有机-无机复合磷钨酸盐[HTA]_3[α-PW_(12)O_(40)]·6H_2O的合成与晶体结构(英文)  

Synthesis and crystal structure of an organic-inorganic composite phosphotungstate[HTA]_3[α-PW_(12)O_(40)]·6H_2O

作　　者：齐秀丽[1,2] 赵浩哲 张景丽[1] 陈利娟[1,2] 

机构地区：[1]河南大学化学化工学院,河南开封475004 [2]河南大学基础实验教学中心,河南开封475004

出　　处：《化学研究》2014年第1期8-12,共5页Chemical Research

基　　金：Supported by the Natural Science Foundation of China(21101055,21301049,U1304208);the Natural Science Foundation of Henan Province(122300410106);the Foundation of Education Department of Henan Province(2010B150006);the Students Innovative Pilot Plan of Henan University(2012,2013)

摘　　要：利用CuCl2·2H2O,1,2,4-三氮唑(TA),L-丝氨酸与Na3[α-PW12O40]·6H2O在乙醇的水溶液中合成了一种有机-无机复合Keggin结构磷钨酸盐[HTA]3[α-PW12O40]·6H2O;利用红外光谱和X射线单晶衍射表征了合成产物的结构,利用元素分析测定了其组成.结果表明,标题化合物属于菱方晶系R-3空间群,晶胞参数为:a=1.793 73(12)nm,b=1.793 73(12)nm,c=2.440 7(3)nm,α=β=90°,γ=120°,Z=6,V=6.800 7(11)nm3,Dc=4.682g·cm-3,GOOF=1.079,R1=0.051 6,wR2=0.137 4.就分子结构而言,标题化合物分子由一个饱和Keggin结构多阴离子[α-PW12O40]3-,三个游离的质子化[HTA]+阳离子和六个结晶水分子组成.An organic-inorganic composite Keggin-type phosphotungstate [HTA]3[α-PW12O40]·6H2O （TA = 1,2,4-triazole） was synthesized via the reaction of CuCl2 · 2 H2 O, Na3 [α-PW12O40]·6H2O, and L-serine with 1,2,4-triazole in aqueous solution of ethanol. The structure of as-synthesized product was characterized by infrared spectrometry and single-crystal X-ray diffraction, and its composition was determined by elemental analysis. It was found that the title compound crystallizes in the rhombohedral space group R-3 with a = 1.793 73（12） nm, b = 1.793 73（12） nm, c = 2.440 7（3） nm, α=β=90°,γ=120°,Z=6,V=6.8007（11）nm3,Dc=4.682g·cm-3,GOOF=1.079,R1=0.0516 and wR2-0.1374. In terms of the molecular structure, the title compound consists of one saturated Keggin phosphotungstate [α-PW12O40]-3 anion, three free monoprotonated [HTA]＋ cations and six lattice water molecules.

关 键 词：多金属氧酸盐 磷钨酸盐 KEGGIN结构 合成 晶体结构 

分 类 号：O614.3[理学—无机化学]