混合价配位聚合物{[Cu(en)_2]_2HPW_9^(VI)W_2~VW^(IV)O_(40)}_2^-[Cu(en)_2H_2O]_2·8H_2O的水热合成与晶体结构

Hydrothermal Synthesis and Crystal Structure of a Mixed-valence Coordination Polymer{[Cu(en)_2 ]_2HPW_9^(VI)W_2~VW^(IV)O_(40)}_2^-[Cu(en)_2H_2O]_2·8H_2O

在水热条件下合成了一个新的混合价配位聚合物{[Cu(en)2]2HPW9VIW2VWIVO40}2[Cu(en)2H2O]2·8H2O,并对其进行了元素分析,IR,UV,TG-DSC等表征.X射线单晶衍射结果表明,化合物属于单斜晶系,P21/c空间群,晶胞参数a=1.88678(12)nm,b=2.30383(14)nm,c=2.61234(16)nm,α=90°,β=95.844(1)°,γ=90°,V=11.2964(12)nm3,Z=4,Dc=3.954g/cm3,R1=0.0975,wR2=0.2041.结构测定结果表明,聚合物中杂多阴离子骨架通过氧桥相连并形成一维无限链.热性质研究表明,形成标题化合物后杂多阴离子骨架分解温度大约在600.4℃,热稳定性较母体杂多酸明显增强.

A novel mixed-valence coordination polymer {[Cu（en）2]2HPW9^VIW2^VW^IVO40}2-[Cu（en）2H2O]2·8H2O was synthesiszed under a hydrothermal condition and characterized by elemental analysis, IR, UV, TG-DSC and single-crystal X-ray diffraction. The title compound crystUized in a monoclinic crystal system, with space group P21/c, a=1.88678（12） nm, b=2.30383（14） nm, c=2.61234（16） nm, a=90°, β=95.844（1）°, γ=90°, V=11.2964（12） nm3, Z=4, Dc=3.954 g/cm3, R1=0.0975, and wR2=0.2041. The structural refinement indicates that the title compound forms a one-dimensional chain from the polyanions （ HPW9^VIW2^VW^IVO40）^6- through O bridge. The result of TG-DSC shows that the title compound is thermally more stable than a-H3PW12O40·H2O.