摘要
利用水热合成法合成了分子组成为(C6H11NH3)5H(P2Mo5O23)4H2O的杂多化合物, 用单晶X-ray衍射方法测定了它的结构,该晶体属于单斜晶系,空间群P21/c, a = 12.830(3), b = 14.848(3), c = 25.258(5) ? b = 92.95(3), Mr = 1483.62, V = 4805.1(17) 3, Z = 4, Dc = 2.051 g/cm3, m = 1.431 mm-1, F(000) = 3000, I >2s(I) 的可观察衍射点4426个, 最终结构偏差因子R = 0.0464, wR = 0.0801, S = 0.731。在[P2Mo5O23]6-杂多阴离子中5个MoO6八面体通过共边和共角相连, 形成1个近似的五角平面骨架, 2个PO4四面体加在五角平面的两侧。热性质研究表明杂多阴离子骨架在547.4 ℃左右分解。
A strandberg-type hepteropoly complex has been prepared by the hydrothermal method and characterized by single-crystal X-ray diffraction analysis. It belongs to monoclinic, space group P21/c with a = 12.830(3), b = 14.848(3), c = 25.258(5) ? b = 92.95(3), V = 4805.1(17) 3, Z = 4, Dc = 2.051 g/cm3, m = 1.431 mm-1, F(000) = 3000, S = 0.722, the final R = 0.0464 and wR = 0.0801 for 4426 observed reflections (I > 2(I))。The results show that the polyanion [P2Mo5O23]6- consists of two PO4 tetrahedra and five MoO6 octahedra which construct a Mo5 ring by sharing edges except for one pair joined by corner sharing. Each face of the Mo5 ring is capped by a tetrahedral PO4 group.
基金
河南省杰出青年基金
河南省教育厅基金资助项目(20011500024)
