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

Journal Article · Mon Dec 15 00:00:00 EST 2014 · Inorganic Chemistry

DOI:https://doi.org/10.1021/ic502617k· OSTI ID:1211147

Klonowski, P; Goloboy, JC; Uribe-Romo, FJ; Sun, FR; Zhu, LY; Gandara, F; Wills, C; Errington, RJ; Yaghi, OM; Klemperer, WG

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.

• Sponsoring Organization: USDOE Advanced Research Projects Agency - Energy (ARPA-E)
• DOE Contract Number: DE-AR0000185
• OSTI ID: 1211147
• Journal Information: Inorganic Chemistry, Vol. 53, Issue 24; ISSN 0020-1669
• Country of Publication: United States
• Language: English