Cyclopentadienyl-ruthenium and -osmium chemistry. Part 11. Reactions and structures of [RuCl(PPh3)2(η-C5H5)] and its trimethyl-phosphine analogue

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Abstract
The crystal structure of the title compound has been determined by single-crystal X-ray diffraction at 295 K and refined by least squares to a residual of 0.036 for 7 290 ‘observed’ reflections. Crystals are triclinic, space group P, with a= 14.493(8), b= 11.315(4), c= 11.745(4)Å, α= 69.99(3), β= 84.67(4), γ= 62.27(3)°, and Z= 2. The ruthenium environment is pseudo-tetrahedral, Ru–Cl 2.453(2), Ru–P 2.337(1), 2.335(1), 2.207Å. The phenyl ring environments are highly crowded and the nature of the steric interactions between them is examined. The structure of the trimethylphosphine analogue [RuCl(PMe3)2(C5H5)] has also been determined, 1 805 ‘observed’ reflections being refined to a residual of 0.059. Crystals are orthorhombic, space group Pbca, with a= 29.251(8), b= 14.703(4), c= 14.649(7)Å, and Z= 16. The two ruthenium environments are similar to that of the triphenylphosphine analogue. The Ru–Cl distances are 2.451 (6), 2.440(5), and Ru–P 2.273(5)–2.280(6)Å. The value of is 2.20 Å. The syntheses and properties of [RuCl(PMe3)2(η-C5H5)] and of the cationic derivatives [RuL(PMe3)2(η-C5H5)]+(L = MeCN, CO, CNBut, or PMe3) are also described.

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