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Synthesis and Characterization of the Platinum-Substituted Keggin Anion α-H2SiPtW11O404-

Lookup NU author(s): Dr Corinne Wills, Dr John ErringtonORCiD


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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.

Publication metadata

Author(s): Klonowski P, Goloboy JC, Uribe-Romo FJ, Sun FR, Zhu LY, Gandara F, Wills C, Errington RJ, Yaghi OM, Klemperer WG

Publication type: Article

Publication status: Published

Journal: Inorganic Chemistry

Year: 2014

Volume: 53

Issue: 24

Pages: 13239-13246

Print publication date: 15/12/2014

Online publication date: 19/11/2014

ISSN (print): 0020-1669

ISSN (electronic): 1520-510X

Publisher: American Chemical Society


DOI: 10.1021/ic502617k


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Funder referenceFunder name
BASF (Ludwigshafen, Germany)
DE-AR-0000185DOE Advanced Research Projects Agency-Energy (ARPA-E)
DEFG02-91ER45439U.S. Department of Energy, Division of Materials Sciences through the Frederick Seitz Materials Research Laboratory
DE-AC02-05CH11231Office of Science, Office of Basic Energy Sciences, of the U.S. Department of Energy
DE-AC02-05CH11231Office of Science, Office of Basic Energy Sciences, of the U.S. DOE