由四核Fe(Ⅱ)金属簇和三缺位Keggin型磷钨酸盐构筑的夹心型多金属氧酸盐(英文)  

Sandwich-type polyoxomolybdate constructed from tetra-nuclear Fe(Ⅱ) cluster and trivacant Keggin tungstophosphate fragment

作　　者：李杰[1] 田淑芳[1] 

机构地区：[1]河南大学基础实验教学中心,河南开封475004

出　　处：《化学研究》2013年第5期459-462,465,共5页Chemical Research

基　　金：河南省教育厅科学技术研究重点项目(12A150004)

摘　　要：利用水热法合成了由四核FeⅡ簇和三缺位Keggin型磷钨酸盐共同构筑而成的夹心型多金属氧酸盐(H2dien)4H2[Fe4(H2O)2(α-B-PW9O34)2]·8H2O(1)(dien=二乙烯三胺);采用红外光谱、X-射线单晶衍射定性表征了产物的结构,利用元素分析测定了其组成.结果表明,化合物1属于三斜晶系,P-1空间群.其多阴离子[Fe4(H2O)2(α-B-PW9O34)2]10-由两个[α-B-PW9O34]9-单元通过Fe4O14(H2O)2簇连接而成;Fe2+离子采用六配位的八面体几何构型.同时,质子化的H2dien2+充当抗衡阳离子,经氢键与杂多阴离子[Fe4(H2O)2(α-BPW9O34)2]10-相互作用形成三维结构.A new inorganic-organic hybrid tungstophosphate built from trivacant Keggin frag- ments and in-situ generated tetra-FeⅡ clusters （ H2 dien）4 H2 [Fe4 （H2 0）2 （a-B-PW90a4 ）2 ] · 8 H2 O（1） （dien = diethylenetriamine） was synthesized by a hydrothermal route. As-synthesized product was characterized by infrared spectrometry and single-crystal X-ray diffraction, while its composition were determined by elemental analysis. Results indicate that compound 1 crys- tallizes in the triclinic space group P-1. The polyoxoanion [-Fe4 （H2 0）2 （a-B-PW9 O34）2]1^- con- sists of two [a-B-PW9O34]9- subunits linked by a rhomb-like Fe4 O14 （H2O）2 cluster. Besides, the six-coordinated FeI cations adopt octahedral coordination geometry, while separately pro- tonated H2 dien2＋ units act as counter-ions to interact with [-Fe4 （H2 O）2 （α-B-PW9 O34）2 ]10- heteropolyanions via hydrogen bonds thereby resulting in a three-dimensional framework.

关 键 词：磷钨酸盐 多金属氧酸盐 水热合成 晶体结构 

分 类 号：O614.3[理学—无机化学]