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在水热条件下,利用三缺位Keggin杂多磷钨酸盐前躯体Na9[α-PW9O34].7H2O与CuCl2、CdSO4、乙二胺反应,合成了一种新的无机-有机复合磷钨酸盐[Cu(en)2][Cu(en)2H2O]2[Cd(H2O)PW11O39].2H2O,并经红外光谱、热重分析、循环伏安、电催化等测试手段进行了表征.结果表明,标题化合物属于单斜晶系,空间群P21/c,晶胞参数:a=1.2872(2)nm,b=1.4781(2)nm,c=3.1965(5)nm,α=90.00°,β=93.270(2)°,γ=90.00°,V=6.0718(16)nm3,Z=4,Dc=3.753g/cm3,GOOF=1.015,R1=0.0653,wR2=0.1384.标题化合物分子由1个[Cu(en)2]2+、2个[Cu(en)2H2O]42+、1个镉取代的杂多阴离子[Cd(H2O)PW11O39]6-及2个H2O组成,并通过铜氧弱作用及氢键形成超分子网络.
Under hydrothermal conditions, a new inorganic-organic complex phosphotungstic acid was synthesized by the reaction of Na9 [α-PW9O34] 7H2O with CuCl2, CdSO4 and ethylenediamine. Salt [Cu (en) 2] [Cu (en) 2H2O] 2 [Cd (H2O) PW11O39] .2H2O was prepared and characterized by IR, TG, cyclic voltammetry and electrocatalysis. , The title compound belongs to the monoclinic space group P21 / c with unit cell parameters of a = 1.2872 (2) nm, b = 1.4781 (2) nm, c = 3.1965 93.270 (2) °, γ = 90.00 °, V = 6.0718 (16) nm3 Z = 4 Dc = 3.753 g / cm3 GOOF = 1.015 R1 = 0.0653 wR2 = 0.1384 The title compound consists of 1 Cu (2) 2 +, 2 [Cu (en) 2H2O] 42 +, one cadmium-substituted heteropolyanion [Cd (H2O) PW11O39] 6- and two H2O, Hydrogen bonds form supramolecular networks.