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Microwave Promoted Oxidative Addition Reactions of Os3(CO)12: Efficient Syntheses of Triosmium Clusters of the Type Os3(μ-X)2(CO)10 and Os3(μ-H)(μ-OR)(CO)10

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Abstract

Microwave heating allows for the high-yield, one-step synthesis of the known triosmium complexes Os3(μ-Br)2(CO)10 (1), Os3(μ-I)2(CO)10 (2), and Os3(μ-H)(μ-OR)(CO)10 with R = methyl (3), ethyl (4), isopropyl (5), n-butyl (6), and phenyl (7). In addition, the new clusters Os3(μ-H)(μ-OR)(CO)10 with R = n-propyl (8), sec-butyl (9), isobutyl (10), and tert-butyl (11) are synthesized in a microwave reactor. The preparation of these complexes is easily accomplished without the need to first prepare an activated derivative of Os3(CO)12, and without the need to exclude air from the reaction vessel. The syntheses of complexes 1 and 2 are carried out in less than 15 min by heating stoichiometric mixtures of Os3(CO)12 and the appropriate halogen in cyclohexane. Clusters 3–6 and 8–10 are prepared by the microwave irradiation of Os3(CO)12 in neat alcohols, while clusters 7 and 11 are prepared from mixtures of Os3(CO)12, alcohol and 1,2-dichlorobenzene. Structural characterization of clusters 2, 4, and 5 was carried out by X-ray crystallographic analysis. High resolution X-ray crystal structures of two other oxidative addition products, Os3(CO)12I2 (12) and Os3(μ-H)(μ-O2CC6H5)(CO)10 (13), are also presented.

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Acknowledgments

We gratefully acknowledge the financial support of The Welch Foundation (Grant R-0021).

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Authors and Affiliations

  1. Department of Chemistry & Biochemistry, Abilene Christian University, ACU Box 28132, Abilene, TX, 79699, USA

    Kayla J. Pyper, David K. Kempe, Jade Y. Jung, Li-Hsing J. Loh, Nigel Gwini, Benjamin D. Lang, Brittney S. Newton, Jonathan M. Sims & Gregory L. Powell

  2. Department of Chemistry, University of North Texas, Denton, TX, 76203, USA

    Vladimir N. Nesterov

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  1. Kayla J. Pyper
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  2. David K. Kempe
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Pyper, K.J., Kempe, D.K., Jung, J.Y. et al. Microwave Promoted Oxidative Addition Reactions of Os3(CO)12: Efficient Syntheses of Triosmium Clusters of the Type Os3(μ-X)2(CO)10 and Os3(μ-H)(μ-OR)(CO)10 . J Clust Sci 24, 619–634 (2013). https://doi.org/10.1007/s10876-012-0532-5

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  • DOI: https://doi.org/10.1007/s10876-012-0532-5

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