化学学报 ›› 1992, Vol. 50 ›› Issue (9): 849-875. 上一篇    下一篇

研究论文

Keggin结构钼硅杂多蓝的合成及晶体结构研究

王恩波;许林;沈恩洪;王作屏;林永华;金松春   

  1. 东北师范大学化学系;中国科学院长春应用化学研究所
  • 发布日期:1992-09-15

The synthesis and crystal structure of molybdenum-silicon blue

WANG ENBO;XU LIN;SHEN ENHONG;WANG ZUOPING;LIN YONGHUA;JIN SONGCHUN   

  • Published:1992-09-15

通过电化学还原的方法得到钼硅多酸的还原产物杂多蓝单晶H~8SiMo~12H~2O.测定了它的晶体结构.晶体空间群PI.a=1.3769(3)nm,b=1.4346(4)nm,c=1.4134(4)nm,a=120.47(2)°,β=110.70(2)°,γ=66.11(2)°;z=2,R=0.0608.确证杂多蓝阴离子呈现Keggin结构和与a-异构体特征,基本保持未还原杂多酸阴离子的结构.但是在结构畸变程度、键角和健长的变化以及结晶水的分布上 有明显不同.同时确定了杂多蓝阴离子结构中4个Mo^5+离子的位置.

关键词: 晶体结构测定, X射线衍射分析, KEGGIN结构, 钼硅杂多蓝, 钼硅杂多酸

The single crystal of heteropoly blue, H8SiMo12O40.12H2O, the electrochem. reduced product of molybdenum-silicon heteropoly acid (H4SiMo12O40), was prepared by electrochem. reduction and evaporation in a nitrogen atomsphere The crystal structure of the product was determine The heteropoly blue H8SiMo12O40.12H2O, is tudenic, space group P1 with a 1.3769(3), b 1.4346(4), c 1.4134(4) nm, a 120.47(2), b 110.70(2), g 66.11(2)? Z = 2 R = 0.0608. The heteropoly blue anion was determine to have Keggin structure and a-isomer and it remained the structure of the unreduced heteropoly acid anion. But the distortion of the structure and the changes of bond length and bond angle take place obviously. The 4 Mo5+ Positions were determine in the structure.

Key words: CRYSTAL STRUCTURE DETERMINATION, X-RAY DIFFRACTION ANALYSIS

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