基于联邻二氮杂茂衍生物/Cu(Ⅰ)修饰的杂多酸盐的合成与性质研究

Synthesis and property of polyoxometalate decorated by bipyrazole derivatives and Cu(Ⅰ)

在水热条件下,采用3,3′,5,5′-四甲基-4,4′-联邻二氮杂茂(H2X)作为有机配体,合成了一种新的多酸基有机-无机杂化化合物[Cu_4(H_2X)_4(SiW12O40)].采用X射线单晶衍射、元素分析、热重分析、红外光谱及X射线粉末衍射等手段对该化合物的结构进行了表征.结果表明:该化合物属于单斜晶系,C2/c空间群;晶胞参数a=2.620 9(5)nm,b=1.528 0(5)nm,c=2.050 2(5)nm,β=112.652(5)°,V=7.577(3)nm^3,Z=4,R1=0.077 8,wR_2=0.152 2.并且发现多酸连接相邻的Cu—H_2X聚合物链形成2D双层结构.

A new organic-inorganic hybrid compound [Cu4 （H2X）4 （SiW12O40 ）] has been synthesized under the hydrothermal conditions by using the 3, 3r, 5,5P-tetramethyl-4, 4′-bipyrazole （H2X） as organic ligand. The compound has been structurally characterized by single crystal X-ray analysis, element analysis, thermogravimetric analysis,IR spectra and X-ray powder diffraction. It crystallizes in the monoclinic system,space group C2/c,a=2. 620 9（5） nm,b=1. 528 0（5） nm,c=2. 050 2（5） nm, β=112.652（5）°,V=7.577（3） nm^3,Z=4,R1= 0.077 8,wR2=0.152 2. Interestingly,{Cu-H2X} chains are joined together by polyoxometalates to generate a 2D double layer.