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在水热条件下,利用三缺位Keggin多钨氧酸盐前驱体Na8[-αHAsVW9O34].11H2O与NiCl2.6H2O、乙二胺反应,合成了一种包含二核镍簇和四核镍簇的有机-无机复合的新型砷钨酸盐(enH2)3[Ni2(H2O)10][Ni4(H2O)2(-αAsVW9O34)2].en.8H2O,并经IR光谱、元素分析、热重分析和X射线单晶衍射等测试手段进行了表征.标题化合物属于三斜晶系,P-1空间群,晶胞参数:α=1.204 23(19),b=1.258 5(2),c=1.593 8(4)nm,α=97.472(3),β=108.229(3),γ=114.779(2)°,V=1.985 2(7)nm3,Z=1,Dc=4.589 g/cm3,GOOF=1.023,R1=0.044 3,wR2=0.113 8.X-射线单晶结构分析表明,标题化合物分子由3个质子化乙二胺阳离子[enH2]2+、1个二核镍簇阳离子[Ni2(H2O)10]4+、1个四核镍簇取代的夹心型多阴离子[Ni4(H2O)2(α-AsVW9O34)2]10-、1个游离的乙二胺分子和8个结晶水分子组成.
Hydrothermal conditions, the use of three vacancies Keggin polyoxotonate precursors Na8 [-αHAsVW9O34] .11H2O and NiCl2.6H2O, ethylenediamine reaction, the synthesis of a binary nickel-containing clusters and tetranuclear nickel clusters (EnH2) 3 [Ni2 (H2O) 10] [Ni4 (H2O) 2 (-αAsVW9O34) 2] .en.8H2O was synthesized and characterized by IR spectroscopy, elemental analysis, thermogravimetric analysis and X-ray single crystal diffraction, etc. The title compound belongs to the triclinic system, P-1 space group with unit cell parameters of α = 1.204 23 (19), b = 1.258 5 (2), c = 1.593 8 (4) nm, α = 97.472 (3) β = 108.229 (3) γ = 114.779 (2) ° V = 1.985 2 (7) nm3 Z = 1 Dc = 4.589 g / cm3 GOOF = 1.023 , R1 = 0.0443, wR2 = 0.113 8.X-ray single crystal structure analysis showed that the title compound consists of three protonated ethylenediamine cations [enH2] 2 +, one dinuclear nickel cluster cation [Ni2 10] 4 +, a tetranuclear nickel-substituted sandwich polyanion [Ni4 (H2O) 2 (α-AsVW9O34) 2] 10-, one free ethylenediamine molecule and eight crystal water molecules.