一维链状超分子化合物[Cu(dafo)_2(H_2O)_2](OPA)_2的合成和晶体结构

用4,5-二氮芴-9-酮(dafo)、邻苯二甲酸和硝酸铜合成了二价铜的一维链状超 分子化合物[Cu(dafo)_2(H_2O)_2]-(OPA)_2(OPA=邻苯二甲酸一价阴离子),其结构 通过单晶X射线衍射法确定。该化合物是单斜晶系,空间群为P2(1)/c。晶胞参数： a = 0.71093(16)nm, b = 1.5724(4)nm, c = 1.5357(3)nm, α=90.000(5) °, β =102.220(4) °,γ=90.000(5) °, V = 1.6778(6)nm~3, Z = 2, F(000) = 814, M_r = 794.17, D_c = 1.527 g/cm~3, μ = 0.727 mm~(-1), R_1 = 0.0406, wR_2 = 0.0930.单晶结构分析表明该化合物具有一维链状结构,该结构是通过氢 键这种弱相互作用形成的。     

二维网状结构超分子化合物[Cu(dafo)2(H2O)2](Cl04)2的两种同分异构体的合成与表征

用4，5—二氮芴-9-酮（dafo）、邻苯二甲酸、高氯酸铜和4，5—二氯芴—9— 酮(dafo)、苯甲酸、高氯酸铜进行混和反应时分别得到亮蓝色和蓝绿色晶体，它们 的结构通过单晶X射线衍射法测定。其单晶结构表明，这两种化合物是同分异构体 ，组成都是C22H16Cl2CuN4O12。这两种化合物是通过氢键形成的具有二维网状结构 的超分子化合物，并通过元素分析、红外光谱、热分析对两种化合物进行了表征。     

二维网状结构超分子化合物[Cu(dafo)2(H2O)2](ClO4)2的两种同分异构体的合成与表征

用4,5-二氮芴-9-酮(dafo)、邻苯二甲酸、高氯酸铜和4,5-二氮芴-9-酮(dafo)、苯甲酸、高氯酸铜进行混和反应时分别得到亮蓝色和蓝绿色晶体,它们的结构通过单晶X射线衍射法测定.其单晶结构表明,这两种化合物是同分异构体,组成都是C22H16Cl2CuN4O12.这两种化合物是通过氢键形成的具有二维网状结构的超分子化合物,并通过元素分析、红外光谱、热分析对两种化合物进行了表征.     

超分子化合物[CO(bppdca)_2(HL)_2(H_2O)_2]·2H_2O]的晶体结构和性质

以N,N′-二(3-吡啶基)-吡啶-3,5-二甲酰胺(bppdca)和1,4-环己烷二羧酸(H2L)为混合配体,利用水热合成方法获得了一个三维的超分子化合物[CO(bppdca)2(HL)2(H2O)2]·2H2O],并通过元素分析、IR和单晶X射线衍射技术确定了该化合物晶体结构.结构分析表明该化合物属单斜晶系,P21/n空间群,晶胞参数a=0.820 65(6)nm,b=1.259 76(9)nm,c=2.479 11(18)nm,β=98.061 0(10)°,Z=2,V=2.537 6(3)nm3,Mr=1 111.98,Dc=1.455g/cm3,F(000)=116 2,μ=0.421mm-1,S=1.018,R=0.041 7,wR=0.102 3.晶体结构分析表明,配合物中的CoⅡ与2个bppdca配体、2个HL阴离子以及2个配位水分子形成单金属配合物.相邻的配合物通过氢键作用拓展成三维超分子框架.另外,也研究了该化合物的热稳定性、荧光性质以及光催化性质.     

