新型席夫碱-Cu(Ⅱ)络合物([CuC_(16)H_(34)N_4O]^(2+)·2ClO_4^-·2H_2O)的合成及晶体结构  

Synthesis and crystal structure of Cu(Ⅱ) complex with a new Schiff base ligand([CuC_(16)H_(34)N_4O]^(2+)·2ClO_4^-·2H_2O)

作　　者：郁兆莲[1] 胡少强[1] 徐艳丽[1] 李森兰[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：《化学研究与应用》2009年第9期1269-1273,共5页Chemical Research and Application

摘　　要：以无水Na2CO3为催化剂、苯为溶剂,对氯苯甲醛与乙二胺经回流分水反应得到对氯苯甲醛-乙二胺席夫碱(1)。再将1与Cu(ClO4)2.6H2O在乙醇溶剂中回流反应,反应液冷至室温析出紫色固体化合物2。2溶于丙酮中,室温放置缓慢蒸发溶剂析出标题化合物3。经元素分析、红外光谱(IR)和X-衍射单晶衍射测定,确定了3的立体化学结构。3的晶体属单斜晶系,P2(1)空间群,分子式为C16H38Cl2CuN4O11,Mr=596.94。晶胞参数:a=8.1429(11),b=15.504(2),c=10.6180(14),β=93.522(2)°,V=1337.9(3)3,Z=2,Dc=1.482 Mg/m3。最终偏差因子R1=0.0566,wR2=0.1446[I>2σ(I)]。In benzene solvent, 4-chlorobenzaldehyde-ethylenediamine Schiff base （1） was synthesized by the reaction of 4- ehlorobenzaldehyde and ethylenediamine catalyzed by anhydrous Na2 CO3 under refluxing in a Dean-Stark apparatus for water separation. Subsequently compound 1 reacted with Cu （ClO4）2·6H2O in ethanol solvent under refluxing, to form a purple solid 2 after cooling to room temperature, compound 2 was dissolved in acetone the solvent was slowly evaporated under room temperature and then the title compound 3 was obtained. The stereochemistry structure of compound 3 was determined by elemental analysis,IR spectra and single-crystal X-ray diffraction. The crystal of compound 3 was attributed to monoclinic system and P2 （ 1 ） space group. Molecular formula：C16H38Cl2CuN4O11 ,Mr =596.94. The crystal lattice parameters are a =8. 1429（ 11 ） A,b = 15. 504（2）A,c = 10. 6180（14） A,β = 93.522（2）°, V= 1337.9（3） A^3 ,Z =2,Dc = 1. 482 Mg/m^3. The final deflection factors Rt = 0. 0566, wR2 = 0. 1446[I 〉2σ（1） ].

关 键 词：对氯苯甲醛 乙二胺 席夫碱 晶体结构 铜络合物 

分 类 号：O614.121[理学—无机化学]