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。     

一维梯状配合物{[Cu2(4,4''-bpy)3(p-Ab)2(H2O)2]·(NO3)2·4H2O}n的晶体结构

合成了一维分子梯状配合物{[Cu2(4,4'-bpy)3(p-Ab)2(H2O)2]·(NO3) 2·4H2O}n(4,4'-bpy=4,4'-联吡啶,p-Ab-=对氨基苯甲酸根离子),该配合物晶体属单斜晶系,P2(1)/c空间群,晶胞参数:a=1.110 7(5) nm,b=1.550 4(3) nm,c=1.450 9(3) nm,β=104.81(3)°,V=2.415 5(12) nm3,Z=2.铜离子周围有3个氧原子和3个氮原子与之配位,其中2个氧原子由对氨基苯甲酸的螯合氧原子提供,另一个氧原子由配位水提供,3个氮原子分别由三个4,4'-联吡啶提供.这六个原子在铜离子周围形成一个畸变的八面体配位环境.配体对氨基苯甲酸只有一种配位形式--双齿螯合,第二配体4,4'-联吡啶的两个氮原子均参与配位,将配合物组装成一维分子梯结构.     

配合物Fe(pda)2(H2O)4和[FeCo(pda)4(H2O)4]n的合成与晶体结构

采用水热法合成了2个3-(3-吡啶基)丙烯酸的配合物:Fe(pda)2(H2O)4(1)和[FeCo(pda)4(H2O)4]n(2)(pda=3-(3-吡啶基)丙烯酸),用红外光谱、元素分析、热重-差热以及X-射线衍射单晶结构分析进行了表征.2个配合物都属于单斜晶系,配合物1的空间群为P21/n,配合物2的为P21/c.配合物1是一个pda配体中仅吡啶基氮原子参与配位、而羧基上的氧原子未参与配位的单核结构,通过大量的氢键作用形成三维超分子体系.2是pda配体桥联Fe和Co的异核二维层状配位聚合物;配体吡啶基上的氮原子和羧基上的氧原子都参与了配位,其中羧基采用单齿配位模式.     

2-氨基苯并噻唑和苯氧乙酸衍生物的铜配合物：位模式和抗菌性能

以苯氧乙酸(Hpa)、对硝基苯氧乙酸(Hpnpa)和对甲基苯氧乙酸(Hpmpa)为原料,分别与2-氨基苯并噻唑(aben)和乙酸铜反应,合成了3种铜配合物[Cu(pa)2(aben)2](1),[Cu2(pnpa)4(aben)2](2)和[Cu(pmpa)2(aben)2].[Cu2(pmpa)4(aben)2](3),并通过元素分析、红外光谱和单晶X-射线衍射对其结构进行了表征。结果表明,3种配合物具有不同的配位模式,配合物1的中心Cu(Ⅱ)分别与2个羧基氧原子和2个噻唑环上的氮原子配位;配合物2的2个Cu(Ⅱ)则分别都与来自4个不同配体的羧基氧原子和1个噻唑环上的氮原子配位,从而在分子中形成了2个近乎垂直的八元环;配合物3为混配型化合物,1个Cu(Ⅱ)的配位数为4,另外2个Cu(Ⅱ)的配位数为5,参与配位的配体原子分别与配合物1和2相同。最低抑菌浓度的测定结果表明,3种配合物对真菌都表现出良好的抑制作用,且由于苯氧乙酸配体中取代基种类的不同,而使得配合物的抗菌效果出现明显的不同。     

