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Cluster syntheses. 14. The syntheses and structural characterization of the high-nuclearity sulfidoruthenium carbonyl cluster compounds Ru/sub 5/(CO)/sub 14/(. mu. /sub 4/-S)/sub 2/, Ru/sub 6/(CO)/sub 17/(. mu. /sub 4/-S)/sub 2/, and Ru/sub 7/(CO)/sub 20/(. mu. /sub 4/-S)/sub 2/

Journal Article · · Inorg. Chem.; (United States)
DOI:https://doi.org/10.1021/ic00264a017· OSTI ID:5648615
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The reaction of Ru/sub 3/(CO)/sub 9/(..mu../sub 3/-S)/sub 2/ (2) with Ru/sub 3/(CO)/sub 12/ under UV irradiation has yielded the higher nuclearity cluster compounds Ru/sub 4/(CO)/sub 9/(..mu..-CO)/sub 2/(..mu../sub 4/-S)/sub 2/ (3), 38%, Ru/sub 5/(CO)/sub 14/(..mu../sub 4/-S)/sub 2/ (4), 20%, and Ru/sub 6/(CO)/sub 17/(..mu../sub 4/-S)/sub 2/ (5), 3%. Thermal decarbonylation of Ru/sub 3/(CO)/sub 9/(..mu../sub 3/-CO)(..mu../sub 3/-S) (1) at 100/sup 0/C has yielded 3, 47%, 5, 10%, and Ru/sub 7/(CO)/sub 20/(..mu../sub 4/-S)/sub 2/ (6), 26%. The large clusters are decomposed to 2 and 3 by reaction with CO at 1 atm. Compounds 4-6 have been characterized by single-crystal X-ray diffraction analyses. For 4: space group P2/sub 1//n, a = 8.787 (2) A, b = 14.550 (3) A, c = 19.741 (3) A, ..beta.. = 98.09 (1)/sup 0/, Z = 4, rho/sub calcd/ = 2.56 g/cm/sup 3/. The cluster consists of an approximately square arrangement of four ruthenium atoms with quadruply bridging sulfido ligands on each face. An Ru(CO)/sub 4/ unit bridges one Ru-Ru edge of the cluster. But the EAN rule the molecule is unsaturated, and one of the Ru-Ru bonds was found to be unusually short, 2.704 (1) A. For 5: space group P2/sub 1/2/sub 1/2/sub 1/, a = 11.211 (2) A, b = 14.666 (4) A, c = 17.611 (4) A, Z = 4, rho/sub calcd/ = 2.63 g/cm/sup 3/. Compound 5 is isomorphous and isostructural with the know osmium homologue. The molecule consists of a pentagonal-bypyramidal cluster of five ruthenium atoms with two sulfido ligands. A Ru(CO)/sub 4/ group bridges one apical-equatorial edge of the cluster. For 6: space group P2/sub 1/2/sub 1/2/sub 1/, a = 11.226 (3) A, b = 14.320 (4) A, c = 21,217 (5) A, Z = 4, rho/sub calcd/ = 2.59 g/cm/sup 3/. Compound 6 is isomorphous and isostructural with the known osmium homologue. The molecule consists of a pentagonal-bipyramidal cluster of five ruthenium atoms and two sulfido ligands. Two Ru(CO)/sub 4/ groups bridge symmetrically adjacent apical-equatorial edges of the cluster.
Research Organization:
Univ. of South Carolina, Columbia
OSTI ID:
5648615
Journal Information:
Inorg. Chem.; (United States), Journal Name: Inorg. Chem.; (United States) Vol. 26:17; 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
CARBONYLS
CHALCOGENIDES
CHEMICAL PREPARATION
COHERENT SCATTERING
CRYSTAL STRUCTURE
DATA
DIFFRACTION
EXPERIMENTAL DATA
INFORMATION
MOLECULAR STRUCTURE
NUMERICAL DATA
REFRACTORY METAL COMPOUNDS
RUTHENIUM COMPOUNDS
SCATTERING
SPACE GROUPS
SULFIDES
SULFUR COMPOUNDS
SYNTHESIS
TRANSITION ELEMENT COMPOUNDS
X-RAY DIFFRACTION