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通过三缺位Keggin结构杂多阴离子[α-A-PW9O34]9-和二氯甲基苯基硅烷在乙腈溶液中反应,合成了一例结构新颖的甲基苯基硅衍生物[(C4H9)4N]3[α-A-PW9O34(C6H5SiCH3)3](1),并对其进行元素分析,红外光谱,紫外光谱,热分析和X-射线单晶衍射等表征。该配合物属于三方晶系,空间群为R3m,晶胞参数:a=2.261 3(2)nm,b=2.261 3(2)nm,c=1.797 6(4)nm,V=7.960 2(18)nm3,Z=3。在配合物中,阴离子[α-A-PW9O34(C6H5SiCH3)3]3-呈C3v对称,3个甲基苯基硅基团连接在三缺位的阴离子[α-A-PW9O34]9-表面,整个阴离子显示“开放结构”。
By the reaction of tri-vacancy Keggin heteropolyanion [α-A-PW9O34] 9- with dichloromethylphenylsilane in acetonitrile, a novel methylphenylsilicone derivative [(C4H9) 4N ] 3 [α-A-PW9O34 (C6H5SiCH3) 3] (1) and characterized by elemental analysis, IR, UV, thermal analysis and X-ray single crystal diffraction. The complex belongs to the triclinic system with the space group R3m and unit cell parameters: a = 2.261 3 (2) nm, b = 2.261 3 (2) nm, c = 1.797 6 (4) nm, V = 7.960 2 ) nm3, Z = 3. In the complex, the anion [α-A-PW9O34 (C6H5SiCH3) 3] 3- is C3v symmetrical and the three methylphenylsilyl groups are connected to the 9-surface of the anion [α-A-PW9O34] The whole anion shows “open structure ”.