两种有机-无机复合杂多化合物的水热合成及结构表征

利用水热法制备了基于饱和Keggin结构阴离子构筑的有机-无机复合多金属氧酸盐(4,4′-bipy)4H4PMo12O40](CH3COO).1.5H2O(1)和(4,4′-Hbipy)2(4,4′-bipy)2HPW12O40].3.5H2O(2)(4,4′-bipy=4,4′-联吡啶),并借助元素分析、红外光谱、紫外光谱、热分析和X射线单晶衍射分析了两种化合物的组成和结构.结果表明,化合物1和2均属于单斜晶系,P2(1)/c空间群.化合物的晶胞参数为:a=1.869 40(13)nm,b=1.404 23(9)nm,c=2.707 76(18)nm,β=105.848 0(10)°,V=6.837 9(8)nm3,Z=4,R1=0.095 4;化合物2的晶胞参数为:a=1.884 80(12)nm,b=1.409 89(9)nm,c=2.664 92(17)nm,β=105.368 0(10)°,V=6.828 4(8)nm3,Z=2,R1=0.097 2.两种化合物结构类似,其结构单元均是由饱和Keggin阴离子与游离的4,4′-联吡啶分子通过静电作用相结合形成的.

Hydrothermal Synthesis and Structural Characterization of Two Organic-Inorganic Composite Heteropoly Compounds

Organic-inorganic heteropoly compounds（4,4′-bipy）4H4PMo12O40]（CH3COO）·1.5 H2O（1） and（4,4′-Hbipy）2（4,4′-bipy）2HPW12O40]·3.5H2O（2）（4,4′-bipy = 4,4′-bipyridine） were synthesized based on construction of saturated Keggin polyoxoanions.Resultant heteropoly compounds were analyzed by means of elemental analysis,infrared spectrometry,ultraviolet spectrometry,thermogravimetric analysis,and X-ray single-crystal diffraction.Results indicate that compound 1 crystallizes in monoclinic system,P2（1）/c space group,with cell parameters a = 1.869 40（13） nm,b = 1.404 23（9） nm,c = 2.707 76（18） nm,β = 105.848 0（10）°,V = 6.837 9（8） nm3,Z = 4,and R1 = 0.095 4.Compound 2 crystallizes also in monoclinic system,P2（1）/c space group,with cell parameters a = 1.884 80（12） nm,b= 1.409 89（9） nm,c = 2.664 92（17） nm,β = 105.368 0（10）°,V = 6.828 4（8） nm3,Z = 2,and R1 = 0.097 2.The two compounds have very similar structure and both consist of a saturated Keggin polyoxoanion and free 4,4′-bipy molecules linked through electrostatic interactions.