| Dawson结构聚金属氧酸盐有机-无机复合物[{Y(DMSO)5(H2O)3}{Y(DMSO)8}][P2W18O62]·2DMSO·2H2O的合成、性质及晶体结构 |
| Synthesis， Characterization and Crystal Structure of a Polyoxometalate-Based Organic-Inorganic Compound，[{Y(DMSO)5(H2O)3}{Y(DMSO)8}][P2W18O62]·2DMSO·2H2O |
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| 摘要: 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[{Y(DMSO)5(H2O)3}{Y(DMSO)8}][P2W18O62]·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[I≥ 2σ(I)]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。 |
| 关键词: Dawson结构 磷钨酸 合成 晶体结构 有机-无机复合物 |
| 基金项目: |
| Abstract: A composite compound of [{Y(DMSO)5(H2O)3}{Y(DMSO)8}][P2W18O62]·2DMSO·2H2O was synthesized from Y2O3， DMSO and α-H6P2W18O62·nH2O in mixed solvent of acetonitrile and water. Its structure was char-acterized via elemental analysis， IR， and single crystal X-ray diffraction analysis. The title compound crystallizes in a monocline lattice， P21/c， with a=1.7614(4)nm， b=3.1527(6)nm， c=2.1523(4)nm， β=90.40(3)°， V=11.963(4)nm3， Mr=5803.06， Z=4， Dc=3.222g·cm-3， μ=18.566mm-1， F(000)=10464， R=0.0745 and wR=0.1438. The result of crystal structure analysis indicates that both Y3+ ions are eight-coordinated and the coordination polyhedra around two Y3+ ions attribute to bicapped distorted trigonal prism. Cyclic Voltam-metry of compound (1mmol·L-1， pH=5.5) in the presence of Na2SO4(0.1mol·L-1) reveals five steps (one，one，one，one，two electron) reductions. CCDC： 199158. |
| Keywords: Dawson structure octadecatungstodiphosphorate synthesis crystal structure organic-inorganic compound |
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| 王敬平,郭东杰,牛景扬.Dawson结构聚金属氧酸盐有机-无机复合物[{Y(DMSO)5(H2O)3}{Y(DMSO)8}][P2W18O62]·2DMSO·2H2O的合成、性质及晶体结构[J].无机化学学报,2003,19(6):579-584. |
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