Fluoride-ion acceptor properties of WSF4: synthesis, characterization, and computational study of the WSF5¯ and W2S2F9¯ anions and 19F NMR spectroscopic characterization of the W2OSF9¯ anion
Date
2012
Authors
Nieboer, Jared
Haiges, Ralf
Hillary, William
Yu, Xin
Richardet, Tyler
Mercier, Hélène P. A.
Gerken, Michael
Journal Title
Journal ISSN
Volume Title
Publisher
American Chemical Society
Abstract
The new [N(CH3)4][WSF5] salt was synthesized by two preparative methods: (a) by reaction of WSF4 with [N(CH3)4][F] in CH3CN and (b) directly from WF6 using the new sulfide-transfer reagent [N(CH3)4][SSi(CH3)3]. The [N(CH3)4][WSF5] salt was characterized by Raman, IR, and 19F NMR spectroscopy and [N(CH3)4][WSF5]·CH3CN by X-ray crystallography. The reaction of WSF4 with half an aliquot of [N(CH3)4][F] yielded [N(CH3)4][W2S2F9], which was characterized by Raman and 19F NMR spectroscopy and by X-ray crystallography. The WSF5– and W2S2F9– anions were studied by density functional theory calculations. The novel [W2OSF9]− anion was observed by 19F NMR spectroscopy in a CH3CN solution of WOF4 and WSF5–, as well as CH3CN solutions of WSF4 and WOF5–.
Description
Author accepted manuscript
Keywords
Salts , Anions , Fluorine , Nuclear magnetic resonance spectroscopy , Mathematical methods
Citation
Nieboer, J., Haiges, R., Hillary, W., Yu, X., Richardet, T., Mercier, H. P. A., & Gerken, M. (2012). Fluoride-ion acceptor properties of WSF4: Synthesis, characterization, and computational study of the WSF5¯ and W2S2F9¯ anions and 19F NMR spectroscopic characterization of the W2OSF9¯ anion. Inorganic Chemistry, 51(11), 6350-6359. https://doi.org/10.1021/ic3005882