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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)]。
Using anhydrous Na2CO3 as catalyst and benzene as solvent, p-chlorobenzaldehyde-ethylenediamine Schiff base (1) was obtained by refluxing chlorobenzaldehyde with ethylenediamine. Then 1 and Cu (ClO4) 2.6H2O refluxed in ethanol solvent, the reaction was cooled to room temperature to precipitate a purple solid compound 2.2 dissolved in acetone, the solvent was slowly evaporated at room temperature to precipitate the title compound 3. The stereochemistry of 3 was confirmed by elemental analysis, IR and X-ray diffraction. 3 crystals are monoclinic, P2 (1) space group, molecular formula C16H38Cl2CuN4O11, Mr = 596.94. Cell parameters: 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. Final deviation factor R1 = 0.0566, wR2 = 0.1446 [I> 2σ (I)].