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Cluster synthesis. 33. New platinum-osmium carbonyl cluster complexes from Pt sub 2 Os sub 5 (CO) sub 17 (. mu. -H) sub 6 : Synthesis and characterization of PtOs sub 5 (CO) sub 15 (. mu. sub 3 -S)(. mu. -H) sub 6 , PtOs sub 5 (CO) sub 18 (. mu. -H) sub 4 , and PtOs sub 4 (CO) sub 15 (. mu. -H) sub 2

Journal Article · · Inorganic Chemistry; (United States)
DOI:https://doi.org/10.1021/ic00014a015· OSTI ID:6069430
; ;  [1]
  1. Univ. of South Carolina, Columbia (United States)

From the reaction of Pt{sub 2}Os{sub 5}(CO){sub 17}({mu}{minus}H){sub 6} with H{sub 2}S at 25C the new platinum-osmium carbonyl cluster complex PtOs{sub 5}{minus}(CO){sub 15}({mu}{sub 3}{minus}S)({mu}{minus}H){sub 6} (2) was obtained in 83% yield. Compound 2 was characterized by ir, {sup 1}H NMR, {sup 13}C NMR, and single-crystal x-ray diffraction analyses. The structure of 2 consists of a PtOs{sub 3} tetrahedron fused to a PtOs{sub 2} triangle with the platinum atom at the vertex-sharing site. There is a triply bridging sulfido ligand on the PtOs{sub 2} triangular grouping. The molecule was shown by variable-temperature {sup 1}H NMR and {sup 13}C NMR spectroscopy to undergo a dynamic process that involves an intramolecular rotation of the Os{sub 2} triangular group relative to the Os{sub 2}S grouping at the platinum atom. {Delta}G {sub 261} = 12.3 kcal/mol. The reaction of Pt{sub 2}Os{sub 5}(CO){sub 17}({mu}-H){sub 6} with Os(CO){sub 5} at 25C yielded two new platinum-osmium carbonyl cluster complexes PtOs{sub 5}(CO){sub 18}({mu}{minus}H){sub 4} (3) and PtOs{sub 4}(CO){sub 15}({mu}{minus}H){sub 2} (4) in 38% and 25% yields, respectively. Both compounds were characterized crystallographically. The cluster of compound 3 consists of a PtOs{sub 5} tetrahedron fused to a PtOs{sub 2} triangle by the vertex-sharing platinum atom. The cluster of compound 3 contains a PtOs{sub 3} tetrahedron with an edge-bridging Os(CO){sub 4} group. The positions of all the hydride ligands in 3 and 4 were determined by a combination of {sup 1}H NMR spectroscopy and crystallography. Compound 3 is readily degraded by CO (25C/1 atm) to yield the products PtOs{sub 2}(CO){sub 10}, H{sub 2}Os{sub 2}(CO){sub 10}, H{sub 2}Os{sub 2}(CO){sub 8}, and H{sub 2}Os(CO){sub 4}. Crystal data for compound 2, 3, and 4 are presented. 12 refs., 3 figs., 10 tabs.

OSTI ID:
6069430
Journal Information:
Inorganic Chemistry; (United States), Journal Name: Inorganic Chemistry; (United States) Vol. 30:14; ISSN 0020-1669; ISSN INOCA
Country of Publication:
United States
Language:
English