di Synthesis and Characterization of the Platinum-Substituted Keggin Anion alpha-H2SiPtW11O404

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 H2SiPtW11O404- (1) and SiW12O404- (2). The former was separated from the latter by extraction into an aqueous solution...

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Bibliographic Details
Published in:Inorganic chemistry 2014-12, Vol.53 (24)
Main Authors: Klonowski, P, Goloboy, JC, Uribe-Romo, FJ, Sun, FR, Zhu, LY, Gandara, F, Wills, C, Errington, RJ, Yaghi, OM, Klemperer, WG
Format: Article
Language:English
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Summary: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 H2SiPtW11O404- (1) and SiW12O404- (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 a-H2SiPtW11O404- was identified as a monosubstituted Keggin anion using elemental analysis, IR spectroscopy, X-ray crystallography, electrospray ionization mass spectrometry, Pt-195 NMR spectroscopy, (183)W NMR spectroscopy, and W-183-W-183 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.
ISSN:0020-1669
1520-510X
DOI:10.1021/ic502617k