以二羧基苯氧乙酸为配体的一维钆(Ⅲ)配位聚合物的合成及晶体结构

利用Williamson合成法合成了3,5-二甲氧酰基苯氧乙酸甲酯(ML),并以之作为配位前驱物与氯化钆在水热条件下发生原位水解-配合反应,得到了3,5-二羧基苯氧乙酸(H3L)与Gd髥形成的一维配位聚合物[H3L2Gd(H2O)4]n,用X-射线单晶衍射法对其进行了结构表征。测定结果表明,该配合物结晶于单斜晶系,C2/c空间群,晶胞参数:a=1.534 4(3)nm,b=2.074 9(3)nm,c=0.716 08(16)nm,β=103.49°,V=2.216 90(225)nm3,Z=4,Dc=2.117 01 g.cm-3。Gd(III)金属中心处于扭曲的双帽三棱柱配位几何构型的中心,与来自4个配体的4个羧基氧原子结合,4个配位水分子则占据了配位环境中剩余的4个顶点。Gd髥金属中心由二齿的配体以Gd-O键连接成Ln2L4型结构单元,并进一步通过共用Gd髥金属中心的方式连接形成一维长链结构。     

铜锌异双核配合物[CuZn(fsan)(H_2O)]·H_2O的合成、晶体结构和电化学性质

合成了标题化合物[CuZn(fsan)(H2O)]H2O [H4(fsan)为N, N?- 二(3-羧基水杨醛叉)缩乙撑二胺],用单晶X-ray衍射法测定了它的晶体结构,该晶体属单斜晶系,空间群P21/n,a = 11.695(2), b = 14.646(3), c = 12.265(3) ? ?= 118.46(3)°, V = 1847.0(6) ?,C18H12CuN2O8Zn, Mr = 513.21, Z = 4, Dc = 1.846 g/cm3, (MoK? = 2.502mm-1,F(000) = 1028,R = 0.0478,wR = 0.0902 (I>2(I)), 2951个可观测衍射点。该分子结构为双核单元,铜原子位于“内部”由2个氮原子和2个酚氧原子构成的平面正方场中。“外部”锌原子与2个酚氧原子、2个端基羧氧原子及轴向水分子中的氧原子配位,锌原子处于变形四方锥几何构型之中。金属原子通过2个酚氧原子桥联在一起。结合晶体结构对配合物做了电化学研究。     

利用氧化加成反应合成[Cu(C_6H_5COO)_2(C_5H_5N)_2(H_2O)]

室温下 ,金属铜粉和过氧化苯甲酰进行氧化加成反应合成了铜化合物 [Cu(C6H5COO) 2 (C5H5N) 2 (H2 O) ](1 )。通过元素分析、电导、红外光谱等方法对配合物进行了表征 ,并经X 射线单晶结构分析确定了配合物的结构 ,晶体属单斜晶系 ,空间群Cc ,a =0 .60 78(4) ,b =1 .5879(4) ,c =2 .30 91 (3)nm ,β =97.61 (2 )°,Z =4,V =2 .2 0 91nm3,R =0 .0 30 7,中心铜原子由单齿配位的苯甲酸根的氧原子和吡啶的氮原子及来自水分子的氧原子形成四方锥配位结构。     

由己二酸根桥联的新颖双U形四核铜配合物:[Cu4(phen)4(NO3)2(H2O)2(adip)4/4(Hadip)4/2](NO3)2·2H2O

邻菲罗啉、己二酸和硝酸铜在水溶液中反应得到一种新颖的四核铜配合物[Cu4(phen)4(NO3)2(H2O)2-(adip)4/4(Hadip)4/2](NO3)2·2H2O(其中H2adip=己二酸),并经元素分析,IR,UV,TG和X射线单晶衍射分析表征.该配合物晶体属三斜晶系,P-1空间群,a=1.0146(2)nm,6=1.0261(2)nm,c=1.8285(4)nm,a=91.66(3)°,β=92.19(3)°,γ=112.76(3)°,V=1.7520(6)nm3,Z=1,Dc=1.639 g/cm3,c66H66Cu4N12O28,Mr=1729.47,F(000)=886,μ=1.294mm-1,R1和wR2分别为0.0447和0.1141.己二酸根通过4个羧基O将两个U形双核亚单元联接成具有一个对称中心的双U形四核结构,其中每个U型亚单元包含晶体学上不对称的2个Cu(Ⅱ)原子.每个Cu(Ⅱ)离子均处于畸变的四方锥配位环境,除与己二酸氢根(Hadip)、己二酸根(adip)和邻菲罗啉(Phen)的N,O配位形成锥底平面外,其中的1个Cu(Ⅱ)与水配位,而另一个Cu(Ⅱ)则与硝酸根配位.配合物晶体结构中存在着广泛的氢键和π…π作用.     

