Synthesis and characterization of the platinum-substituted keggin anion α-H2SiPtW11O404-

Peter Klonowski, James C. Goloboy, Fernando J. Uribe-Romo, Furong Sun, Lingyang Zhu, Felipe Gándara, Corinne Wills, R. John Errington, Omar M. Yaghi, Walter G. Klemperer

Research output: Contribution to journalArticle

Abstract

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 α-H2SiPtW11O404- 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-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.

Original languageEnglish (US)
Pages (from-to)13239-13246
Number of pages8
JournalInorganic Chemistry
Volume53
Issue number24
DOIs
StatePublished - Dec 15 2014

ASJC Scopus subject areas

  • Physical and Theoretical Chemistry
  • Inorganic Chemistry

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    Klonowski, P., Goloboy, J. C., Uribe-Romo, F. J., Sun, F., Zhu, L., Gándara, F., Wills, C., Errington, R. J., Yaghi, O. M., & Klemperer, W. G. (2014). Synthesis and characterization of the platinum-substituted keggin anion α-H2SiPtW11O404-. Inorganic Chemistry, 53(24), 13239-13246. https://doi.org/10.1021/ic502617k