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 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
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