溶剂对三(苯并咪唑-2-甲基)胺和间苯二胺四乙酸的铜配合物晶体结构的影响

本文利用三(苯并咪唑-2-甲基)胺和间苯二胺四乙酸为配体与硝酸铜在CH3COCH3/CH3OH/H2O混合溶液中反应得到配合物[Cu(ntb)(H2mpda)].0.5CH3COCH3.2H2O(1),在DMF/CH3OH/H2O混合溶液中反应得到配合物[Cu(ntb)(H2mpda)].DMF.CH3OH.2H2O(2)(ntb=三(苯并咪唑-2-甲基)胺,H4mpda=间苯二胺四乙酸)。2个配合物的中心的铜离子分别与1个ntb配体的4个氮原子和1个H2mpda的氧原子配位形成三角双锥的配位构型。受溶剂的影响,配合物中配体的相对位置和构象有较大的区别,配合物2的配位构型更加扭曲。两个配合物均通过氢键连接形成不同的复杂三维网络。     

铜配合物[Cu(2,2''''-bipy)(pydco)(H2O)]·4H2O的合成与晶体结构

配合物[Cu(2,2’-bipy)(pydco)(H2O)].4H2O(2,2’-bipy=2,2’联吡啶,pydco=氮氧化-2,6-二甲酸吡啶)的结构由X-射线测定,配合物属三斜晶系,P墿空间群,晶胞参数:a=0.68120(14),b=1.1850(2),c=1.2554(3)nm,α=86.06(3),β=81.60(3),γ=86.16(3)°,V=0.99854(4)nm3,Z=2。2,2’联吡啶提供两个配位原子(N1,N2),氮氧化-2,6-二甲酸吡啶提供两个配位氧原子以及一个配位水提供一个氧原子参与了配位,中心Cu(II)离子是一个畸变的四角锥结构。有趣的是,配合物的结晶水组成了一条条的水带,配合物分子正是由这些水带中的氢键连接在一起的。     

Synthesis and Structure of anti-Configuration Complex [Cu(tssb)_2]·2[(H_3O)Cl]·4H_2O

1 INTRODUCTION The complexes of amino acid Schiff base have attracted considerable attention because of their bio- activities[1, 2]. Taurine is a special amino acid in be- ings, and recently the complexes of taurine conden- sation salicylaldehyde Schiff …     

Synthesis and Crystal Structure of Mn（phen）（PhCOO）2（H2O）

1 INTRODUCTION During the last decade the manganese che- mistry has aroused great interest due to its diverse redox functions of enzymes in photosystem Ⅱ and its specially structural, magnetic and spectroscopic properties[1, 2]. A lot of manganese complexes involving carboxylate ligands have been reported, and their properties been fully explored[3, 4]. The coordination environment of the manganese site in biosystem often consists of oxygen and nitrogen atoms from the carboxylate groups…     

Synthesis and Crystal Structure of Mn(phen)(CF_3COO)(H_2O)_3·NO_3

1 INTRODUCTION The manganese(II) ion is a biologically essential element. Knowledge of its importance is increasing as more and more enzymes are found to contain manganese ions at the active center[1, 2]. The X-ray crystallographic structures of a consi…     

Synthesis and Structure of a New Copper(II) Complex Cu(C_(13)H_9N_3O_2Br)_2.H_2O

1 INTRODUCTION Owing to their biological activities and chemical/industrial versalities, considerable attention has been continually attracted to metal-hydrazine complexes. For instance, Schiff base hydrazine and its analogues have been well studied in order to better understand the action mechanism of Vitamin B6-containing enzymes[1~3]. Six-coordinated copper(Ⅱ) complexes are of considerable interest, mainly due to their coordination geometry and spectroscopic properties[4]. Due to th…     

