具有二维超分子结构的{[Ni(oxbe)]_2Mg(H_2O)_2}·2DMF·DMA的合成及晶体结构  

Synthesis and Crystal Structure of {[Ni(oxbe)]_2Mg(H_2O)_2}·2DMF·DMA with 2D Superamolecular Structure

作　　者：陶偌偈[1] 李付安[1] 臧双全[1] 梅崇珍[1] 牛景扬[1] 

机构地区：[1]河南大学化学化工学院,开封475001

出　　处：《化学通报》2005年第3期233-236,共4页Chemistry

基　　金：河南省科技厅基金 (0 3110 2 0 80 0 )';河南省教委 (2 0 0 2 15 0 0 0 3)资助项目

摘　　要：合成了一种中心对称的草酰胺桥联异三核配合物 {[Ni(oxbe) ]2 Mg(H2 O) 2 }·2DMF·DMA[oxbe为N (2 羧基苯 ) N′ (2 氨乙基 )不对称草酰胺 (H3 oxbe)的脱氢阴离子 ;DMF为N ,N 二甲基甲酰胺 ;DMA为二甲胺 ]。用单晶X射线衍射法测定了它的晶体结构 ,该晶体属单斜晶系 ,空间群C2 c ,晶胞参数a=2 2 61 7(5 ) ,b =1 7 1 73 (4 ) ,c=1 0 881 (4 ) ,β =1 1 5 40 (2 )°,V =3 81 8(2 ) 3 ,Ni2 MgC3 0 H44N8O13 ,Mr=866 46,Z =4,Dc=1 5 0 8g cm3 ,μ(MoKα) =1 0 75mm-1,F(0 0 0 ) =1 80 8,R =0 0 660 ,wR =0 1 772 (I >2б(I) ) ,3 75 5个可观察衍射点。该三核分子为中心对称结构 ,镁离子位于 6个氧原子所构成的变形八面体的中心 ,两个镍离子则分别位于两端由N3 O构成的近似平面四方场中 ,中心Mg2 + 与两端的Ni2 + 通过草酰胺阴离子桥联在一起。Ni(oxbe)] 2Mg(H 2O) 2}·2DMF·DMA,the centrosymmetrical oxamido-bridge d heterotrinuclear complex, has been synthesized, where oxbe is anion of the deh ydrogen dissymmetrical ligand:N-benzoato-N-(2-aminoethyl)oxamido(H 3oxbe), DMF= N,N-Dimethylformamide, DMA= N,N-Dim ethylamine. And its c rystal structure was determined by single-crystal X-ray diffraction method. Th is compound crystallizes in the monoclinic, space group C2/c, the cell parameter s are a=22.617(5)?, b=17.173(4)?, c=10.881(4)?, β=115.40 (2)°, V=38.18(2)?3, Z=4,Ni 2MgC 30H 44N 8O 13, M r=866.902, D c=1.508Mg/m3,μ(MoKα)=1.075mm -1, F(000)=1808,R=0.0660,wR=0.1772〔I>2б(I)〕,for 3755 observ ed reflect ions, with I>2б(I). The heterotrinuclear molecular structure is centro sym metrical. Magnesium atom lies on the symmetrical center of a distorted octahedra l geometry formed by six oxygen atoms; two terminal nickel atoms are in approxim ately square planar environment consisting of N 3O. The inner Mg(Ⅱ) ion and t he outer Ni(Ⅱ) ions are bridged by two oxamido anion groups.

关 键 词：NI2 N-二甲基甲酰胺 草酰胺桥联 单晶X射线衍射 异三核配合物 晶体结构 单斜晶系 DMF 合成 二甲胺 

分 类 号：O621[理学—有机化学]