehydrate

1 INTRODUCTION Recently the chemistry of transition metal com- plexes containing macrocyclic ligand has become in- creasingly important[1～12]. However, the structurally characterized transition metal complexes containing macrocyclic ligand teta are stil…     

铜配合物[CuL2(ClO4)2]的合成、晶体结构及热稳定性(L=3-对溴苯基-4-对甲苯基-5-(2-吡啶基)-1，2，4-三氮唑)

以3-对溴苯基-4-对甲苯基-5-(2-吡啶基)-1,2,4-三氮唑(L)作为配体,合成了1个铜配合物trans-[CuL2(ClO4)2],对其进行了红外、电喷雾质谱、热重分析和单晶结构表征,该配合物属于三斜晶系,空间群P1,a=0.829 29(15)nm,b=0.854 48(16)nm,c=1.502 7(3)nm,α=83.517(2)°,β=89.200(2)°,γ=73.064(2)°,V=1.011 9(3)nm3,Z=1,R1=0.041 2。单晶结构表明,铜离子处于1个扭曲的八面体配位环境中,2个高氯酸根离子呈反式配位,每个配体L通过三氮唑上的1个氮原子和吡啶氮原子参与配位。热重分析表明该配合物在310℃开始发生分解。     

氮杂大环双核铜锌金属配合物的合成结构及溶液中配位稳定性研究

在合成模型化合物之前 ,有必要先了解合成的大环配体在溶液中与金属离子的配位行为及其稳定性 ,以便选择不同结构的大环配体和控制反应的 p H值合成出结构和催化性能较好的模型化合物 [1～ 3] .本文报道了大环配体与 Cu( )和 Zn( )形成的配合物 ,对其结构和溶液中的配位稳定性进行了研究 .1　实验部分1 .1　试剂与仪器配体 L以 2 ,6-吡啶二甲醛和二乙烯三胺为原料 ,按文献 [4]报道的方法经 2 + 2合成得到 .其纯度经元素分析、红外光谱、核磁共振氢谱和质谱鉴定 .其它试剂均为分析纯 . p H滴定采用二次蒸馏水 .Perkin- Elmer 2 4 0型元…     

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.     

由间苯二甲酸和Medpq配体构筑的一种新型零维铜(Ⅰ)的配合物的水热合成及晶体结构测定

A metal-organic Complex [Cu₂(ipt)(Medpq)₂]_n (ipt=isophthalic acid, Medpq=2-methyldipyrido[3,2-f:2′,3′-h]quinoxaline) 1 has been hydrothermally synthesized and structurally characterized by elemental analysis, IR spectrum, TG and single-crystal X-ray diffraction. Title compound crystallizes in the monoclinic system, space group C2/c, with a=2.389 2(6) nm, b=0.709 60(18) nm, c=1.922 2(5) nm, β=108.655(3), V=3.087 8(14) nm³, C₃₈H₂₄Cu₂N₈O₄, M_r=783.73, D_c=1.686 g·cm^-3, Z=4, the final R=0.055 4 and wR=0.128 5. In the crystal structure, the copper atom is three-coordinated with one carboxylate oxygen atom from carboxylate groups and two nitrogen atoms from Medpq ligand, showing a slightly distorted triangle geometry. Furthermore, it exhibits a zero-dimensional structure with ipt-Cu- medpq as building units. CCDC: 747544.     

2-(1H-1,2,4-三氮唑)乙酸Cu(Ⅱ)配合物的水热合成、晶体结构及性质

A copper(Ⅱ) complex [CuL2] [L=2-(1H-1,2,4-triazol-1-yl)acetic acid] has been synthesized by means of hydrothermal method, and characterized by elemental analysis, IR spectra and X-ray diffraction. Crystal data for this complex: monoclinic, space group P21/n, a=0.481 3(2) nm, b=1.151 1(6) nm, c=0.993 9(5) nm, β=100.528(8)°, V=0.541 4(5) nm3, Z=2, F(000)=318, Dc=1.937 g·cm-3, Final GooF=1.109, R1=0.027 6, wR2=0.075 6. The crystal structure shows the copper(Ⅱ) atom is six-coordinated by two triazole nitrogen atom and four carboxylate group oxygen atom from four distinct L- ligand, thereby forming a 2D network structure. The cyclic voltammetric behavior of the complex was described.     

