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{[PMo12O40][Ce(DMF)7]2}·{PMo12O40}的合成及晶体结构

Synthesis and crystal structure of {[PMo12O40][Ce(DMF)7]2}·{PMo12O40}

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【作者】 李晓辉; 何喆;

【Author】 LI Xiao-hui,HE Zhe(School of Chemistry and Chemical Engineering,Liaoning Normal University,Dalian 116029,China)

【机构】 辽宁师范大学化学化工学院;

【摘要】 以α-H3PMo12O40.24H2O,CeCl3.7H2O和DMF(N,N-二甲基甲酰胺)为原料,在乙腈和水的混合溶剂中合成了具有Keggin结构的标题化合物{[PMo12O40][Ce(DMF)7]2}.{PMo12O40}.以单晶X-射线衍射分析I、R光谱和TG分析对其进行了表征.该化合物属于单斜晶系,P2(1)/c空间群.晶体结构中包含2个[Ce(DMF)7]3+配阳离子和2个[PMo12O40]3-阴离子,其中1个多酸阴离子独立存在,而另1个多酸阴离子同时与2个[Ce(DMF)7]3+配阳离子配位.在配阳离子中,Ce3+与7个DMF分子中的7个氧和1个多酸阴离子的1个端基氧配位.IR光谱和X-射线单晶结构分析显示在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.热分析表明,由于Ce3+阳离子的影响,标题化合物中[PMo12O40]3-阴离子的稳定性明显提高.

【Abstract】 The title compound {[PMo12O40][Ce(DMF)7]2}·{PMo12O40} with Keggin structure has been synthesized in acetonitrile-water by reaction of α-H3PMo12O40·24H2O with CeCl3·7H2O and DMF(N,N-Dimethylformamide),and characterized by single crystal X-ray diffraction,IR spectrum and TG analysis.It is in monoclinic system with space group P2(1)/c.The crystal contains two [Ce(DMF)7]3+ coordination cations and two [PMo12O40]3-anions.One of the two polyanions is isolated and the other is coordinated to two [Ce(DMF)7]3+ cations.Each Ce3+ center coordinated with seven O atoms from seven DMF molecules and a terminal O atom from one polyanion.The IR spectrum and single-crystal X-ray diffraction studies indicate that there is strong interaction between the polyanion and organic group in the solid state.The thermal analysis showed that the stability of the [PMo12O40]3-polyanion was enhanced due to the influence of Ce3+ ions.

【基金】 辽宁省教育厅科学技术研究项目(2008364)
  • 【文献出处】 辽宁师范大学学报(自然科学版) ,Journal of Liaoning Normal University(Natural Science Edition) , 编辑部邮箱 ,2011年01期
  • 【分类号】O621.4
  • 【被引频次】1
  • 【下载频次】58
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