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Acetylene substitution in the triruthenium clusters Ru3 (CO)12-n(MeCN)n (where n = 0, 2). X-ray diffraction structures for Ru3(CO)9(μ2-H)(μ3-η2-C≡CC6H4Me-4) and Ru4(CO)12(μ4-η2-HC≡CPh)

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Abstract

The clusters Ru3(CO)12 (1) and Ru3(CO)10 (MeCN)2 (2) react with added phenylacetylene and p-tolylacetylene to give the tri- and tetraruthenium ruthenium clusters Ru3(CO)9-(μ2-H)(μ3-η2-HC≡CAr) and Ru4(CO)12(μ4-η2-HC≡CAr) (where Ar = Ph, C6H4Me-4). The two new clusters derived from the p-tolylacetylene ligand have been isolated and characterized in solution by IR and 1H NMR spectroscopy, and the solid-state structures for Ru4(CO)12(μ4-η2-HC≡CPh) (4) and Ru3(CO)9(μ2-H)(μ3-η2-C≡CC6H4Me-4) (5) have been determined by X-ray diffraction analysis. Ru4(C)12(μ4-η2-HC≡CPh) (4) crystallizes in the monoclinic space group P21/n, a = 20.135(1) Å, b = 9.330(1) Å, c = 26.186(2) Å, β = 97.419(6) °, V = 4878.1(1) Å3, Z = 8, dcalc = 2.294 g·cm-3; R = 0.0278, Rw = 0.0364 for 4967 observed reflections with I > 3σ(I). Ru3(CO)9(μ2-H)(μ3-η2-C≡CC6-Me-4) (5) crystallizes in the monoclinic space group P21/c, a = 8.6825(7) Å, b = 12.8409(7) Å, c = 19.213(1) Å, β = 90.001(6) °, V = 2142.1(3) Å3, Z = 4, dcalc = 2.082 g·cm-3; R = 0.0264, Rw = 0.0337 for 2241 observed reflections with I > 3σ(I). The X-ray data confirm the expected closo polyhedral cores for both clusters 4 and 5.

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Acknowledgment

We are grateful for financial support from the Robert A. Welch Foundation (Grants B-1202-SGB and B-1039-MGR) and the UNT Faculty Research Program.

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  1. Center for Organometallic Research and Education, Department of Chemistry, University of North Texas, Denton, Texas, 76203, USA

    Huafeng Shen, Simon G. Bott & Michael G. Richmond

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  1. Huafeng Shen
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  2. Simon G. Bott
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  3. Michael G. Richmond
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Shen, H., Bott, S.G. & Richmond, M.G. Acetylene substitution in the triruthenium clusters Ru3 (CO)12-n(MeCN)n (where n = 0, 2). X-ray diffraction structures for Ru3(CO)9(μ2-H)(μ3-η2-C≡CC6H4Me-4) and Ru4(CO)12(μ4-η2-HC≡CPh). J Chem Crystallogr 27, 25–33 (1997). https://doi.org/10.1007/BF03543084

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