Synthesis and Crystal Structure of a Dinuclear Cu(Ⅱ) Complex [Cu(C_(13)H_9N_2O)Cl]_2·(CH_3CN)_2 with Ligand 2-Benzimidazol

A new dinuclear copper complex, [Cu(C13H9N2O)Cl]2·(CH3CN)2 (C30H24Cl2Cu2N6O2), has been synthesized and characterized by X-ray structure determination. It crystallizes in the tricli- nic system, space group P1, with a = 7.6677(14), b = 9.2375(17), c = 11.227(2) , α = 81.338(3), β = 88.173(4), γ = 66.199(3)o, V = 718.9(2) 3, Z = 1, Mr = 698.53, F(000) = 354, Dc = 1.613 g/cm3, μ(MoKα) = 1.705 mm-1, the final R = 0.0645 and wR = 0.1364 for 2474 unique reflections with 1809 observed ones (I > 2σ(I)). In the title complex, each copper(II) atom is located at the center of a distorted tetrahedron consisting of four coordinate atoms (one nitrogen atom, two oxygen anions, and one chlorine atom). Two copper(II) atoms are bridged by two oxygen anions (O(1) and O(1a)) of two phenolates to form a Cu(II)–Cu(II) binuclear entity, and the distance between two copper(II) atoms is 3.0144(15) .     

Synthesis and Crystal Structure of a Dinuclear Cu(Ⅱ) Complex [Cu(C13H9N2O)Cl]2·(CH3CN)2 with Ligand 2-Benzimidazol

A new dinuclear copper complex, [Cu(C13H9N2O)Cl]2·(CH3CN)2 (C30H24Cl2Cu2N6O2),has been synthesized and characterized by X-ray structure determination. It crystallizes in the triclinic system, space group P1-, with a = 7.6677(14), b = 9.2375(17), c = 11.227(2) (A), α = 81.338(3),β= 88.173(4), γ = 66.199(3)°, V = 718.9(2) (A)3, Z = 1, Mr = 698.53, F(000) = 354, Dc = 1.613 g/cm3,μ(MoKα) = 1.705 mm-1, the final R = 0.0645 and wR = 0.1364 for 2474 unique reflections with 1809 observed ones (I＞ 2σ(Ⅰ)). In the title complex, each copper(Ⅱ) atom is located at the center of a distorted tetrahedron consisting of four coordinate atoms (one nitrogen atom, two oxygen anions,and one chlorine atom). Two copper(Ⅱ) atoms are bridged by two oxygen anions (O(1) and O(1a)) of two phenolates to form a Cu(Ⅱ)-Cu(Ⅱ) binuclear entity, and the distance between two copper(Ⅱ)atoms is 3.0144(15) (A).     

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。     

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…     

单核镍(Ⅱ)配合物[Ni(IDB)_2][C_6H_4(OH)COO].ClO_4.CH_3CH_2OH.H_2O的合成和晶体结构

标题配合物是由三齿配体N, N-二(2-苯并咪唑亚甲基)胺(IDB)、Ni(ClO4)2·6H2O与水杨酸钠在乙醇溶液中反应得到的紫色晶体。用X-射线衍射测定了其单晶结构。结果表明,该晶体属三斜晶系,P 空间群,化学式:C41H43ClN10NiO9,Mr = 914.01,a = 11.010(2),b = 13.800(3),c = 15.550(3) 牛 = 100.75(3),?= 102.97(3), = 107.56(3)? V = 2111.3(7) ?,Z = 2,F(000) = 952,Dc = 1.438 g/cm3,(MoK) = 0.591 mm-1,8215个独立可观测点(I>2(I))。最终偏离因子R(I>2(I)):R = 0.0591, wR = 0.1325;R(全部数据): R = 0.1302,wR = 0.1572。结构分析表明,镍(Ⅱ)分别与2个IDB配体中的苯并咪唑的4个氮和胺基的2个氮配位形成畸变的八面体构型。