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.     

邻苯二甲酸根桥联Zn(Ⅱ)超分子配合物的合成、表征和晶体结构

用Zn(NO3 ) 2 ,phen(邻菲咯啉 )和phth(邻苯二甲酸 )混合反应得到了配位聚合物 {[Zn2 (phen) 2 (phth) 2 (H2 O) 2 ]·2H2 O}n.通过元素分析、红外光谱对配合物进行了表征 .用X射线单晶衍射仪测定了配合物的晶体结构 .配合物为单斜晶系 ,P2 ( 1) /n空间群 .晶胞参数a =0 964 3 ( 3 )nm ,b =0 8976( 3 )nm ,c =2 14 10 ( 7)nm ,β =90 776( 5 )° ,Z =4,V =1 85 3 1( 10 )nm3 ,Dc=1 5 98g/cm3 ,μ =1 3 67mm-1,F( 0 0 0 ) =912 ,R1=0 0 40 9,wR2 =0 0 818,锌原子为五配位 ,呈畸变三角双锥构型 ,通过邻苯二甲酸根的桥联作用形成了一维螺旋链状结构 ,相邻的螺旋链之间靠π π堆积形成二维网状超分子结构 .     

混合配体配合物镉(Ⅱ)-邻菲罗啉-丙二酸根异构体的结构特征研究

由硝酸镉、邻菲罗啉和丙二酸混合反应,得到无色透明单晶.经X射线单晶衍射法测定了该晶体的分子结构,在1个晶胞中存在两个混合配体配合物异构体,其组成为C₂₇H₁₈O₄N₄Cd.晶体学数据为:三斜晶系,P-1空间群.a=0.14432(5)m,b=0.15517(5)nm,c=0.16098(6)nm,α=107.048(6)°,β=98.989(6)°,γ=116.481(6)°,Z=2,F(000)=1287,D_c=1.453g/cm3,μ=0.802mm^-1,R₁=0.0645,wR₂=0.1756.该异构体的差别在于丙二酸根中2个羧基中各1个氧原子配位(1)或1个羧基中2个氧原子同时配位(2).1和2之间靠氢键和π-π堆积等弱相互作用形成超分子结构.