配合物[NH3(CH2)4NH3]Co(hedpH2)(H2O)2的水热合成与表征(hedpH4=1-羟亚乙基二膦酸)

采用水热合成法以丁二胺作为模板剂合成了钴的有机二膦酸超分子化合物[NH3(CH2)4NH3]Co(hedpH2)2(H2O)2 [hedpH4 = 1-羟亚乙基二膦酸, CH3C(OH)(PO3H2)2]。用元素分析、红外光谱、紫外-可见光谱、热重分析以及单晶结构解析对其进行了表征。该化合物的化学式为:C8H30N2CoO16P4,Mr = 593.15,晶体属单斜晶系,空间群C2/c,晶胞参数a = 16.128(2), b = 12.427(1), c = 12.610(2) ? b = 121.389(9), V = 2157.3(4) 3, Z = 4, Dc = 1.826 g/cm3, m(MoKa) = 1.172 mm-1, F(000) = 1228。结构用直接法解出,最终偏离因子R = 0.0285, wR = 0.0747。该化合物的结构包含单核的Co(hedpH2)2- 阴离子,阴离子之间通过氢键连结形成具有空隙的三维超分子骨架结构,双质子化的丁二胺分子位于空隙中。     

Anderson-B-型多金属氧酸盐[Co(2,2-′bipy)_3]H-[Al(OH)_6(Mo_6O_(18))]·5H_2O的合成及晶体结构

以A lC l3.6H2O、Na2MoO4.2H2O、CoC l2.6H2O和2,2′-联吡啶为主要原料合成了Anderson-B-型多金属氧酸盐[Co(2,2-′b ipy)3]H[A l(OH)6(Mo6O18)].5H2O,进行了红外光谱、紫外光谱、差热分析和单晶结构测定。晶体学测定结果表明,化合物属于三斜晶系,Pī空间群,晶胞参数:a=1.216 0(2),b=1.221 5(2),c=1.780 0(4)nm,α=86.83(3)°,β=88.76(3)°,γ=89.82(3)°,V=2.639 4(9)nm3,Z=2,R1=0.079 4,wR2=0.176 6。化合物结构分析表明,在晶体学上,标题化合物分子是由1个[Co(2,2-′b ipy)3]2 配阳离子,1个H 离子,2个1/2[A l(OH)6(Mo6O18)]3-多阴离子和5个结晶水分子组成。多阴离子[A l(OH)6(Mo6-O18)]3-借助水分子和金属配离子通过超分子作用形成二维网状结构,网状结构之间又借助超分子作用形成三维无限伸展结构。差热分析表明,标题化合物的失重过程分为2步,多阴离子骨架破坏温度为547.5℃。     

超分子化合物{[2-(4-chlorophenyl)benzimidazoleH]_2~(2+)·[SbCl_5]~(2-)}_n的水热合成、晶体结构及荧光性质

采用水热法合成了一种新的超分子化合物{[2-(4-chlorophenyl)benzimidazoleH]22+.[SbCl5]2-}n.通过元素分析、红外光谱、荧光光谱及X射线单晶衍射对其结构和性质进行了测定.结构分析表明;该晶体属于单斜晶系,P21/c空间群,晶胞参数为:a=0.583 0(9)nm,b=1.612 5(3)nm,c=1.616 3(3)nm,β=94.181(2)°,Z=2,化学式为C26H20Cl7N4Sb,Mr=758.36,V=1.515 5(4)nm3,Dc=1.662 g.cm-3,μ=1.551 mm-1,F(000)=748,R1=0.089 1,wR2=0.256 8.Sb3+与其周围6个氯离子配位,构成一个6配位的畸变八面体构型,配阴离子与2-(4-氯苯基)苯并咪唑阳离子以静电引力、氢键及π-π堆积作用形成三维网状超分子化合物.荧光测试显示该化合物具有较好的光致发光性能.     

