摘要
利用Sb2O3,Na2WO4合成了一个巨型的穴状化合物(NH4)16H2[NaSb9W21O86].15.5H2O.晶体衍射数据显示,该化合物属于六方晶系,P6-2c空间群,a=b=1.78025(9)nm,c=2.2510(2)nm,α=β=90(9)°,γ=120(2)°,V=6.1783(7)nm3,Z=2,Dc=3.722Mg/m3,F(000)=6086,μ=21.494mm-1,R1=0.0365,wR2=0.0871[I≥2σ(I)].晶体解析表明,该化合物多阴离子[NaSb9W21O86]18-由3个[SbW7O24]3-亚单元和2个环形的[Sb3O7]5-基团连接形成双环孔穴,一个Na+阳离子通过配位键作用嵌入该空穴内.整个穴状物阴离子呈涡轮状结构,3个[SbW7O24]3-亚单元作为3个叶片.
A gigantic cryptate polyoxometalate ( NH4 ) 16 H2 [ NaSb9 W21O86 ] · 15.5 H2 O has been synthesized and characterized by IR spectroscopy, elemental analysis and single-crystal X-ray structural analysis. X-ray single-crystal diffraction indicates that the title compound crystallizes in a hexagonal lattice, P62c space group, with a =b = 1.780 25(9) nm, c=2.251 0(2) nm, α=β= 90(9)°, T = 120(2)°, V=6.178 3(7) nm^3, Z =2, Dc =3.722 Mg/m^3 F(000) =6 086,μ =21.494 mm^-1 R1 = 0.036 5, ωR2 = 0. 087 1 [ I ≥ 2σ(I) ]. Structure analysis reveals that the polyoxoanion [ NaSb9 W21O86 ] ^18-, containing three [ SbW7O24 ] ^3- subunits linked by two cyclic [ Sb3O7 ] ^5- groups, results in a bicyclic cavity, in which a Na^+ is incorporated and coordinated to six oxygen atoms. The whole polvoxoanion can be described as a turbine with three [ SBW7O24 ]^ 3- moieties acting as three vanes.
出处
《化学研究》
CAS
2007年第2期1-5,共5页
Chemical Research
基金
Supported by the Program for New Century Excellent Talents in University of Henan Province(2005HANCET-02)
the Natural Science Foundation of Henan Province,the Program for Training Young Excellent Cadreman Teachers in University of Henan Province,the Stress Founda-tion of Henan University(05ZDZR002)
关键词
多金属氧酸盐
晶体结构
穴状物
锑钨酸盐
polyoxometalate
crystal structure
cryptate
antimoniotungstate