Synthesis and Characterization of the Platinum-Substituted Keggin Anion 伪-H2SiPtW11O404鈥?/sup>

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• 作者：Peter Klonowski ; James C. Goloboy ; Fernando J. Uribe-Romo ; Furong Sun ; Lingyang Zhu ; Felipe G谩ndara ; Corinne Wills ; R. John Errington ; Omar M. Yaghi ; Walter G. Klemperer
• 刊名：Inorganic Chemistry
• 出版年：2014
• 出版时间：December 15, 2014
• 年：2014
• 卷：53
• 期：24
• 页码：13239-13246
• 全文大小：448K
• ISSN：1520-510X

文摘

Acidification of an aqueous solution of K₈SiW₁₁O₃₉ and K₂Pt(OH)₆ to pH 4 followed by addition of excess tetramethylammonium (TMA) chloride yielded a solid mixture of TMA salts of H₂SiPtW₁₁O₄₀^{4鈥?/sup> (1) and SiW₁₂O₄₀4鈥?/sup> (2). The former was separated from the latter by extraction into an aqueous solution and converted into tetra-n-butylammonium (TBA) and potassium salts TBA-1 and K-1. The 伪-H₂SiPtW₁₁O₄₀4鈥?/sup> was identified as a monosubstituted Keggin anion using elemental analysis, IR spectroscopy, X-ray crystallography, electrospray ionization mass spectrometry, 195Pt NMR spectroscopy, 183W NMR spectroscopy, and 183W鈥?sup>183W 2D INADEQUATE NMR spectroscopy. Both TBA-1 and K-1 readily cocrystallized with their unsubstituted Keggin anion salts, TBA-2 and K-2, respectively, providing an explanation for the historical difficulty of isolating certain platinum-substituted heteropolyanions in pure form.}