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报道了α-Keggin型(NH4)4HPW10V2O40·2.5H2O的水热合成方法,采用X-ray单晶衍射测定了晶体结构.结构分析表明:该晶体属于三斜晶系,空间群为P1,晶胞参数:a=1.322 3(3)nm,b=1.324 3(3)nm,c=1.325 3(3)nm,α=75.98(3)°,β=75.99(3)°,γ=76.06(3)°,Z=2,R1(wR2)=0.081 2(0.198 0).杂多酸阴离子作为一个整体是有序α-Keggin结构,但由于异构体存在,钨和钒原子在晶体学上无序分布在12个配原子位置上,钒在每个配原子位置上占有率并不相等,平均值为0.167,总占有率为2.00.元素分析、热重分析、UV、IR、31p NMR光谱支持单晶X-ray衍射结果.“,”It has been reported that the title compound was synthesized by a hydrothermalmethod and structurally characterized by single crystal x - ray diffraction. The crystal datawere shown below: triclinic, space groupP1,α=1.322 3(3)nm, b = 1. 324 3(3)nm, c =1.325 3(3)nm, α=75.98(3)°,β= 75.99(3)°, γ= 76.06(3)°,Z= 2, R1(wR2) =0. 081 2(0. 1980). Although the heteropolyanion is ordered a - Keggin structure, W and Vatoms are disorderly distributed in 12 addenda atoms crystallographically. The occupationprobability of V on each addenda atom is unequal, the mean value is 0. 167 and the totalprobability on anion is 2.00. The result was supported by elemental analysis, therrogravimetric analysis, UV- Vis, IR,31P NMR spectra.