含有两个簇阴离子[As_8V_(14)O_(42)(SO_4)]^(6-)的金属-氧簇合物(H_2en)_6[As_8V_(14)O_(42)(SO_4)]_28H_2O的水热合成与晶体结构  

Hydrothermal Synthesis and Crystal Structure of (H_2en)_6[As_8V_(14)O_(42)(SO_4)]_28H_2O Containing Two [As_8V_(14)O_(42)(SO_4)]^(6-)Cluster Anions

作　　者：丁红[1,2] 曾庆新[1] 杨国昱[1] 徐吉庆[3] 

机构地区：[1]中国科学院福建物质结构研究所结构化学国家重点实验室 [2]吉林大学无机合成与制备化学国家重点实验室,长春130023 [3]吉林大学无机合成与制备化学国家重点实验室

出　　处：《Chinese Journal of Structural Chemistry》2003年第5期620-626,共7页结构化学（英文）

基　　金：然科学基金(批准号:20171045;20271050);高等学校博士学科点专项科研基金;福建福建省自然科学基金(批准号:E0210029); 国家财政部和中科院"引进国外杰出人才"专项基金资助

摘　　要：合成了一种新的砷-钒-氧簇合物(H2en)6[As8V14O42(SO4)]28H2O(en为乙二胺),用元素分析、IR和TG-DTA等手段进行了表征,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,P21/c空间群,晶胞参数a = 20.9235(4),b = 11.9382(2),c = 43.5783(6) 牛琤 = 102.13,V = 10642.1(3) ?,Z = 4,Mr = 4678.01,Dc = 2.920 g/cm3,F(000) = 8944,m = 7.437 mm-1,R = 0.0735,wR = 0.1361。结构测定表明,结构中2个簇阴离子{[As8V14O42(SO4)]6-}与有机铵阳离子[H2en]2+之间靠静电作用相结合,同时与H2O通过氢键构成无限的三维骨架结构。The title compound (H2en)6[As8V14O42(SO4)]28H2O was synthesized by hydrothermal method and its structure was determined by single-crystal X-ray diffraction. It crystallizes in the monoclinic system, space group P21/c with a = 20.9235(4), b = 11.9382(2), c = 43.5783(6) ? b = 102.13, V = 10642.1(3) ?, Z = 4, Mr = 4678.01 g/mol, Dc = 2.920 g/cm3, F(000) = 8944, m = 7.437 mm-1, R = 0.0735, wR = 0.1361, S = 1.125, (/s)max = 0.001, (r)max = 1.812 and (r)min = 1.537 e/3. The compound is constructed from two [As8V14O42(SO4)]6- cluster anions, eight water molecules and six deprotonated ethylenediamine cations, which are connected by hydrogen bonds, forming a three-dimensional framework.

关 键 词：水热合成 金属一氧簇化合物 晶体结构 砷 钒 多金属氧酸盐 结构分析 

分 类 号：O614[理学—无机化学]