摘要
在水热条件下,利用三缺位Keggin多钨氧酸盐前驱体Na8[-αHAsVW9O34].11H2O与NiCl2.6H2O、乙二胺反应,合成了一种包含二核镍簇和四核镍簇的有机-无机复合的新型砷钨酸盐(enH2)3[Ni2(H2O)10][Ni4(H2O)2(-αAsVW9O34)2].en.8H2O,并经IR光谱、元素分析、热重分析和X射线单晶衍射等测试手段进行了表征.标题化合物属于三斜晶系,P-1空间群,晶胞参数:α=1.204 23(19),b=1.258 5(2),c=1.593 8(4)nm,α=97.472(3),β=108.229(3),γ=114.779(2)°,V=1.985 2(7)nm3,Z=1,Dc=4.589 g/cm3,GOOF=1.023,R1=0.044 3,wR2=0.113 8.X-射线单晶结构分析表明,标题化合物分子由3个质子化乙二胺阳离子[enH2]2+、1个二核镍簇阳离子[Ni2(H2O)10]4+、1个四核镍簇取代的夹心型多阴离子[Ni4(H2O)2(α-AsVW9O34)2]10-、1个游离的乙二胺分子和8个结晶水分子组成.
An organic-inorganic composite novel arsenotungstate containing di-/tetra-nuclear nickel clusters(enH2 )3 [Ni2 (H2O)10] [Ni4 (H2O)2 (α As^VW9O34 )2]·en·8H2O is synthesized by reaction of trivaeant Keggin polyoxotungstate precursor Na8 [α HAs^VW9O34]·11H2O与NiCl2·6H2O and ethylenediamine (en) under hydrothermal conditions and characterized by IR spectrum, elemental analysis, thermogravimetric analysis and X-ray single crystal diffraction. The title compound crystallizes in the trielinic space group P-1 with α= 1. 204 23(19), b= 1.258 5(2),c=1.593 8(4) nm,α=97.472(3),β=108.229(3),γ=114.779(2)^*,V=1.985 2(7) nm^3 , Z= 1, Dc= 4. 589 g/cm^3,GOOF= 1. 023,R1 =0.044 3, wR2 =0. 1138. X-ray single-crystal structural analysis indicates that the title compound consists of 3 diprotonated [enH2]^2+ cations, 1 di-nickel cluster cation [Ni2 (H2O)10]^4+,1 tetra- nickel substituted sandwich-type polyoxoanion [Ni4 (H2O)2 (α -As^VW9O34 )2]^10- , 1 free en molecule and 8 crystal
出处
《河南大学学报(自然科学版)》
CAS
北大核心
2009年第6期602-606,共5页
Journal of Henan University:Natural Science
基金
河南省基础与前沿技术研究计划项目(092300410119)
河南大学自然科学基金(2008YBZR010)
关键词
多金属氧酸盐
砷钨酸盐
水热合成
簇合物
polyoxometalate
arsenotungstate
hydrothermal synthesis
cluster