d1 Oxosulfido-Mo(V) Compounds: First Isolation and Unambiguous Characterization of an Extended Series

CJ Doonan; C Gourlay; DJ Nielsen; VWL Ng; PD Smith; DJ Evans; GN George; JM White; CG Young

Journal article

d1 Oxosulfido-Mo(V) Compounds: First Isolation and Unambiguous Characterization of an Extended Series

CJ Doonan, C Gourlay, DJ Nielsen, VWL Ng, PD Smith, DJ Evans, GN George, JM White, CG Young

Inorganic Chemistry | Published : 2015

DOI: 10.1021/acs.inorgchem.5b00708

Abstract

Reaction of TpiPrMoVIOS(OAr) with cobaltocene in toluene results in the precipitation of brown, microcrystalline oxosulfido-Mo(V) compounds, [CoCp2][TpiPrMoVOS(OAr)] (Cp- = η5-C5H5-, TpiPr- = hydrotris(3-isopropylpyrazol-1-yl)borate, OAr- = phenolate or 2-sBu, 2-tBu, 3-tBu, 4-sBu, 4-Ph, 3,5-sBu2, 2-CO2Me, 2-CO2Et or 2-CO2Ph derivative thereof). The compounds are air- and water-sensitive and display ν(Mo=O) and ν(Mo-S) IR absorption bands at ca. 890 and 435 cm-1, respectively, 20-40 cm-1 lower in energy than the corresponding bands in TpiPrMoOS(OAr). They are electrochemically active and exhibit three reversible cyclovoltammetric waves (E(MoVI/MoV) = -0.40 to -0.66 V, E([CoCp2]+/CoCp2) = -0.9..

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University of Melbourne Researchers

Jonathan White Author

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Funding Acknowledgements

We thank Ms. N. Newey, Drs. H. H. Harris and S. Z. Knottenbelt, and Prof. M. L. Kirk for experimental assistance or helpful discussions. We gratefully acknowledge the financial support of the Albert Shimmins Memorial Fund, the Australian Nuclear Science and Technology Organization, the Australian Research Council, and the Petroleum Research Council (administered by the American Chemical Society). Portions of this research were performed at the SSRL, a Directorate of SLAC National Accelerator Laboratory, and the Office of Science User Facility operated for the U.S. Department of Energy Office of Science by Stanford University. SSRL is funded by the Department of Energy (DOE) BES, with further support by DOE OBER and the National Institutes of Health.