[Co(enMe)_3]_2[As_8V_(14)O_(42)(H_2O)]·10H_2O的水热合成、性质和晶体结构

合成了一种新的砷-钒-氧簇合物Co(enMe)3]2As8V14O42(H2O)]10H2O(enMe为1,2-丙二胺),用元素分析、IR和TGA-DTA等进行了表征,并用X射线衍射法测定了晶体结构。结果表明,该晶体属单斜晶系,C2/c空间群,晶胞参数a=28.990(7),b=15.540(6),c=22.77(1),b=131.24(4),Mr=2744.68,V=7714(7)3,Z=4,F(000)=5232,m(MoKa)=7.239mm-1,Dc=2.363g/cm3,R=0.069,Rw=0.073。结构测定表明,结构中簇阴离子As8V14O42(H2O)]4-与配位阳离子Co(enMe)3]2+之间靠静电作用相结合,同时通过氢键构成无限的三维骨架结构。

Hydrothermal Synthesis, Properties and Crystal Structure of [Co(enMe)3]2[As8V14O42(H2O)]·10H2O

The title compound Co(enMe)3]2As8V14O42(H2O)]10H2O was hydrothermally synthesized and its structure was determined by single-crystal X-ray analysis. It crystallizes in monoclinic, space group C2/c with a = 28.990(7), b = 15.540(6), c = 22.77(1) ? b = 131.24(4), T = 293(2) K, Mr = 2744.68, m(MoKa) = 7.239 mm-1, V = 7714(7) 3, Z = 4, Dc = 2.363 g/cm3, R = 0.069, Rw = 0.073, (?s)max = 0.008, S = 1.54, (r)max = 1.09 and (r)min = 1.13 e/?. This compound contains ten H2O molecules and one As8V14O42(H2O)]4- anion which has fourteen distorted VO5 square pyramids and eight AsO3 triangular pyramids with a H2O molecule at its center, and two distorted octahedrally coordinated Co(Ⅱ) complex cations. The anion and coordinated Co(Ⅱ) ions are connected by hydrogen bonds, forming a 3-dimensional framework.