一例基于{PMo_(6)}单元的杂多钼酸盐的合成、结构及表征  

Synthesis, structure and characterization of a {PMo_(6)} subunit-based heteropolymolybdate

作　　者：李蕊 张泽霖 付明辉 张鑫 武贺臣 马鹏涛[1] LI Rui;ZHANG Zelin;FU Minghui;ZHANG Xin;WU Hechen;MA Pengtao(College of Chemistry and Chemical Engineering,Henan University,Kaifeng 475004,Henan,China;Henan Experimental Wenbo School,Zhengzhou 450002,Henan,China)

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》2018年第4期376-380,共5页Chemical Research

基　　金：河南大学大学生创新训练计划(201810475016)

摘　　要：采用常规水溶液合成法成功制备了一例新颖的有机-无机杂化的杂多钼酸盐(C_(3)N_(2)H_(5))_(4)H[HPMo_(6)O_(21)(O_(2)CC_(6)H_(4)NH_(2))_(3)]·6H_(2)O(1),并通过X射线单晶衍射、红外光谱、紫外光谱、热失重分析等方法对该化合物的结构进行表征.结构分析表明,化合物1属于三斜晶系,P-1空间群,晶胞参数a=1.3191(9)nm,b=2.0688(15)nm,c=2.3222(16)nm,V=5.701(7)nm3.化合物1包含1个[HPMo_(6)O_(21)(O_(2)CC_(6)H_(4)NH_(2))_(3)]^(5-)阴离子,4个[C_(3)N_(2)H_(5)]^(+)阳离子,1个H+质子和6个结晶水.化合物1聚阴离子结构中包含一个{PMo6}结构单元,3个对氨基苯甲酸配体通过羧基上的两个氧原子以近乎垂直的方式连接在{PMo_(6)}单元同一侧.紫外光谱研究表明,化合物1在水溶液中6 h内保持相对稳定,能够稳定存在的pH范围大致是7.5~10.5.A new heteropolymolybdate(C_(3)N_(2)H_(5))_(4)H[HPMo_(6)O_(21)(O_(2)CC_(6)H_(4)NH_(2))_(3)]·6H_(2)O(1)has been synthesized and characterized by X-ray single-crystal diffraction,IR spectrum,UV spectrum and thermogravimetric(TG)analyses.Structural analyses showed that 1 crystallizes in the triclinic P-1 space group with the cell parameters:a=1.3191(9)nm,b=2.0688(15)nm,c=2.3222(16)nm,V=5.701(7)nm 3.Compound 1 consists of one[HPMo_(6)O_(21)(O_(2)CC_(6)H_(4)NH_(2))_(3)]^(5-)polyanion,four[C3N2H5]+ions,one H+proton and six lattice water molecules.Three 4-aminobenzoic acid ligands covalently grafted onto the{PMo_(6)}subunit through two oxygen atoms from the carboxyl group.The study of UV spectra indicates that 1 is stable in the pH value ranging from 7.5 to 10.5 in solution.

关 键 词：杂多钼酸盐 {PMo_(6)}结构单元 对氨基苯甲酸 紫外光谱 

分 类 号：O612.6[理学—无机化学]