锑离子帽式修饰的α-Keggin结构杂多钼酸盐的合成、结构及性质研究

Synthesis,structure and properties study of Sb-bicappedα-Keggin type polyoxometalates

用钼酸钠、二氧化硅、二氧化锑做原料,在水热条件下合成了2种新的锑离子帽修饰的α-Keggin型多金属氧酸盐(HC5H5N)3SiMo5^ⅤMo7^ⅥSb2O40 (1)和[Cu(C10H8N2)3](HC5H5N)[SiMo5^ⅤMo7^ⅥSb2O40]·7H2O(2)(C5H5N=吡啶;C10H8N2=2,2′-联吡啶).通过元素分析、红外光谱和X射线衍射方法确定了2种化合物的结构.结果表明:化合物1属于单斜晶系,C2/c空间群,晶胞参数a=4.500 2(3)nm,b=1.401 48(9)nm,c=1.527 17(4)nm,β=103.579 0(10)°,V=9.362 6(10)nm^3,Z=8,R1=0.062 0,wR2=0.136 2;化合物2属于单斜晶系,P2(1)/n空间群,晶胞参数a=1.572 03(6)nm,b=2.171 07(9)nm,c=2.706 79(11)nm,β=94.659 0°,V=9.207 7(6)nm^3,Z=4,R1=0.121 9,wR2=0.163 4.

Two new(HC5H5N)3SiMo12Sb2O40(1)and [Cu(C(10)H8N2)3](HC5H5N)[SiMo12Sb2O40]·7H2O(2)based on Sb-bicappedα-Keggin type polyoxometalates are synthesized under hydrothermal conditions by utilizing Na2MoO4 ·2H2O,SiO2,Sb2O3,2,2′-bipyridine and Cu(CH3COO)2 as raw materials.And the compounds are structurally characterized by elemental analysis,IR and single crystal X-ray diffractions.The two compounds both crystallize in the monoclinic system.For 1,space group C2/c,a=4.500 2(3)nm,b=1.401 48(9)nm,c=1.527 17(4)nm,β=103.579 0(10)°,V=9.362 6(10)nm^3,Z=8,R1=0.062 0,wR2=0.136 2.For 2,space group P21/n,a=1.572 03(6)nm,b=2.171 07(9)nm,c=2.706 79(11)nm,β=94.659 0°,V=9.207 7(6)nm^3,Z=4,R1=0.121 9,wR2=0.163 4.