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Article: Cluster synthesis. 7. Role of bridging sulfido ligands in the synthesis of platinum osmium carbonyl cluster compounds

TitleCluster synthesis. 7. Role of bridging sulfido ligands in the synthesis of platinum osmium carbonyl cluster compounds
Authors
Issue Date1984
Citation
Inorganic Chemistry, 1984, v. 23, n. 26, p. 4723-4732 How to Cite?
AbstractThe four platinum osmium sulfido carbonyl cluster compounds PtOs3(CO)10(PMe2Ph)2(μ 3-S) (I), PtOs3(CO)9(PMe2Ph)3(μ 3-S) (II), PtOs3(CO)9(PMe2Ph)2(μ 3-S) (III), and PtOs3(CO)8(PMe2Ph)3(μ 3-S) (IV) have been obtained from the reaction of Os3(CO)10(μ3-S) with Pt(PMe2Ph)4 at room temperature. All the products were characterized by IR and 1H NMR spectroscopy. Compounds I, II, and IV were also characterized by X-ray crystallographic analyses. All three compounds crystallize in the triclinic space group P1: (I) a = 8.558 (2) Å, b = 13.814 (3) Å, c = 15.214 (5) Å, α = 109.15 (2)°, β = 93.05 (2)°, γ = 95.75 (2)°, Z = 2, ρcalcd = 2.67 g/cm3; (II) a = 10.404 (4) Å, b = 13.746 (7) Å, c = 29.332 (16) Å, α = 85.23 (5)°, β = 88.43 (4)°, γ = 74.25 (4)°, Z = 4, ρcalcd = 2.48 g/cm3; (IV) a = 9.761 (4) Å, b = 11.926 (5) Å, c = 16.412 (6) Å, α = 78.57 (3)°, β = 89.16 (3)°, γ = 87.98 (6)°, Z = 2, ρcalcd = 2.55 g/cm3. All three structures were solved by the heavy-atom method and were refined to the final residuals RF = 0.060 and RwF = 0.071 for I, RF = 0.037 and RwF = 0.039 for II, and RF = 0.032 and RwF = 0.037 for IV. I and II are approximately planar clusters of one platinum and three osmium atoms. They have five metal-metal bonds and a triply bridging sulfido ligand on the PtOs2 triangular face. IV consists of a tetrahedral cluster of one platinum and three osmium atoms with a triply bridging sulfido ligand on the Os3 face. III is believed to be structurally analogous to IV. III and IV can be formed by the decarbonylation of I and II, respectively. This decarbonylation reaction is reversible. UV irradiation of solutions of II yields the compound HPtOs3(CO)7(PMe2Ph)2(PMe 2C6H4)(μ3-S) (V) in addition to IV. V was characterized by X-ray diffraction analysis: space group P1l, a = 10.432 (3) Å, b = 12.727 (6) Å, c = 14.448 (4) Å, α = 98.46 (3)°, β = 93.82°, γ = 91.82 (3)°, Z = 2, ρcalcd = 2.47 g/cm3. The structure of V was solved by the heavy-atom method and was refined to the final residuals RF = 0.037 and RwF = 0.042. V consists of a tetrahedral cluster of one platinum and three osmium atoms and has a triply bridging sulfido ligand on the triosmium face. The phenyl ring of one of the PMe2Ph ligands is orthometalated on a metal atom adjacent to the primary coordination site. © 1984 American Chemical Society.
Persistent Identifierhttp://hdl.handle.net/10722/219476
ISSN
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DC FieldValueLanguage
dc.contributor.authorAdams, Richard D.-
dc.contributor.authorHor, T. S Andy-
dc.date.accessioned2015-09-23T02:57:11Z-
dc.date.available2015-09-23T02:57:11Z-
dc.date.issued1984-
dc.identifier.citationInorganic Chemistry, 1984, v. 23, n. 26, p. 4723-4732-
dc.identifier.issn0020-1669-
dc.identifier.urihttp://hdl.handle.net/10722/219476-
dc.description.abstractThe four platinum osmium sulfido carbonyl cluster compounds PtOs3(CO)10(PMe2Ph)2(μ 3-S) (I), PtOs3(CO)9(PMe2Ph)3(μ 3-S) (II), PtOs3(CO)9(PMe2Ph)2(μ 3-S) (III), and PtOs3(CO)8(PMe2Ph)3(μ 3-S) (IV) have been obtained from the reaction of Os3(CO)10(μ3-S) with Pt(PMe2Ph)4 at room temperature. All the products were characterized by IR and 1H NMR spectroscopy. Compounds I, II, and IV were also characterized by X-ray crystallographic analyses. All three compounds crystallize in the triclinic space group P1: (I) a = 8.558 (2) Å, b = 13.814 (3) Å, c = 15.214 (5) Å, α = 109.15 (2)°, β = 93.05 (2)°, γ = 95.75 (2)°, Z = 2, ρcalcd = 2.67 g/cm3; (II) a = 10.404 (4) Å, b = 13.746 (7) Å, c = 29.332 (16) Å, α = 85.23 (5)°, β = 88.43 (4)°, γ = 74.25 (4)°, Z = 4, ρcalcd = 2.48 g/cm3; (IV) a = 9.761 (4) Å, b = 11.926 (5) Å, c = 16.412 (6) Å, α = 78.57 (3)°, β = 89.16 (3)°, γ = 87.98 (6)°, Z = 2, ρcalcd = 2.55 g/cm3. All three structures were solved by the heavy-atom method and were refined to the final residuals RF = 0.060 and RwF = 0.071 for I, RF = 0.037 and RwF = 0.039 for II, and RF = 0.032 and RwF = 0.037 for IV. I and II are approximately planar clusters of one platinum and three osmium atoms. They have five metal-metal bonds and a triply bridging sulfido ligand on the PtOs2 triangular face. IV consists of a tetrahedral cluster of one platinum and three osmium atoms with a triply bridging sulfido ligand on the Os3 face. III is believed to be structurally analogous to IV. III and IV can be formed by the decarbonylation of I and II, respectively. This decarbonylation reaction is reversible. UV irradiation of solutions of II yields the compound HPtOs3(CO)7(PMe2Ph)2(PMe 2C6H4)(μ3-S) (V) in addition to IV. V was characterized by X-ray diffraction analysis: space group P1l, a = 10.432 (3) Å, b = 12.727 (6) Å, c = 14.448 (4) Å, α = 98.46 (3)°, β = 93.82°, γ = 91.82 (3)°, Z = 2, ρcalcd = 2.47 g/cm3. The structure of V was solved by the heavy-atom method and was refined to the final residuals RF = 0.037 and RwF = 0.042. V consists of a tetrahedral cluster of one platinum and three osmium atoms and has a triply bridging sulfido ligand on the triosmium face. The phenyl ring of one of the PMe2Ph ligands is orthometalated on a metal atom adjacent to the primary coordination site. © 1984 American Chemical Society.-
dc.languageeng-
dc.relation.ispartofInorganic Chemistry-
dc.titleCluster synthesis. 7. Role of bridging sulfido ligands in the synthesis of platinum osmium carbonyl cluster compounds-
dc.typeArticle-
dc.description.natureLink_to_subscribed_fulltext-
dc.identifier.scopuseid_2-s2.0-0346650246-
dc.identifier.volume23-
dc.identifier.issue26-
dc.identifier.spage4723-
dc.identifier.epage4732-

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