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Issue 8, 1982
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Reactions of CS2 with metal cluster carbonyls of the iron triad: reaction of [Os6(CO)18] and X-ray crystal structure of [Os4(CO)12(CS)S]

Abstract

The reaction of [Os6(CO)18] with excess CS2 in heptane at 165 °C under CO pressure gives the known compounds [Os3(CO)8(CS)S2](1) and [Os3(CO)9S2](2), and also [Os4(CO)12(CS)S](3). A single crystal X-ray diffraction study shows that in (3) the four Os atoms adopt a ‘butterfly’ configuration, but with an Os ⋯ Os separation of 3.598(2)Å across the ‘backbone’, which is non-bonding. Three of the Os atoms are capped by a µ3-S ligand, while a CS ligand, which acts as a four-electron donor, lies on the other side of the metal framework. The carbon atom of this ligand is co-ordinated to all four metal atoms but the sulphur atom is only co-ordinated to one. The molecule (3) crystallises in space group P[1 with combining macron] with a = 14.834(6), b= l0.048(5), c= 7.682(5)Å, α= 108.84(3), β= 92.99(3), γ= 95.64(3)° and Z= 2. The structure was solved by a combination of direct methods and Fourier difference techniques, and refined by blocked-cascade least squares to R= 0.058 for 3 249 observed diffractometer data.

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Article type: Paper
DOI: 10.1039/DT9820001641
Citation: J. Chem. Soc., Dalton Trans., 1982,0, 1641-1644
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    Reactions of CS2 with metal cluster carbonyls of the iron triad: reaction of [Os6(CO)18] and X-ray crystal structure of [Os4(CO)12(CS)S]

    P. V. Broadhurst, B. F. G. Johnson, J. Lewis and P. R. Raithby, J. Chem. Soc., Dalton Trans., 1982, 0, 1641
    DOI: 10.1039/DT9820001641

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