一维链状超分子化合物[Zn(dafo)2(H2O)2](NO3)2(dafo=4,5-二氮芴-9-酮)的合成、表征和晶体结构

超分子化学是分子间弱相互作用和分子组装的化学,近年来超分子晶体日益受到重视,超分子化合物在材料,催化,药物等领域有广泛的应用前景[1,2]。4,5鄄二氮芴鄄9鄄酮(dafo)是一种多吡啶配体,它含有羰基,易衍生出各种桥联配体,该化合物及其衍生物有特殊的结构和性能[3~5]。Dafo具有     

{Cd(dmt)_2(Hchdc)_2(H_2O)_2}_n配合物的合成与表征

通过水热合成的方法,以1,4-环己烷二羧酸、2,4-二氨基-6-甲基三嗪和CdCl_2·2.5H_2O为原料合成了一种单核的化合物{Cd(dmt)_2(Hchdc)_2(H_2O)_2}_n(dmt=2,4-diamino-6-methyl-triazine,H2chdc=1,4-cyclohexanedicarboxylic acid),并进行了IR和X射线单晶衍射(常温)的分析.结果表明,该化合物属于P2/c空间群,单斜晶系,晶胞参数:a=1.330 26(11)nm,b=0.541 47(4)nm,c=2.415 54(16)nm,β=115.751(3)°,V=1.567 1(2)nm~3,Z=2,Dc=1.570g/cm~3,F(000)=764,R1=0.035 2,wR2=0.092 7.该化合物中,中心金属离子Cd(II)与氧相连形成六配位构型,并通过4种不同的氢键作用最终形成了三维的堆积结构.     

铜-有机多酸配合物[CuI(2,2'-bipy)_2]{[CuII(2,2'-bipy)_2]_2(BW_(12)O_(40))}·4H_2O的原位合成、晶体结构与表征

在水热条件下,K5BW12O4·nH2O,CuSO4·5H2O,2,2'-联吡啶-3,3'-二羧酸在水溶液中进行原位反应,得到一维链状化合物[CuI(2,2'-bipy)2]{[CuII(2,2'-bipy)2]2(BW12O40)}·4H2O,并对其进行了元素分析,IR,TG,CV和单晶X射线衍射表征.结果表明,化合物属于单斜晶系,P21/n空间群,晶胞参数a=1.88365(14)nm,b=2.04178(15)nm,c=2.16724(16)nm,α=90°,β=96.6720(10)°,γ=90°,V=8.2786(11)nm3,Z=4,Dc=3.255g/cm3,R1=0.0575,wR2=0.1073.化合物分子结构单元由1个铜-有机多酸阴离子{[CuII(2,2'-bipy)2]2(BW12O40)}-,1个配位阳离子[CuI(2,2'-bipy)2]+,4个结晶水分子构成.化合物分子通过氢键和π-π堆积作用形成二维超分子体系.电化学研究表明,化合物存在三步氧化还原过程.     

Synthesis and Crystal Structure of Two-dimensional Network Supramolecular Complex [Cu(dafo)_2(H_2O)_2](ClO_4)_2

ＩｎｔｒｏｄｕｃｔｉｏｎＴｈｅｓｕｐｒａｍｏｌｅｃｕｌａｒｃｏｍｐｌｅｘｅｆｏｒｍｅｄｂｙｔｈｅｗｅａｋｉｎｔｅｒａｃｔｉｏｎｓ (ｅｌｅｃｔｒｏｓｔａｔｉｃｉｎｔｅｒａｃｔｉｏｎ ,ｈｙｄｒｏｇｅｎｂｏｎｄｓ ,ｖａｎｄｅｒＷａａｌｓｆｏｒｃｅ ,ｓｈｏｒｔ ｒａｎｇｅｅｘｃｌｕｓｉｏｎｆｏｒｃｅ ,ｅｔｃ .)ｏｆｍｏｒｅｔｈａｎｔｗｏｓｏｒｔｓｏｆｓｐｅｃｉｅｓｉｓａｎｏｒｇａｎｉｚｉｎｇｅｎｔｉｔｙｔｈａｔｕｓｕａｌｌｙｐｏｓｓｅｓｓｅｓｓｐｅｃｉａｌｓｔｒｕｃｔｕｒｅａｎｄｆｕｎｃｔｉｏｎ .1Ｓｕｐ…     