3-甲基-4-对甲基苯基-5-(2-吡啶基)-1，2，4-三唑双核锰(Ⅱ)配合物的合成及晶体结构

A dinuclear Mn(Ⅱ) complex [Mn₂L₂(μ-Cl)₂Cl₂(H₂O)₂] (1) was synthesized by reaction of ligand L with MnCl₂ ·4H₂O 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=2.018 0(15) nm, b=0.894 0(6) nm, c=1.932 1(14) nm, β=97.506(12)°. V=3 456(4) nm3, Z=4, D_c=1.515 Mg·m^-3, μ=1.081 mm^-1, F(000)=1 608, and final R₁=0.043 8, wR₂=0.109 9. The result shows a Mn(Ⅱ) ion was six-coordinated by a bidentate 3-methyl-4-( p-methylphenyl)-5-(2-pyridyl)-1,2,4-triazole, one chlorine and one bridging chlorine atom in the basal positions and one chloride atom and one water molecule in the axial one, to form a distorted octahedral-pyramidal geometry. CCDC: 713047.     

Synthesis and Crystal Structure of a New Complex [CuL(Phen)]·NO3

A new mononuclear copper(Ⅱ) complex [CuL(Phen)]·NO3 (L = 2-{2-[(3,5-dibro- mosalicylidene)amino]ethyl}-1H-1,3-benzimidazole, Phen = 1,10-phenanthroline) has been synthe-sized and its crystal structure was determined by X-ray diffraction method. It crystallizes in mono- clinic, space group C2/c with a = 24.966(7), b = 15.673(4), c = 16.600(5) (A), β = 123.981(4)o, C28H20Br2CuN6O4, Mr = 727.86, V = 5386(2) (A)3, Z = 8, Dc = 1.795 g/cm3, μ(MoKα = 3.826 mm-1, F(000) = 2888, the final R = 0.0508 and wR = 0.1024 for 5440 independent reflections with Rint = 0.1134. The title compound is composed of [CuL(Phen)]+ cation and NO3- anion. The coordination geometry around copper atom is a highly distorted trigonal bipyramid consisting of one benzi-midazole nitrogen atom, one phenolato oxygen atom and one phenanthroline nitrogen atom on the equatorial plane together with one imine nitrogen atom and one phenanthroline nitrogen atom occupying the axial positions. The hydrogen bonding and π-π stacking interactions link the copper complex molecules into a 3-D supramolecular structure.     

Syntheses and Crystal Structures of Mono- and Binuclear Copper( Ⅱ ) Mixed-ligand Complexes Involving Schiff Base

The mononuclear copper(Ⅱ) complex [Cu(L)(2-AP)] 1 and binuclear copper(Ⅱ)complex [Cu(L)(py)]2 2 (L = C1oH1 1O5NS, taurine o-vanillin, py = prydine, 2-AP = 2-aminopyridine)with mixed ligand have been synthesized and characterized by X-ray diffraction method. Crystal data for 1: orthorhombic, space group Pbca with a = 11.921(4), b = 15.816(6), c = 17.076(6) (A), V=3219.7(19) (A)3, C15H17CuN3O5S, Z = 8, Mr = 414.92, Dc = 1.712 g/cm3,μ(MoKα) = 1.520 mm-1,F(000) = 1704, the final R = 0.0300 and wR = 0.0705 for 2840 observed reflections with I ＞ 2σ(I);and crystal data for 2: monoclinic, space group P21/c with a = 7.929(3), b = 17.038(5), c = 11.734(4)(A), β = 98.162(6)°, V = 1569.1 (9) (A)3, C15H16CuN2O5S, Z = 4, Mr = 399.90, Dc = 1.693 g/cm3, F(000)= 820,μ(MoKα) = 1.554 mm-1, the final R = 0.0351 and wR = 0.0848 for 2767 observed reflections (I ＞ 2o(I)). The molecular structure of complex 1 consists of one tetra-coordinated Cu(Ⅱ) atom generating a slightly distorted square plane, and a one-dimensional chain structure is formed by intermolecular hydrogen bonds. Complex 2 consists of a diphenolic hydroxyl O-bridged binuclear copper(Ⅱ) structure. The crystal structures of complexes 1 and 2 reveal that the coordinate copper centers are bound to both nitrogen and oxygen atom donors. The usual N,O-trans arrangement of ligands is observed in both cases.     

