Synthesis and characterisation of the platinum group mixed metal clusters [Os3M(μ-H)3(CO)12] (M = Rh, Ir); X-ray crystal structure of [Os3Rh(μ-H)3(CO)12]

Peter Sundberg; Bertil Norén; Brian F. G. Johnson; Jack Lewis; Paul R. Raithby

doi:10.1016/0022-328X(88)80326-7

Synthesis and characterisation of the platinum group mixed metal clusters [Os₃M(μ-H)₃(CO)₁₂] (M = Rh, Ir); X-ray crystal structure of [Os₃Rh(μ-H)₃(CO)₁₂]

Peter Sundberg, Bertil Norén, Brian F. G. Johnson, Jack Lewis, Paul R. Raithby

Research output: Contribution to journal › Article › peer-review

Abstract

The mixed-metal cluster [Os₃Rh(μ-H)₃(CO)₁₂] (1) has been prepared in 60% yield by the reaction of the reaction of the co-ordinatively unsaturated cluster [Os₃(μ-H)₂(CO)₁₂] with the dimer [Rh(CO)₂Cl)₂]. The analogous iridium complex [Os₃Ir(μ-H)₃(CO)₁₂] (2) is best prepared by the reaction of the anion [Os₃H(CO)₁₁]^- with the labile cyclooctadiene complex [(Ir(cod)Cl)₂], and is obtained in 40% yield. Both complexes 1 and 2 have been characterized by IR, ¹H NMR, and ESCA (Electron Spectroscopy for Chemical Analysis) spectroscopic techniques, and the structure of 1 has been confirmed by a single crystal X-ray analysis, which shows it to be isostructural with the known cobalt analogue [Os₃Co(μ-H)₃(CO)₁₂]. Complex 1 crystallises in the triclinic space group p1, with a 8.288(2), b 9.185(2), c 13.655(2) Å, α 82.26(2), β 80.10(1), γ 68.9191)°, Z = 2; 2897 observed data with F> 5σ(F) were refined by blocked-cascade least squares to R = 0.055 and R_w = 0.058.

Original language	English
Pages (from-to)	383-391
Number of pages	9
Journal	Journal of Organometallic Chemistry
Volume	353
Issue number	3
DOIs	https://doi.org/10.1016/0022-328X(88)80326-7
Publication status	Published - 4 Oct 1988

ASJC Scopus subject areas

Biochemistry
Physical and Theoretical Chemistry
Organic Chemistry
Inorganic Chemistry
Materials Chemistry

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10.1016/0022-328X(88)80326-7

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@article{242beaaac01a483b8fd2df5a0cd5cfc2,

title = "Synthesis and characterisation of the platinum group mixed metal clusters [Os3M(μ-H)3(CO)12] (M = Rh, Ir); X-ray crystal structure of [Os3Rh(μ-H)3(CO)12]",

abstract = "The mixed-metal cluster [Os3Rh(μ-H)3(CO)12] (1) has been prepared in 60% yield by the reaction of the reaction of the co-ordinatively unsaturated cluster [Os3(μ-H)2(CO)12] with the dimer [Rh(CO)2Cl)2]. The analogous iridium complex [Os3Ir(μ-H)3(CO)12] (2) is best prepared by the reaction of the anion [Os3H(CO)11]- with the labile cyclooctadiene complex [(Ir(cod)Cl)2], and is obtained in 40% yield. Both complexes 1 and 2 have been characterized by IR, 1H NMR, and ESCA (Electron Spectroscopy for Chemical Analysis) spectroscopic techniques, and the structure of 1 has been confirmed by a single crystal X-ray analysis, which shows it to be isostructural with the known cobalt analogue [Os3Co(μ-H)3(CO)12]. Complex 1 crystallises in the triclinic space group p1, with a 8.288(2), b 9.185(2), c 13.655(2) {\AA}, α 82.26(2), β 80.10(1), γ 68.9191)°, Z = 2; 2897 observed data with F> 5σ(F) were refined by blocked-cascade least squares to R = 0.055 and Rw = 0.058.",

author = "Peter Sundberg and Bertil Nor{\'e}n and Johnson, {Brian F. G.} and Jack Lewis and Raithby, {Paul R.}",

year = "1988",

month = oct,

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doi = "10.1016/0022-328X(88)80326-7",

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journal = "Journal of Organometallic Chemistry",

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T1 - Synthesis and characterisation of the platinum group mixed metal clusters [Os3M(μ-H)3(CO)12] (M = Rh, Ir); X-ray crystal structure of [Os3Rh(μ-H)3(CO)12]

AU - Sundberg, Peter

AU - Norén, Bertil

AU - Johnson, Brian F. G.

AU - Lewis, Jack

AU - Raithby, Paul R.

PY - 1988/10/4

Y1 - 1988/10/4

N2 - The mixed-metal cluster [Os3Rh(μ-H)3(CO)12] (1) has been prepared in 60% yield by the reaction of the reaction of the co-ordinatively unsaturated cluster [Os3(μ-H)2(CO)12] with the dimer [Rh(CO)2Cl)2]. The analogous iridium complex [Os3Ir(μ-H)3(CO)12] (2) is best prepared by the reaction of the anion [Os3H(CO)11]- with the labile cyclooctadiene complex [(Ir(cod)Cl)2], and is obtained in 40% yield. Both complexes 1 and 2 have been characterized by IR, 1H NMR, and ESCA (Electron Spectroscopy for Chemical Analysis) spectroscopic techniques, and the structure of 1 has been confirmed by a single crystal X-ray analysis, which shows it to be isostructural with the known cobalt analogue [Os3Co(μ-H)3(CO)12]. Complex 1 crystallises in the triclinic space group p1, with a 8.288(2), b 9.185(2), c 13.655(2) Å, α 82.26(2), β 80.10(1), γ 68.9191)°, Z = 2; 2897 observed data with F> 5σ(F) were refined by blocked-cascade least squares to R = 0.055 and Rw = 0.058.

AB - The mixed-metal cluster [Os3Rh(μ-H)3(CO)12] (1) has been prepared in 60% yield by the reaction of the reaction of the co-ordinatively unsaturated cluster [Os3(μ-H)2(CO)12] with the dimer [Rh(CO)2Cl)2]. The analogous iridium complex [Os3Ir(μ-H)3(CO)12] (2) is best prepared by the reaction of the anion [Os3H(CO)11]- with the labile cyclooctadiene complex [(Ir(cod)Cl)2], and is obtained in 40% yield. Both complexes 1 and 2 have been characterized by IR, 1H NMR, and ESCA (Electron Spectroscopy for Chemical Analysis) spectroscopic techniques, and the structure of 1 has been confirmed by a single crystal X-ray analysis, which shows it to be isostructural with the known cobalt analogue [Os3Co(μ-H)3(CO)12]. Complex 1 crystallises in the triclinic space group p1, with a 8.288(2), b 9.185(2), c 13.655(2) Å, α 82.26(2), β 80.10(1), γ 68.9191)°, Z = 2; 2897 observed data with F> 5σ(F) were refined by blocked-cascade least squares to R = 0.055 and Rw = 0.058.

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Synthesis and characterisation of the platinum group mixed metal clusters [Os₃M(μ-H)₃(CO)₁₂] (M = Rh, Ir); X-ray crystal structure of [Os₃Rh(μ-H)₃(CO)₁₂]

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