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将MnCO3 与2,4,6-三硝基间苯二酚(斯蒂芬酸、TNR)分散于蒸馏水中, 加热搅拌制备出斯蒂酚酸锰溶液,再与碳酰肼(CHZ)水溶液反应制备〔Mn2 (TNR)2(CHZ)2(H2O)4〕·2H2O(C14H26Mn2N14O24, Mr= 884.36),并对其进行了元素分析和红外表征,利用单晶分析测定了晶体结构。该化合物为双核配合物,属三斜晶系,空间群为P1,晶体学数据如下:a= 7.280(1),b= 10.318(1),c= 11.106(1),α= 94.56(1),β= 91.86(1),γ= 106.88(1)°,V= 794.4(2)3,Z= 1,Dc= 1.849g.cm - 3, μ=9.15cm - 1, F(000)= 450, I> 2σ(I)的独立可观测点个数为2783,最终偏离因子R=0.0272, Rw = 0.0639。分子为中心对称,配位多面体为略有畸变的五角双锥体构型。
MnCO3 and 2,4,6-trinitro-resorcinol (Stephenic acid, TNR) are dispersed in distilled water, and the solution of manganese stearate is prepared by heating and stirring, and then reacting with carbonic hydrazide (CHZ) aqueous solution to prepare [ Mn2 (TNR) 2 (CHZ) 2 (H2O) 4] · 2H2O (C14H26Mn2N14O24, Mr = 884.36) was synthesized and characterized by elemental analysis and IR. The crystal structure was determined by single crystal analysis. The compound is a dinuclear complex and belongs to the triclinic system with space group P1. The crystallographic data are as follows: a = 7.280 (1), b = 10.318 (1), c = 11.106 , Α = 94.56 (1), β = 91.86 (1), γ = 106.88 (1) °, V = 794.4 (2) 3, Z = 1 and Dc = 1.849 g. The number of independent observable points with cm = 3, μ = 9.15cm - 1, F (000) = 450, I> 2σ (I) is 2783, the final deviation factor R = 0.0272, Rw = 0.0639. Molecular symmetry center, coordination polyhedron with a slightly distorted pentagonal bipyramid configuration.