Synthesis and Structure of [Cu2（μ—NO2）（aepy）4]（ClO4）3 （aepy=2—（2—Aminoethyl）pyridine）

1 INTRODUCTION There has been great and considerable interest in the study of copper nitrite complexes because they are relevant to the study of copper-containing enzymes involved in the denitrification process[1]; in particular, copper-nitrite complexes are potentially relevant to the nitrite reductases[2] (the enzyme from Achromobacter Cycloclastes) which convert NO2－ to NO and/or N2O. Many attempts have been made to synthesize a variety of copper-nitrite complexes, in which the n…     

Synthesis and Crystal Structure of a [Cu(HTren)Cl_2]ClO_4·H_2O Complex (Tren = Tris(2-aminoethyl)amine)

1INTRODUCTION Investigation of the coordination chemistry of copper(II)continues to be stimulated by interest in developing modes for copper proteins and in under-standing the factors which give rise to the seemingly infinite variety of distortions from regular stereo-chemistry observed in Cu(II)complexes[1,2].For more than decades,due to the unique coordination polyhedra and their easy preparation,tripodal copper complexes have attracted much attention in addition to their special chemi…     

Novel copper(II)-dien-imidazole/imidazolate-bridged copper(II) complexes. Crystal structure of [Cu(dien)(Him)](ClO4)2 and of [(dien)Cu(mu-im)Cu(dien)](ClO4)3, a homobinuclear model for the copper(II) site of the CuZn-superoxide dismutase

The imidazolate-bridged binuclear copper(II)-copper(II) complex [(dien)Cu(mu-im)Cu(dien)](ClO(4))(3) and related mononuclear complexes [Cu(dien)(H(2)O)](ClO(4))(2), [Cu(dien)(Him)](ClO(4))(2) were synthesized with diethylenetriamine (dien) as capping ligand. The crystal structure of mononuclear [Cu(dien)(Him)](ClO(4))(2) and binuclear complex [(dien)Cu(mu-im)Cu(dien)](ClO(4))(3) have been determined by single crystal X-ray diffraction methods. The mononuclear complex [Cu(dien)(Him)](ClO(4))(2) crystallizes in the orthorhombic, Pca2(1) with a = 9.3420(9) A, b = 12.3750(9) A, c = 14.0830(9) A, beta = 90.000(7)(o) and Z = 4 and binuclear complex [(dien)Cu(mu-im)Cu(dien)](ClO(4))(3) crystallizes in the monoclinic space group P2(1)/a, with a = 15.017(7) A, b = 11.938(6) A, c = 15.386(6) A, beta = 110.30(4)(o) and Z = 4. The molecular structures show that copper(II) ions in an asymmetrically elongated octahedral coordination (type 4 + 1 + 1) and in binuclear complex Cu(1) atom has a asymmetrically elongated octahedral coordination (type type 4 + 1 + 1) and Cu(2) atom exhibits a square base pyramidal coordination (type 4 + 1). The bridging ligand (imidazolate ion, im) lies nearly on a straight line between two Cu(2+), which are separated by 5.812 A, slightly shorter than the value in copper-copper superoxide dismutase (Cu(2)-Cu(2)SOD). Magnetic measurements and electron spin resonance (ESR) spectroscopy of the binuclear complex have shown an antiferromagnetic exchange interaction. From pH-dependent cyclic voltametry (CV) and electronic spectroscopic studies the complex has been found to be stable over a wide pH range (7.75-12.50).     

