| 12-钨磷酸二甲基胺盐的制备和结构研究 |
| SYNTHESIS AND CRYSTAL STRUCTURE OF TRI-(DIMETHYLAMMONIUM)DODECATUNGSTOPHOSPHATE |
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| 摘要: 本文由12-钨磷酸与二甲基甲酰胺反应制备了12-钨磷酸二甲基胺盐[(CH)3)2NH2]3(PW12O40)·nH2O,用红外光谱和热重差热分析研究了化合物的性质,用X射线单晶结构分析测定了化合物的结构.晶体属单斜晶系,空间群为C2h3-C2/m,结晶学参数为:a=19.345(7),b=16.506(2),c=12.711(2)Å,β=101.83(2)°,V=3972.5(Å3,Z=4,Dc=3.037g/cm3.结构测定共收集了4414个独立衍射点,其中2917个I>3σ(I)独立可观察衍射点,结构用全矩阵最小二乘法修正后最后R=0.0856,Rw=0.1186.在分子结构中,杂阴离子为完整的α-Keggin型结构,三个二甲基胺阳离子位于一组W3O13三联体与其他三组W3O13三联体通过共顶点相连而形成的面上.由于阳离子与杂阴离子骨架氧之间的氢键作用.致使WO6八面体发生较大的畸变,与阳离子发生氢键作用的WO6八面体中的W-O键显著减弱,在红外光谱中表现为υW-O吸收峰的分裂. |
| 关键词: 12-钨磷酸盐 二甲基胺 N,N-二甲基甲酰胺 晶体结构 |
| 基金项目: |
| Abstract: The crystal of [(CH3)2NH2]3(PW12O40)·2H2O has been synthesized and studied by IR spec trum, TG-DTA thermal analysis and X-ray single crystal analysis. The crystal is monoclinic, with space group C2h3-C2/ m. The crystal data are: a=19.345(7), b=16.506(2), c=12.711(2)Å, β=101.83(2)°, V=3972.5Å3, and Z=4, Dc=3.039g/cm3. The structure was determined from 4414 reflections, of which 2917 with I> 3δ(I)were considered as observed, and refined by a full-matrix least-squares method to R=0.0856 and Rw==0.11856. The heteropolyanion is of perfect α-Keggin type structure. The three cations(CH3)2NH2+ are in the faces constituted by one W3O13triplet linked with the other three W3O13triplets by shared corner. Because of the hydrogen-bonding association between hydrogens of cations with oxygens of heteropolyanion, the WO6 octahedron of the Keggin structure is distorted, and the W-O bonds of the WO6 octahedra associating with cations are weakened obviously, leading to the split of W-O vibration absorption peaks in the IR spectrum. |
| Keywords: dodecatungstophosphate dimethylammonium N,N-dimethyIformamide crystal structure |
| 投稿时间：1988-04-29 |
| 摘要点击次数: 1870 |
| 全文下载次数: 1769 |
| 丁建平,顾翼东,吴光,王溥义.12-钨磷酸二甲基胺盐的制备和结构研究[J].无机化学学报,1991,7(1):1-6. |
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