Synthesis,Structure and Fluorescence of a Copper(II) Complex [Cu_2(bipy)_2(Hpht)_2Cl](Hpht)(bipy=2,2'-Bipyridine,H_2pht=o-Phthalic Acid)

1 INTRODUCTION o-Phthalic acid (H2pht) is a versatile ligand for co-ordinating to metal ions in various modes, such asmonodentate bonding through a carboxylic O atom[1],bidentate fashion via two carboxylic O atoms[2] andtriple coordination through its three carboxylic Oatoms[3], and bridging mode with two or four Oatoms of its carboxylate groups[4]. The coordinationproperties thus allow for the preparation of complex-es with a large variety of architectures, forming iso-lated mono-, di…     

(C5H7S2)2[Cu3I5]的合成和晶体结构

我们曾经对二硫代乙酰丙酮和多种金属离子的配合反应进行了系统的研究.在成功合成(C_5H_7S_2)_2[CuBr_3]的基础上,最近我们试图用类似方法合成(C_5H_7S_2)[CuI_3].但对产物晶体的X 射线衍射分析结果却表明,所得到的化合物的分子式为(C_5H_7S_2)_2[Cu_3I_5].[Cu_3I_5]~(2-)是以[CuI_3]配位三角形和两个相邻[CuI_4]配位四面体连接的无限链状配合阴离子形式存在.     

配合物Cu(C14H9NO3)(C3H4N2)的合成、晶体结构及性质研究

合成了配合物Cu(C₁₄H₉NO₃)(C₃H₄N₂)[C₁₄H₉NO₃^2- 为N-(2-羧基苯基)-水杨醛亚胺,C₃H₄N₂为咪唑].晶体属正交晶系,空间群Pca2₁,晶胞参数a=0.94453(12)nm,b=1.12278(9)nm,c=2.9123(4)nm,V=3.0885(6)nm³,Mr=370.84,Z=8,最终的偏离因子R=0.036,wR=0.087,GOF=0.975.三齿Schiff碱配体中的二个氧原子、一个氮原子和咪唑的一个氮原子与铜原子配位,形成扭曲的平面正方形结构.通过元素分析,IR,UV,CV和TG表征了配合物的结构.     

四聚体手性配合物｛［Cu(C20H26N4O2)Cl］Cl·4H2O｝4的合成及晶体结构

将L-苯丙氨酸与乙二胺通过一定反应双缩得到具有手性结构的N,N′-双(L-苯丙氨酸)缩乙二胺, 此配体与氯化铜发生配位, 生成一种四聚体手性Cu(Ⅱ)配合物, 将此配合物溶在甲醇中培养出单晶. 通过X射线衍射分析测得其分子结构. 此配合物单晶属于四方晶系, 空间群I4. 晶胞参数为a=2.504 4(4) nm, b=2.504 4(4) nm, c=0.870 7(3) nm, V=5.461(2) nm 3, Dc=1365 g/cm3, Z=8.     

钒氧配合物[VOL(C9H6NO)]·CH2Cl2的合成与晶体结构

A oxovanadium(Ⅴ) complex of [VOL(C₉H₆NO)]·CH₂Cl₂[H₂L=2-hydroxy-1-naphthaldehyde 4-methoxy-benzoylhydrazone, C₉H₆NO^-=8-hydroxyquinoline anion] has been synthesized and characterized by elemental analyses, IR and single crystal X-ray diffraction. The crystal crystallizes in triclinic system, the space group is P1, with the crystal cell parameters a=1.087 0(2) nm, b=1.107 1(2) nm, c=1.269 3(3) nm, α=67.84(3)°, β=79.26(3)°, γ=73.85(3)° and V=1.353 1(6) nm³ , M_r=614.34, R=0.0503, wR=0.1409. The V(Ⅴ) atom is six-coordinated by one O atom of oxo group, two O atoms and one N atom of the tridentate hydrazone ligand, as well as one N atom and one O atom of 8-hydroxyquinoline ligand, thus defining a distorted octahedral VO(ONO)(NO) geometry. A two-dimensional supramolecular layer structure is formed through π-π stacking interactions. CCDC: 268672.     

