{"id":{"repo_id":"lethbridge","oai_identifier":"oai:opus.uleth.ca:10133/668"},"canonical_url":"https://search.dev.ndltd.org/etd/lethbridge/oai:opus.uleth.ca:10133/668","repository":{"repo_id":"lethbridge","name":"University of Lethbridge","base_url":"https://opus.uleth.ca/server/oai/request"},"display":{"title":"The preparation and characterization of tungsten and molybdenum sulfide fluorides","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.","abstract_html":"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.","abstract_has_math":false,"creators":["Nieboer, Jared","University of Lethbridge. Faculty of Arts and Science"],"institution":null,"degree_name":null,"degree_level":null,"degree_discipline":null,"degree_department":null,"school":null,"contributors":[],"advisors":[],"committee_chairs":[],"committee_members":[],"year":2007,"date_issued":"2007","date_published":"2007","updated_at":"2026-07-27T20:02:08Z","subjects":["Dissertations, Academic","Tungsten -- Synthesis","Molybdenum -- Synthesis","Tungsten -- Research","Molybdenum -- Research"],"languages":[],"rights":[],"rights_urls":[],"identifier_entries":[{"key":"dc:identifier","label":"Identifier","values":["hdl:10133/668"],"render_values":[{"text":"hdl:10133/668","href":null,"code":true}]}]},"links":{"outbound_url":null,"outbound_label":null,"outbound_source":null},"metadata_groups":[{"id":"academic_context","label":"Academic Context","entries":[{"key":"dc:date.issued","label":"Date","values":["2007"]},{"key":"dc:type","label":"Dc Type","values":["Thesis"]}]},{"id":"subjects_keywords","label":"Subjects and Keywords","entries":[{"key":"dc:subject","label":"Dc Subject","values":["Dissertations, Academic","Tungsten -- Synthesis","Molybdenum -- Synthesis","Tungsten -- Research","Molybdenum -- Research"]}]},{"id":"identifiers","label":"Identifiers","entries":[{"key":"dc:identifier","label":"Identifier","values":["hdl:10133/668"]}]},{"id":"additional","label":"Additional Metadata","entries":[{"key":"dc:description.other","label":"Dc Description Other","values":["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."]},{"key":"dc:title","label":"Title","values":["The preparation and characterization of tungsten and molybdenum sulfide fluorides"]}]}],"canonical_facts":{"dc:date.issued":["2007"],"dc:description.other":["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."],"dc:identifier":["hdl:10133/668"],"dc:subject":["Dissertations, Academic","Tungsten -- Synthesis","Molybdenum -- Synthesis","Tungsten -- Research","Molybdenum -- Research"],"dc:title":["The preparation and characterization of tungsten and molybdenum sulfide fluorides"],"dc:type":["Thesis"]},"updated_at":"2026-07-27T20:02:08Z"}