Synthesis and spectroscopic characterisation of closo-Ru4(CO)1242-HC2Ph) and closo-Ru4(CO)9(μ-CO)242-HC2Ph) (μ4-Se). Crystal structure of closo-Ru4(CO) 1242-HC2Ph)

Mathur, Pradeep ; Ghosh, Sundargopal ; Munkir Hossain, Md. ; Satyanarayana, C. V. V. ; Rheingold, Arnold L. ; Yap, Glenn P. A. (1997) Synthesis and spectroscopic characterisation of closo-Ru4(CO)1242-HC2Ph) and closo-Ru4(CO)9(μ-CO)242-HC2Ph) (μ4-Se). Crystal structure of closo-Ru4(CO) 1242-HC2Ph) Journal of Organometallic Chemistry, 538 (1-2). pp. 57-61. ISSN 0022-328X

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Official URL: http://linkinghub.elsevier.com/retrieve/pii/S00223...

Related URL: http://dx.doi.org/10.1016/S0022-328X(96)06900-8

Abstract

Reaction of the chalcogen stabilised butterfly cluster Fe2(CO)6μ-SeC(H)=C(Ph)Se with Ru3(CO)12occurs under thermal conditions affording the clusters FeRu2(CO)9(μ-Se)2 (2), closo-Ru4(CO)1242-HC2Ph) (3) and closo-Ru4(CO)9(μ-CO)242-HC2Ph)(μ4-Se) (4) in 30%, 22% and 18% yield respectively. They were characterised by IR and 1H, 13C and 77Se NMR spectroscopy. Compound 3 was further characterised by X-ray methods: space group P21/n, a = 20.138(4), b = 9.333(2), c = 26.219(6) Å, β = 97.43(2)°, Z = 8, ρcalc = 2.291 g cm-3. The structure was solved using direct methods and was refined to the final values of the residuals R = 0.0377 and Rw = 0.0455. The molecule consists of a butterfly arrangement of four ruthenium atoms with a quadruply bridged alkyne ligand. Compound 4 was characterised by comparison of its spectroscopic data with that of the analogous S-compound.

Item Type:Article
Source:Copyright of this article belongs to Elsevier Science.
Keywords:Ruthenium; Selenium; Alkyne; Carbonyl; Cluster; X-ray Diffraction
ID Code:24833
Deposited On:30 Nov 2010 09:27
Last Modified:30 Nov 2010 09:27

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