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由硝酸钴水溶液和肼基甲酸甲酯(NH2NHCOOCH3, mcz)的水溶液反应, 首次制备出了配合物[Co(mcz)3](NO3)2H2O, Mr = 471.23, 测定了其晶体结构。晶体属单斜晶系, P21/n空间群。晶体学参数为: a = 13.648(3), b = 8.234(1), c = 16.144(4) ? b=91.96(2), V=1813.1(5) ?, Z=4, Dc = 1.726 g/cm3, m(MoKa ) = 1.030 mm1, F(000)=972, R=0.0359, wR = 0.0935。在该配合物中, 肼基甲酸甲酯作为双齿配体, 由羰基氧原子和1位氮原子与钴原子配位, 形成五员平面螯合环, 配合物分子中共有3个这样的螯合环, 中心离子为六配位八面体构型。配合物的外界为2个硝酸根离子, 并含有1个结晶水分子, 通过库仑力与内界结合在一起, 相邻分子间以氢键作用连接。采用TG、DTG, DSC和IR技术研究了标题化合物热分解机理。在程序升温条件下, 该配合物有2个吸热峰和3个放热峰, 由TG-DTG分析和IR分析结果表明, 300 ℃时的最终分解产物为CoO。
The crystal structure of the complex [Co (mcz) 3] (NO3) 2H2O and Mr = 471.23 was prepared by the reaction of aqueous solution of cobalt nitrate and aqueous solution of methyl carbazate (NH2NHCOOCH3, mcz) Crystal is monoclinic, P21 / n space group. The crystallographic parameters are: a = 13.648 (3), b = 8.234 (1), c = 16.144 (4)? B = 91.96 (2), V = 1813.1 (5) cm3, m (MoKa) = 1.030 mm1, F (000) = 972, R = 0.0359, wR = 0.0935. In this complex, methyl carbazate acts as a bidentate ligand and is coordinated by a carbonyl oxygen atom and a nitrogen atom to a cobalt atom to form a five-membered planar chelating ring. There are three such chelates in the complex molecule Heterocyclic ring, the center ions for the six coordination octahedral configuration. The complex is composed of two nitrate ions and one crystal water molecule. The Coulomb force combines with the inner bound, and the adjacent molecules are connected by hydrogen bonds. The thermal decomposition mechanism of the title compound was studied by TG, DTG, DSC and IR. Under temperature programmed conditions, the complex has two endothermic peaks and three exothermic peaks. The results of TG-DTG analysis and IR analysis show that the final decomposition product at 300 ℃ is CoO.