论文部分内容阅读
由硝酸镍水溶液和肼基甲酸甲酯 (NH2 NHCOOCH3 ,MCZ)的水溶液反应 ,制备出未见文献报道的配合物 [Ni(MCZ) 3 ] (NO3 ) 2 ·H2 O .晶体结构测定结果表明 ,该晶体属单斜晶系 ,P2 1/n空间群 ,晶体学参数为 :a =1.3 681(2 )nm ,b =0 .8188(1)nm ,c =1.60 2 9(4 )nm ,β =92 .16(2 )° ,V =1.7943 (6)nm3 ,Dc=1.744g·cm-3 ,Z =4,F(0 0 0 ) =976,μ(MoKα) =1.166mm-1.结构采用全矩阵最小二乘法优化 ,除氢原子采用各向同性热参数外 ,其它非氢原子均采用各向异性热参数修正 ,最终偏离因子R1=0 .0 3 3 7,wR2 =0 .0 85 7.在该配合物分子中 ,肼基甲酸甲酯作为双齿配体 ,由羰基氧原子和端基氮原子与Ni2 + 配位 ,形成五元平面螯合环 ,配合物分子中共有三个这样的螯合环 ,中心离子为六配位八面体构型 .配合物的外界是两个硝酸根离子和一个水分子 ,通过库仑力和氢键与内界结合在一起 .采用TG DTG ,DSC ,IR等表征了标题化合物的热稳定性 .在程序升温条件下 ,该配合物的热分解过程是由一个弱的吸热过程和三个较强的连续的放热过程组成的 ,由TG DTG和IR分析结果证明 ,在 3 2 5℃时的最终分解产物为NiO ,得到了化合物的热分解机理 .
(Ni (MCZ) 3] (NO 3) 2 · H 2 O was prepared by the reaction of aqueous nickel nitrate and aqueous solution of methyl carbazate (NH 2 NHCOOCH 3, MCZ) The crystal belongs to monoclinic space group P2 1 / n with the following crystallographic parameters: a = 1.3681 (2) nm, b = 0.81 8 (1) nm, c = 1.6029 = 92 .16 (2) °, V = 1.7943 (6) nm3, Dc = 1.744 g · cm -3, Z = 4, F (O 0 0) = 976, and Mo (MoKα) = 1.166 mm -1. All-matrix least-squares method was used to optimize, except for hydrogen atoms using isotropic thermal parameters, other non-hydrogen atoms were modified by anisotropic thermal parameters, the final deviation from the factor R1 = 0 .0 3 3 7, wR2 = 0. 0 85 7. In the complex molecules, methyl carbazate as a bidentate ligand, carbonyl oxygen atoms and terminal nitrogen atoms and Ni2 + coordination, the formation of five yuan plane chelating ring, a total of three molecules in the complex The center ion is a hexacoordinate octahedron with two nitrate ions and one water molecule, which are bound to the inner boundary through Coulomb’s force and hydrogen bond.The TG DTG, DSC, IR, etc. characterize the thermal stability of the title compound Under the temperature programmed conditions, the thermal decomposition process of the complex consisted of a weak endothermic process and three strong continuous exothermic processes. The results of TG DTG and IR analysis showed that the complex was stable at 325 ℃ When the final decomposition product is NiO, the thermal decomposition mechanism of the compound is obtained.