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用中温水热法合成出一种新的α-Keggin结构化合物[Co(2,2’-bpy)2H2O]12[Mo12V6O42(VO4)][Mo8V8O40(VO4)]3.8H2O,并对其进行了元素分析、IR谱、TGA及X-射线单晶衍射等系列表征。该簇合物属三斜晶系,空间群P-1,a=1.57287(2)nm,b=2.46159(3)nm,c=0.52347(3)nm,α=76.6220(3)°,β=92.078°,γ=79.9390(4)°,V=9.1934(2)nm3,Z=2,Dc=4.642 g.cm-3,μ=4.642mm-1,F(000)=12420,R1=0.0751,wR2=0.1964。化合物中基本构筑单元为三种具有α-Keggin结构的聚阴离子簇,簇与簇之间通过配位阳离子[Co(2,2’-bpy)2H2O]2+桥连成三维结构。化合物中包含少见的六帽α-Keggin结构簇单元。并且在同一晶胞中同时存在聚阳离子和聚阴离子。
A new α-Keggin structure compound [Co (2,2’-bpy) 2H2O] 12 [Mo12V6O42 (VO4)] [Mo8V8O40 (VO4)] 3.8H2O was synthesized by mesophilic hydrothermal method. Analysis, IR spectrum, TGA and X-ray single crystal diffraction series characterization. The cluster is a triclinic system with space group P-1, a = 1.57287 (2) nm, b = 2.46159 (3) nm, c = 0.52347 (3) nm, 92.078 °, γ = 79.9390 (4) °, V = 9.1934 nm 2, D = 4.642 g · cm -3, μ = 4.642 mm -1, F 000 = 12420, wR2 = 0.1964. The basic building blocks in the compounds are three polyanionic clusters with α-Keggin structure, which are bridged into a three-dimensional structure by coordinating the cation [Co (2,2’-bpy) 2H2O] 2+ between the clusters. Compounds contain rare six-cap α-Keggin structure cluster unit. And polycation and polyanion coexist in the same unit cell.