一例基于Keggin型多酸阴离子的双加帽杂多铌酸盐的合成、结构及表征  

Synthesis, crystal structure and characterization of a bicapped heteropolyoxoniobate based on Keggin-type polyoxoanion

作　　者：武贺臣 张泽霖 李丽 王勇[1] 马鹏涛[1] 

机构地区：[1]河南大学化学化工学院,河南开封475004 [2]河南省实验文博学校,河南郑州450002

出　　处：《化学研究》2017年第5期563-567,共5页Chemical Research

基　　金：河南省教育厅科学技术研究重点项目基金(14A150028)

摘　　要：在水热条件下,成功合成了一例基于Keggin型多酸阴离子的双加帽杂多铌酸盐[Ni(en)_3]_3[Ni(en)_2(H_2O)_2]_2H[VNb_(12)O_(40)(VO)_2]·10H_2O(1),并通过红外光谱、热重分析和X射线单晶衍射等方法对该化合物进行了表征.X射线单晶衍射分析表明,化合物1属于正交晶系,Pna2(1)空间群,晶胞参数a=3.051 7(3)nm,b=1.561 0(1)nm,c=2.271 9(3)nm,V=10.823(3)nm^3.化合物1包含1个Keggin型聚阴离子[VNb_(12)O_(40)(VO)_2]^(11-)和3个镍配离子.在阴离子结构中,中心钒原子被12个铌原子包围形成经典Keggin型结构的[VNb_(12)O_(40)]^(15-)阴离子,另外两个{VO}基团分别加帽于[VNb_(12)O_(40)]^(15-)阴离子的两端.A new Keggin heteropolyoxoniobate [Ni（en）3]3[Ni（en）2（H2O）2]2H[VNb12O40（VO）2]·10H2O （1） has been synthesized by hydrothermal method, and was characterized by IR spectrum,thermogravimetric （TG） analysis and X-rays diffraction. X-ray structural analysis indicates that compound 1 crystallizes in the orthorhombic Pna2（1） space group with the cell constants：a = 3.051 7（3）nm, b = 1.561 0（1） nm, c = 2.271 9（3） nm, V = 10.823（3） nm3. Compound 1 consists of a bi-capped Keggin polyanion [VNb12O40（VO）2]11-and three nickel-complexes as the countercations. Thepolyanion can be described as a decorated Keggin cluster with one vanadium atom as the central het-eroatom surrounded by twelve niobium atoms along with two {VO} groups capping two opposite sides.

关 键 词：杂多铌酸盐 双加帽 KEGGIN型 晶体结构 

分 类 号：O614.5[理学—无机化学]