[Co(mcz)_3](NO_3)_2·H_2O的制备、分子结构和热分解机理  

Preparation, Molecular Structure and Thermal Decomposition Mechanisms of [Co(mcz)_3](NO_3)_2·H_2O

作　　者：宋江闯[1] 张同来[1] 张建国[1] 李玉锋[1] 马桂霞[1] 郁开北[2] 

机构地区：[1]北京理工大学爆炸灾害预防控制国家重点实验室,北京100081 [2]中科院成都分院分析测试中心,成都610041

出　　处：《Chinese Journal of Structural Chemistry》2004年第3期347-351,共5页结构化学（英文）

摘　　要：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 new synthesized compound [Co(mcz)3](NO3)2H2O has been prepared by using the aqueous of cobalt nitrate and methylcarbazate(mcz) as reagents, and its crystal structure was determined by single-crystal diffraction analysis with the following data: monoclinic, space group P21/n, a = 13.648(3), b = 8.234(1), c = 16.144(4) ? b = 91.96(2), Mr = 471.23, V = 1813.1(5) ?, Z = 4, Dc = 1.726 g/cm3, m(MoKa) = 1.030 mm1, F(000) = 972, R = 0.0359 and wR = 0.0935. Methylcabazate serves as a bidentate ligand coordinating to the cobalt cation with its carbonyl oxygen atom and the first nitrogen atom, and thus a five-membered chelating ring is formed. There exist three such rings in the molecule with the coordination number of six and configuration of octahedron. Thermal decomposition mechanisms of the compound were studied by using TG-DTG, DSC and IR techniques. They confirmed that the decomposition process includes two endothermic proceeds and three exothermic proceeds, and the final residue at 300 ℃ is CoO.

关 键 词：[Co(mcz)3](NO3)2·H2O 制备 分子结构 热分解机理 肼基甲酸甲酯 钴配合物 含能材料 

分 类 号：O627[理学—有机化学]