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以Na10[A-α-SiW9O34].18H2O、CuCl2.2H2O、EuCl3、联咪唑、4,4′-联吡啶为原料,利用水热法合成了有机-无机复合Keggin结构硅钨酸盐[H2bpy][H2bbpy][α-SiW12O40].2H2O[bpy=4,4′-bipyridine,bbpy=N-(2-(4,4′-bipyridyl))-4,4′-bipyridine],并借助元素分析、红外光谱和X射线单晶衍射对其组成和结构进行了表征.结果表明,标题化合物属于单斜晶系,P2(1)/c空间群,晶胞参数为:a=1.149 92(13)nm,b=2.137 6(3)nm,c=2.248 2(3)nm,β=98.406(2)°,V=5.466 7(111)nm3,Z=4,Dc=4.109g/cm3,GOOF=1.038,R1=0.057 5,wR2=0.118 4.其分子由1个饱和的硅钨酸盐[α-SiW12O40]4-阴离子,1个游离的双质子化[H2bbpy]2+阳离子,1个游离的双质子化[H2bpy]2+阳离子和2个结晶水分子组成.值得指出的是,4,4′-联吡啶分子在水热条件下发生反应,形成N-(2-(4,4′-联吡啶基))-4,4′-联吡啶.
The organic-inorganic composite Keggin structure silicotungstates [H2bpy] was synthesized by hydrothermal method using Na10 [A-α-SiW9O34] .18H2O, CuCl2.2H2O, EuCl3, biimidazole and 4,4’-bipyridine as raw materials. [H2bbpy] [α-SiW12O40] .2H2O [bpy = 4,4’-bipyridine, bbpy = N- IR spectra and X-ray single crystal diffraction.The results show that the title compound belongs to the monoclinic space group P2 (1) / c with unit cell parameters of a = 1.149 92 (13) nm , b = 2.137 6 (3) nm, c = 2.248 2 (3) nm, β = 98.406 (2) °, V = 5.466 7 (111) nm3, Z = 4, Dc = 4.109 g / cm3, GOOF = 1.038 , R1 = 0.057 5, wR2 = 0.118 4. The molecule consists of one saturated silicotungstate [α-SiW12O40] 4-anion, one free bis-protonated [H2bbpy] 2+ cation, one free bis Protonated [H2bpy] 2+ cation and two crystal water molecules.It is worth noting that the 4,4’-dipyridyl molecule reacts under hydrothermal conditions to form N- (2- (4,4’-bis Pyridyl)) - 4,4’-bipyridyl.