Coordination chemistry of amine bis(phenolate) cobalt(II), nickel(II), and copper(II) complexes

Cobalt(II), nickel(II), and copper(II) (1, 2, and 3) complexes of the dianionic form of the bis(phenolate) ligand N,N-bis(3,4-dimethyl-2-hydroxybenzyl)-N',N'-dimethylethylenediamine (H2L) have been synthesized by electrochemical oxidation of the appropriate metal in an acetonitrile solution of the ligand. When copper is used as the anode, the addition of 1,10-phenanthroline to the electrolytic phase gave rise to a different compound [CuL]2.2CH3CN (4). The compounds [CoL]2.2CH3CN (1), [Ni2L2(H2O)].H2O (2), [CuL]2.3H2O (3), and [CuL]2.2CH3CN (4) were characterized by microanalysis, IR, electronic spectroscopy, FAB mass spectrometry, magnetic measurements and by single-crystal X-ray diffraction. The crystal structures show that the complexes have a dinuclear structure. In compounds 1, 3, and 4, two metal ions are coordinated by the two amine nitrogens and the two phenol oxygen atoms of a deprotonated pendant phenol ligand, with one phenolic oxygen atom from ligand acting as a bridge. In compounds 1 and 3, each metal center has a geometry that is closest to trigonal bipyramidal. Magnetic susceptibility data for both compounds show an antiferromagnetic coupling with 2J = -15 cm(-1) for the cobalt(II) complex and a strong antiferromagnetic coupling with 2J = -654 cm(-1) for the copper(II) complex. However, in 4 the geometry around the metal is closer to square pyramidal and the compound shows a lower antiferromagnetic coupling (2J = -90 cm(-1)) than in 3. The nickel atoms in the dimeric compound 2 are hexacoordinate. The NiN2O4 chromophore has a highly distorted octahedral geometry. In this structure, a dianionic ligand binds to one nickel through the two amine nitrogen atoms and the two oxygen atoms and to an adjacent nickel via one of these oxygen atoms. The nickel atoms are linked through a triple oxygen bridge involving two phenolic oxygens, each from a different ligand, and an oxygen atom from a water molecule. The two nickel ions in 2 are ferromagnetically coupled with 2J = 19.8 cm(-1).     

基于3-甲基-4-对溴苯基-5-(2-吡啶基)-1，2，4-三氮唑的锰配合物的合成和晶体结构

以3-甲基-4-对溴苯基-5-(2-吡啶基)-1,2,4-三氮唑作为配体(L),合成了1个新的锰配合物[MnL2(NCS)2],对其进行了红外、电喷雾质谱和单晶结构表征,该配合物属于单斜晶系,空间群P21/n,a=1.6480(2)nm,b=0.90707(13)nm,c=2.1919(3)nm,β=97.454(2)°,V=3.248 8(8)nm3,Z=4,R1=0.043 9。单晶结构表明,锰离子处于1个扭曲的八面体配位环境中,2个硫氰根离子呈顺式配位,每个配体L通过三氮唑上1个氮原子和吡啶上1个氮原子参与配位。     

一个不对称三芳基三氮唑锰配合物的合成、晶体结构和性质研究

以3-对甲氧苯基-4-对氯苯基-5-(2-吡啶基)-1,2,4-三氮唑(L)为配体,合成了1个单核锰配合物trans-[MnL2(NCS)2],对其进行了红外、电喷雾质谱、热重和单晶结构表征,该配合物属于单斜晶系,空间群为P21/c,a=1.458 5(3)nm,b=0.915 00(18)nm,c=1.616 3(3)nm,β=101.70(3)°,V=2.112 2(7)nm3,Z=2,R1=0.058 5。单晶结构表明,锰离子处于1个扭曲的八面体配位环境中,2个硫氰根离子呈反式配位,每个配体L通过三氮唑上1个氮原子和吡啶上1个氮原子参与配位。热重分析表明该配合物在260℃开始发生分解。变温磁化率显示该配合物为顺磁性(1.8～300 K)。