叠氮桥联四氮杂十四环席夫碱双核铜(Ⅱ)配合物[Cu_2^(2+)(C_(32)H_(64)N_8N_3^-)]_2(ClO_4^-)_6·H_2O的合成与表征  

Synthesis and Crystal Structure of Tetraaza Macrocyclic Schiff Base Binuclear Copper (Ⅱ) Complex Bridged by Azide Group [Cu_2^(2+)(C_(32)H_(64)N_8N_3^-)]_2(ClO_4^-)_6·H_2O

作　　者：康海霞[1] 王建革[1] 鲁严瑞[1] 李森兰[1] 王利亚[1] 

机构地区：[1]洛阳师范学院化学化工学院,河南洛阳471022

出　　处：《化学通报》2010年第10期910-914,共5页Chemistry

基　　金：国家自然科学基金项目(20771054)资助

摘　　要：用丙酮和乙二胺在高氯酸催化下合成了四氮杂十四元环席夫碱(1),并用1与碱式碳酸铜和叠氮化钠反应,生成铜的双核大环配合物。通过X-射线单晶衍射和红外光谱对其进行了结构表征。该配合物属单斜晶系,P2(1)空间群,晶胞参数为a=0.93214(8)nm,b=2.03665(17)nm,c=2.6540(2)nm;β=99.6590(10)°;V=4.9670(7)nm3,Z=2,Dc=1.387mg/m3,Mr=2074.76,F(000)=2172,最终R=0.0557,wR=0.1241。该配合物包括2个不对称的双核结构、6个高氯酸根和1个水分子。每一个双核结构中的铜原子都是五配位,它们分别和大环配体上的4个氮原子及叠氮根两端的氮原子配位形成畸变的四方锥构型。A tetraaza macrocyclic Schiff base was synthesized through the reaction of acetone and ethylenediamine under catalysis of perchloric acid. Then the Schiff base was reacted with Cu2 （OH）2 CO3 and NaN3 to form binuclear copper （ Ⅱ ） macrocyclic complex. The characterization of IR and X-Ray single crystal diffraction showed that the prepared complex belongs to monoclinic system with space group P2（1）,a = 0. 93214（8） nm,b = 2. 03665（17）nm,c = 2. 6540（2） nm; β = 99. 6590（10）°; V = 4. 9670（7） nm3 ,Z = 2,Dc = 1. 387Mg /m3 ,Mr = 2074. 76,F （ 000 ） = 2172,final R = 0. 0557,wR = 0. 1241. The complex consists of two asymmetry binuclear structures,six ClO 4- and one water molecule. The copper atom in each binuclear structure is five-coordinated by five nitrogen atoms （four nitrogen atoms come from the Schiff base and one nitrogen atom comes from the azido anion）. As result,a slightly distorted square pyramid geometry is formed.

关 键 词：四氮杂十四环 叠氮桥联 双核铜配合物 晶体结构 

分 类 号：O627.12[理学—有机化学]