The preparation and characterization of tungsten and molybdenum sulfide fluorides
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Date
2007
Authors
Nieboer, Jared
University of Lethbridge. Faculty of Arts and Science
Journal Title
Journal ISSN
Volume Title
Publisher
Lethbridge, Alta. : University of Lethbridge, Faculty of Arts and Science, 2007
Abstract
Silanethiolate salts of K(18-crown-6)+, N(CH3)4
+, Cs+, K+ were synthesized and
characterized by vibrational and NMR spectroscopy. The [N(CH3)4][SSi(CH3)3] salt was
used to prepare the new [N(CH3)4][WSF5] salt directly from WF6. Alternatively,
[N(CH3)4][WSF5] was prepared by the reaction of WSF4 with [N(CH3)4][F].
Pure WSF4 was prepared via a facile new route and was fully characterized by
Raman, infrared, and 19F NMR spectroscopy, and an improved crystal structure. The
Lewis-acid properties of WSF4 were studied in reactions with pyridine, yielding the new
WSF4·C5H5N adduct, which was studied by Raman and 19F NMR spectroscopy. A 2:1
stoichiometry of WSF4 and [N(CH3)4][F] yielded W2S2F9
- in solution. The novel
W2SOF9
- anion was characterized in solution by 19F NMR spectroscopy.
Molybdenum sulfide tetrafluoride was synthesized and unambiguously
characterized by Raman, infrared, and 19F NMR spectroscopy and single-crystal X-ray
diffraction.
The experimental characterization of WSF4, MoSF4, WSF5
-, and SSi(CH3)3
- was
supplemented by density functional theory calculations.
Description
xv, 131 leaves : ill. ; 29 cm.
Keywords
Dissertations, Academic , Tungsten -- Synthesis , Molybdenum -- Synthesis , Tungsten -- Research , Molybdenum -- Research