Synthesis and characterization of (Et/sub 4/N)(M(CO)/sub 5/SR) and (Et/sub 4/N)/sub 2/(M/sub 2/(CO)/sub 8/(SR)/sub 2/) complexes (M = Cr, Mo, W). Ligand substitution reactions and x-ray crystal structure of (Et/sub 4/N)/sub 2/(W/sub 2/(CO)/sub 8/(SPh)/sub 2/)
Journal Article
·
· Inorg. Chem.; (United States)
A series of complexes (Et/sub 4/N)(M(CO)/sub 5/SR) (M = Cr, Mo, W; R = H, Ph), have been synthesized and characterized by /sup 1/H and /sup 13/C NMR and ir spectroscopies. Gentle heating causes these complexes to lose a carbonyl ligand, yielding the doubly bridged sulfur dimers M/sub 2/(CO)/sub 8/(..mu..-SR)/sub 2//sup 2 -/. The x-ray crystal structure of (Et/sub 4/N)/sub 2/(W/sub 2/(CO)/sub 8/(SPh)/sub 2/) has been determined. The complex crystallizes in the triclinic space group P /anti 1/ with unit cell parameters a = 9.8664 (17) /angstrom/, b = 9.8566 (22) /angstrom/, c = 11.8270 (26) /angstrom/, ..cap alpha.. = 65.790 (16)/degrees/, ..beta.. = 81.710 (16)/degrees/, ..gamma.. = 82.000 (16)/degrees/, V = 1034.0 (4) /angstrom//sup 3/, and Z = 1. Both mono- and dinuclear metal complexes readily react with phosphorus donor ligands to afford the carbon monoxide substituted complexes cis-M(CO)/sub 4/(P)(SR)/sup -/ (P = PMe/sub 3/, P(OMe)/sub 3/, PPh/sub 3/). In addition, the dimers react with 1 atm of carbon monoxide to re-form the mononuclear species M(CO)/sub 5/SR/sup -/ in quantitative yields. Unsuccessful attempts to insert CO/sub 2/, COS, or CS/sub 2/ into the M-SR bond in the M(CO)/sub 5/SR/sup -/ derivatives are noted. 25 references, 3 figures, 15 tables.
- Research Organization:
- Texas A and M Univ., College Station (USA)
- OSTI ID:
- 6181315
- Journal Information:
- Inorg. Chem.; (United States), Journal Name: Inorg. Chem.; (United States) Vol. 27:20; ISSN INOCA
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400201* -- Chemical & Physicochemical Properties
400202 -- Isotope Effects
Isotope Exchange
& Isotope Separation
AROMATICS
CARBONYLS
CHROMIUM COMPLEXES
COMPLEXES
CRYSTAL STRUCTURE
DATA
EXPERIMENTAL DATA
INFORMATION
MOLYBDENUM COMPLEXES
NUMERICAL DATA
ORGANIC COMPOUNDS
ORGANIC NITROGEN COMPOUNDS
ORGANIC SULFUR COMPOUNDS
SYNTHESIS
TRANSITION ELEMENT COMPLEXES
TUNGSTEN COMPLEXES
400201* -- Chemical & Physicochemical Properties
400202 -- Isotope Effects
Isotope Exchange
& Isotope Separation
AROMATICS
CARBONYLS
CHROMIUM COMPLEXES
COMPLEXES
CRYSTAL STRUCTURE
DATA
EXPERIMENTAL DATA
INFORMATION
MOLYBDENUM COMPLEXES
NUMERICAL DATA
ORGANIC COMPOUNDS
ORGANIC NITROGEN COMPOUNDS
ORGANIC SULFUR COMPOUNDS
SYNTHESIS
TRANSITION ELEMENT COMPLEXES
TUNGSTEN COMPLEXES