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以α-H6P2W18O62·nH2O,Y2O3,DMSO(二甲亚砜)为原料合成了Dawson结构聚金属氧酸盐有机-无机复合物犤狖Y(DMSO)5(H2O)3狚狖Y(DMSO)8狚犦犤P2W18O62犦·2DMSO·2H2O(1),化合物晶体属于单斜晶系,P21/c空间群,Mr=5803.06,a=1.7614(4)nm,b=3.1527(6)nm,c=2.1523(4)nm,β=90.40(3)°,V=11.963(4)nm3,Dc=3.222g·cm-3,μ=18.566mm-1,Z=4,F(000)=10464。由17342个可观测衍射点犤I≥2σ(I)犦用于精修所有的结构参数,得一致性因子R=0.0745,wR=0.1438。结构解析表明,化合物中两个Y3+离子的配位环境均为八配位的畸变双冠三棱柱构型。CV行为研究表明,标题化合物中阴离子(pH=5.5)存在五步还原过程,得电子数依次为1,1,1,1,2。化合物的IR光谱和X-射线衍射结果表明,固态条件下配阳离子与杂多阴离子之间存在较强的相互作用。
The Dawson structure polyoxometalate organic-inorganic composite was synthesized from α-H6P2W18O62 · nH2O, Y2O3 and DMSO (DMSO) 5 (H2O) 3 The crystal of the compound belongs to the monoclinic space group P21 / c, Mr = 5803.06, a = 1.7614 (4) nm, b = 3.1527 (6) nm, c = 2.1523 (4) nm, β = 90.40 (3) °, V = 11.963 (4) nm3, Dc = 3.222g · cm-3, μ = 18.566mm-1, Z = 4, F (000) = 10464. From 17342 observable diffraction points 犤 I ≥ 2σ (I) 犦 for the refinement of all the structural parameters, the consistency factor R = 0.0745, wR = 0.1438. Structural analysis shows that the coordination environment of the two Y3 + ions in the compound is an eight-coordinate distorted double-crown triangular prism configuration. CV behavior studies show that the title compound anion (pH = 5.5) there is a five-step reduction process, the number of electrons were 1,1,1,1,2. The IR spectra and X-ray diffraction results of the compounds show that there is a strong interaction between the cationic and heteropolyanions under the solid state conditions.