[Mn(SCZ)_3](PA)_2·H_2O的晶体结构及热分解机理  

Crystal Structure and Thermal Decomposition Mechanism of [Mn(SCZ)_3](PA)_2·H_2O

作　　者：马桂霞[1] 张同来[1] 邵兵[1] 张建国[1] 宋江闯[1] 李玉锋[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4期445-451,共7页结构化学（英文）

摘　　要：制备得到了新配合物[Mn(SCZ)3](PA)2H2O,用元素分析和FT-IR对其结构进行了表征。用X-射线单晶衍射对其结构进行了测定,采用MoKa射线、l=0.071073nm,收集到5054个独立衍射点,其中的3812个可观测衍射点用于结构计算和修正。晶体属三斜晶系,P空间群,化学式C15H21N15O18Mn,Mr=754.41。晶体学参数a=0.7991(2),b=1.2968(3),c=1.4791(2)nm,a=72.78(1),b=84.36(1),g=81.80(2),V=1.4466(5)nm3,Z=2,Dc=1.732g/cm3,F(000)=770,S=1.07,m(MoKa)=0.565mm-1。最终偏离因子R=0.0634,wR=0.1292。中心Mn2+为六配位畸变八面体构型,它同时与3个SCZ分子配位,形成3个稳定的平面畸变五员环。苦味酸根阴离子通过静电引力和氢键与配位阳离子结合。分子间通过大量氢键在整个空间构成无限延伸的三维网状结构。[Mn(SCZ)3](PA)2H2O的热分解有2次剧烈的放热质量损失过程,热分解最终产物为MnO。A new coordination compound [Mn(SCZ)3](PA)2H2O has been obtained, and its molecular structure was characterized by using X-ray single-crystal diffraction, elemental analysis and FT-IR technique. The crystal belongs to triclinic, space group P with a = 0.7991(2), b = 1.2968(3), c = 1.4791(2) nm, a = 72.78(1), b = 84.36(1), g =81.80(2), C15H21N15O18Mn, V =1.4465(5) nm3, Z = 2, Dc = 1.732 g/cm3, Mr = 754.41, F(000) = 770, S = 1.037 and m(MoKa) = 0.565 mm-1. The final R and wR are 0.0634 and 0.1292, respectively for 3812 observed reflections with I>2s(I). The Mn2+ is six-coordinated, and SCZ acts as the bidentate ligand. Mn2+ coordinates to the oxygen and nitrogen atoms of three SCZ molecules to form three stable five-membered rings. The PA anions and coordination cations are bonded together by electrostatic attraction and hydrogen bonds, and the complicated three-dimensional net structure is constructed, which strongly enhances the stability of the coordination compound. The thermal decomposition processes of [Mn(SCZ)3](PA)2H2O contain two intensive exothermic stages, and the exothermic temperature is higher than 200 ℃. The final decomposed residue is MnO.

关 键 词：[Mn(SCZ)3](PA)2·H2O 晶体结构 热分解机理 锰配合物 三维网状结构 苦味酸 氨基脲 

分 类 号：O627[理学—有机化学]