Abstract
Abstract Ru3(CO)12 reacts with di-tert-butylphosphine and acetic acid in di-n-butylether under reflux to form bis[μ-acetatodicarbonyl(di-tert-butylphosphine)ruthenium (1)] (1) in 80% yield. The crystal structure of 1 has been determined by single crystal X-ray diffraction methods. Crystal data for 1: C24H42O8P2Ru2, M = 722.7, orthorhombic, space group Pbca, a = 12.955 (2), b = 17.347 (2), c = 28.638 (4) Å, U = 6435.8 (5) Å3, Dc = 1.492 gcm−3, λ(Mo Kα) = 0.71073 Å, graphite monochromator, μ = 10.56 cm−1. Methods: MULTAN, difference Fourier, full-matrix least-squares. Refinement of 2298 reflections (I<3σ(I) out of 6288 unique observed (3° >20 >50°) gave R and Rw values of 0.050 and 0.057, respectively. All non-hydrogen atoms were refined with anisotropic thermal parameters. Hydrogen atoms were not located. Data/parameter ratio = 7.07, shift to error ratio = 0.38, highest peak in the final difference Fourier = 0.70 Å−3. Data were collected on an Enraf-Nonius CAD-4 diffractometer at 23 ± 2° C. The complex has a Ru-Ru bond of 2.735 (1) Å which is bridged by two cis acetate groups. The CO groups also occupy cis locations on each Ru, while the two t-Bu2PH ligands occupy axial positions trans to the metal-metal bond. The coordination geometry about each Ru atom is roughly octahedral. The overall geometry of the molecule can be described as that of a “sawhorse-like” structure.
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