Abstract
The reaction of Ru 5(CO) 15(μ 4-S) with HC 2Ph at 68°C has resulted in the formation of the complex Ru 5(CO) 13(μ-CO)(μ 4-η 2-HC 2Ph)(μ 4-S), 1 in 60% yield. Compound 1 was found to react with Ru(CO) 5 at 80°C to yield the enlarged cluster Ru 6(CO) 17(μ 4-η 2-HC 2Ph)(μ 4-S), 2 in 53% yield. Compound 2 was characterized structurally. Crystal data : Ru 6SO 17C 25H 6, M = 1216.80, monoclinic, P2 1/ c (No. 14), a = 11.050(2), b = 22.503(5), c = 29.26(1) Å, β = 90.80(3)°, V = 7276(4) Å 3, D c = 2.27 g cm −3, Z = 8, λ(Mo- K α ) = 0.71073 Å (graphite monochromator) μ = 24.9 cm −1. Methods: MITHRIL difference Fourier, full-matrix least-squares. Refinement of 4647 reflections ( F 2 ⩾ 3σ( F 2)), (1° < 2θ < 42°), gave R and R w values of 0.049 and 0.048, respectively. Data/parameters ratio = 9.54, highest peak in final difference Fourier = 0.79 e Å −3. The molecule consists of a distorted square of four ruthenium atoms that contains a quadruply bridging sulphido ligand on one side of the cluster and a quadruply bridging alkyne ligand on the other side. Ru(CO) 4 groups bridge adjacent edges of the cluster. The Ru(CO) 4 groups can be cleaved off sequentially by treatment with CO at 80°C/1 atm.
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