含氧桥的笼状化合物[Mo_5P_2O_(23)]^(6-)[(CH_3)_2NH_2]_5^(5+)-[H_3O]^+·1/2(CH_3)_2NCHo·1/2H_2O的合成和结构

Synthesis and Crystal Structure of Cage-Shaped Compound [Mo_5P_2O_(23)][(CH_3)_2NH_2]_5[H_3O]·1/2DMF·1/2H_2O Containing [Mo_5P_2O_(23)]^(6-) group

[Mo_5P_2O_(23)]^(6-)[(CH_3)_2NH_2]_5^(5+)[H_3O]^+·1/2DMF·1/2H_2O(DMF=(CH_3)_2NC-HO)(M_r=1204.67)的晶体属三斜晶系,空间群P,晶胞参数a=16.438(6);b=22.22(1);c=11.325(5),α=104.25(4);β=108.97(3);γ=97.68(4)°,V=3688(3),Z=4,D_c=2.17gcm^(-1),R=0.056,R_w=0.074,晶胞中每个不对称单元含有两个[Mo_5P_2O_(23)]^(6-)[(CH_3)_2NH_2]_5^(5+)[H_3O]^+·1/2DMF·1/2H_2O,阴离子[Mo_5P_2O_(23)]^(6-)中的Mo、P原子成一个畸变五角双锥构型。有一个阴离子的所有原子(Mo、P、O)位置完全确定,而另一个阴离子有一个磷酸根的三个氧原子位置出现二重位置统计分布。化合物的阳离子为二甲胺阳离子和水合氢离子。

Here we reporte the synthesis and structure of [Mo5P2O23][(CH3)2NH2]5[H3O]·1/2DMF ·1/2H2O,( Mr = 1204. 67) whic is the triclinic, space group P1, with a=16. 438(6), b=22. 22(1), c=11.325(5)A,α=104.25(4),β=108. 97(3), γ=97.68(4)°, V=3688(3)A3, Z = 4, Dc = 2. 17 g/cm3, R=0. 056, Rw = 0. 074. The crystal structure shown that each asymmetry unit contains two [Mo5P2O23][(CH3)2NH2]5 [H3O]·1/2DMF·1/2H2O molecules. The core [Mo5P2] structures in the two set molecules shown a distorted pentagonal bipyramidal configuration. It is interesting that in the two sets of the anion configurations, one has the sites of all atoms defined whereas the other has three of the four oxygen atoms in a PO43- group occupied statistically on twofold sites. The cations are [(CH3)2NH2]3 + and [H3O]+.