一种新颖的有机-无机杂化多金属氧酸盐配合物的合成与晶体结构

Synthesis and Crystal Structure of a Novel Organic-Inorganic Hybrid Polyoxometalate Complex

利用水热法合成了一种新的多金属氧酸盐[Fe(phen)3]2(PMo10V3ⅤVⅣO44).DMF,采用红外光谱、单晶X-射线衍射、差热-热重和XPS等方法对其进行了表征.结果表明:化合物是由杂多阴离子(PMo10V3ⅤVⅣO44)4-,[Fe(phen)3]4+片段和DMF分子组成;配合物通过氢键作用相互连接形成三维超分子结构;晶体属于三斜晶系,P1空间群;晶胞参数:a=1.413 41(4)nm,b=1.835 09(6)nm,c=1.967 63(7)nm,α=83.225 0(10)°,β=69.787 0(10)°,γ=87.021 0(10)°,V=4.755 4(3)nm3,Z=1,Rgt(F)=0.045 9,ωRref(F2)=0.107 9,S=1.016.

A novel polyoxometalate [Fe（phen）3]2（PMo10VⅤ3VⅣO44）·DMF has been synthesized by Hydrothermal method and characterized by single-crystal X-ray diffraction,IR,TG-DTA and XPS.The results indicate that the structure of the title compound consists of（PMo10VⅤ3VⅣO44）4-heteropolyoxoanion,[Fe（phen）3]4＋ fragments and DMF molecules.The title compound formed the 3D supramolecular structure via intermolecular hydrogen-bonding interactions.The title compound crystallized in the triclinic,space group P1 with a=1.413 41（4） nm,b=1.835 09（6） nm,c=1.967 63（7） nm,α=83.225 0（10）°,β=69.787 0（10）°,γ=87.021 0（10）°,V=4.755 4（3） nm3,Z=1,Rgt（F） =0.045 9,ωRref（F2） =0.107 9,S=1.016.