Mn(CHZ)_2(N_3)_2配合物的合成、晶体结构与热分解研究(英文)

Preparation Crystal Structure and Thermal Decomposition Mechanism of Mn(CHZ)_2(N_3)_2

合成了以碳酰肼(CHZ)为配体,以叠氮离子为混合配体的配合物:Mn(CHZ)2(N3)2,并对其进行了元素分析及红外表征。利用X射线单晶分析测定了其晶体结构,晶体属于三斜晶系,P墿空间群,晶体学数据为:a=8.2217(17),b=8.7427(18),c=9.4532(19),α=86.376(4)°,β=69.104(3)°,γ=74.019(3)°,V=609.8(2)3,Dc=1.738g.cm-3,Z=2,R1=0.0316,wR2[I>2σ(I)]=0.0826,S=1.132。中心Mn(Ⅱ)离子与两个碳酰肼分子和两个叠氮离子配位形成六配位八面体结构,其中碳酰肼分子通过羰基上的氧原子和端基上的氮原子以二齿螯合配体方式配位,叠氮离子通过端基氮原子以单齿配体方式配位。用DSC、TG-DTG技术研究了标题配合物的热分解,研究结果表明,在500℃,分解的最终残渣为MnO。

A mixed ligand complex of manganese（Ⅱ） earbohydrazide azide, Mn（CHZ）2 （ N3 ）2 （ CHZ = earbohydrazide）, was synthesized and eharaeterized by using elemental analysis and Fourier transform infrared （FT-IR） spectrum. Its crystal structure was determined by single crystal X-ray diffraction analysis. The crystal belongs to trielinie, Pi space group, a = 8.2217（17）A, b =8.7427（18） A, c = 9. 4532（19）A, a = 86. 376（4）°, β = 69. 104（3）°, -y =74. 019（3）°,V=609.8（2）A^3, D_c=1.738 g·cm^-3, Z=2, R1 =0.0316, wR_2[I〉2σ（1）] =0.0826 andS=1.132. The central Mn（Ⅱ） ion is six-coordinated with two earbohydrazide molecules and two monodentate azido ligands, and earbohydrazide serves as bidentate ligands through the earbonyl oxygen atom and one of the terminal nitrogen atoms. The thermal decomposition mechanism of the complex was studied by using differential scanning calorimetry （ DSC ）, thermogravimetry-derivative thermogravimetry （TG-DTG） and FT-IR techniques. Results show that the final residue of thermal decomposition at 500℃ is MnO.