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Clusters containing carbene ligands. 7. Preparation of Os sub 3 (CO) sub 8 (C(H)NMe sub 2 )(. mu. sub 3 -S)(. mu. -H) sub 2 and the nature of its reactions with secondary and tertiary amines

Journal Article · · Journal of the American Chemical Society; (USA)
DOI:https://doi.org/10.1021/ja00165a028· OSTI ID:6619989
; ; ; ;  [1]
  1. Univ. of South Carolina, Columbia (USA)
+ Show Author Affiliations
Os{sub 3}(CO){sub 9}({mu}{sub 3}-CO)({mu}{sub 3}-S) and Os{sub 3}(CO){sub 10}({mu}-SPh)({mu}-H) were found to react with NMe{sub 3} to yield the complex Os{sub 3}-(CO){sub 8}(C(H)NMe{sub 2})({mu}{sub 3}-S)({mu}H){sub 2} (1a) in yields of 31% and 26%, respectively. Os{sub 3}(CO){sub 10}({mu}CNMe{sub 2})({mu}-H) was found to react with H{sub 2}S to yield 1a in 36% yield. Compound 1a was analyzed by a single-crystal X-ray diffraction analysis and was found to contain a secondary (dimethylamino)carbene ligand terminally coordinated to a sulfur-bridged triosmium cluster. 1e was decarbonylated at 145{degree}C to give Os{sub 3}(CO){sub 7}(C(H)N(Et)(CH{sub 2}){sub 2}NMe{sub 3})({mu}{sub 3}-S)({mu}-H){sub 2} (2e) in 41% yield. Compound 2e was characterized by a single-crystal X-ray diffraction analysis and was found to contain a terminally coordinated C(H)N(Et)(CH{sub 2}){sub 2}NMe{sub 2} carbene ligand chelated to the cluster through coordination of the NMe{sub 2} group. A mechanism is proposed that involves iminium ligand intermediates that couple to the carbene ligand to form a nitrogen-containing metallacycle.
OSTI ID:
6619989
Journal Information:
Journal of the American Chemical Society; (USA), Journal Name: Journal of the American Chemical Society; (USA) Vol. 112:9; ISSN 0002-7863; ISSN JACSA
Country of Publication:
United States
Language:
English

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Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400201* -- Chemical & Physicochemical Properties
CARBENES
CHEMICAL REACTIONS
COMPLEXES
CRYSTAL STRUCTURE
DATA
DATA ANALYSIS
EXPERIMENTAL DATA
INFORMATION
MEASURING INSTRUMENTS
MEASURING METHODS
NUMERICAL DATA
ORGANIC COMPOUNDS
ORGANOMETALLIC COMPOUNDS
OSMIUM COMPLEXES
RADICALS
SYNTHESIS
TRANSITION ELEMENT COMPLEXES