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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。
The complex of azido (CHZ) ligand and azido ion was synthesized and characterized by elemental analysis and IR. The crystal structure was determined by X-ray single crystal analysis. The crystal belongs to the triclinic system with P 墿 space group. The crystallographic data are: a = 8.2217 (17), b = 8.7427 (18), c = 9.4532 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, [I> 2σ (I)] = 0.0826, S = 1.132. The center Mn (Ⅱ) ions coordinate with two hydrazide molecules and two azide ions to form a hexacoordinated octahedron structure, in which the carbonyl hydrazide molecules pass through the oxygen atom on the carbonyl group and the nitrogen atom on the end group in the form of a bidentate Chelating ligand mode coordination, azide ions through the terminal nitrogen atoms to monodentate ligand coordination. The thermal decomposition of the title complex was studied by DSC and TG-DTG techniques. The results showed that the final residue decomposed at 500 ℃ was MnO.