Synthesis and Structure of [Er4（μ3—OH）4（Hpro）4（Pro）2（H2O）7]（ClO4）6.7H2O

1 INTRODUCTION The design and synthesis of polynuclear com- plexes have attracted chemists?attention in the contemporary chemistry, since their clusters maybe lead to novel materials with magnetic, optical, electronic and catalytic properties of the constituent metals[1～3]. It is also prevalently interesting to synthesize high-nuclearity metal complexes for their nanoscopic dimensions[3, 4]. Spectroscopic properties of the lanthanides are widely used in the study of biological systems. …     

Heterotetranuclear Cu_2~IPd_2~Ⅱ Complex with Bis(diphenylphosphino)methane and Diethyldithiocarbamate

1 INTRODUCTION The design of heterometallic complexes of photoluminescnece is of current interest for the inorganic chemists[1, 2]. The coordination flexibility of -dppm ligand as well as the easy substitution of weakly coordinated solvate donors by stronger donors makes the binuclear compound [M2(m- dppm)2(sol)2]2+ excellent building block for con- structing various molecular materials with desired properties[3～5]. We are devoted to developing heterometallic photoluminescent transitio…     

Synthesis and Crystal Structure of a Dicopper(Ⅰ) Complex with Bis(diphenylphosphino)methane and Diethyldithiocarbamate

1 INTRODUCTION Dithiocarbamate derivatives and their metal complexes are extremely versatile compounds which have been used, for example, in the treatment of alcoholism, sarcoma cell and as possible pro- tection against the lethal effect of X-rays etc[1]. Owing to the striking structure features and diversified applications of the metal complexes with dithiocarbamate[2～6], it is of theoretical and practical significance to study the coordination chemistry much more adequately. The meta…     

Synthesis and Crystal Structure of a 2-D Hydrogen-bonded Supramolecular Network {[Cu_4(OH)_4(2,2'-bpy)_4(bqdc)]·2ClO_4}_n

The title compound {[Cu4(OH)4(2,2'-bpy)4(bqdc)]·2ClO4}n 1 (bqdc = 2,2'-biquino- line-4,4'-dicarboxylic acid) has been synthesized by hydrothermal method. Its crystal structure is of triclinic, space group P1 with a = 7.6561(5), b = 12.4652(8), c = 15.7501(10) , α = 80.0480(10), β = 87.7900(10), γ = 74.0800(1)o, V = 1423.65(16) 3, Z = 2, C30H23ClN5O8Cu2, Mr = 744.06, Dc = 1.736 g/cm3, μ = 1.651 mm─1, F(000) = 754, the final R = 0.0421 and wR = 0.1163 for 4973 observed reflections with I > 2σ(I). In 1, tetra-copper chair-like clusters of [Cu4(OH)4(2,2'-bpy)4]4+ are connected by bqdc ligands to form one-dimensional chains, which are further connected by hydrogen bonds to generate a two-dimensional supramolecular network .     

Synthesis and Crystal Structure of a 2-D Hydrogen-bonded Supramolecular Network {[Cu4(OH)4(2,2''-bpy)4(bqdc)]·2ClO4}n

The title compound {[Cu4(OH)4(2,2'-bpy)4(bqdc)]·2ClO4}n 1 (bqdc = 2,2'-biquinoline-4,4'-dicarboxylic acid) has been synthesized by hydrothermal method. Its crystal structure is of triclinic, space group P-1 with a = 7.6561(5), b = 12.4652(8), c = 15.7501(10) (A), α= 80.0480(10), β= 87.7900(10), γ = 74.0800(1)°, V = 1423.65(16) (A)3, Z = 2, C30H23ClN5O8Cu2, Mr = 744.06, Dc = 1.736 g/cm3, μ = 1.651 mm-1, F(000) = 754, the final R = 0.0421 and wR = 0.1163 for 4973 observed reflections with Ⅰ＞ 2σ(Ⅰ). In 1, tetra-copper chair-like clusters of [Cu4(OH)4(2,2'-bpy)4]4 are connected by bqdc ligands to form one-dimensional chains, which are further connected by hydrogen bonds to generate a two-dimensional supramolecular network .