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Structural characterization of MoOCl3(THF)2, the pre-reagent for Kauffmann olefination reactions

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Abstract

Single crystals of molybdenum-oxy-di-tetrahydrofuran-trichloride were obtained by the reaction of Mo2Cl10, tetrahydrofuran, sulfur, and P4S3 in carbon disulfide after layering the solution with n-hexane. Single crystal structure determination at T = 123 K reveals that MoOCl3(THF)2 crystalizes in the orthorhombic space group P212121 with the lattice constants a = 7.8620(9) Å, b = 12.302(1) Å, c = 14.043(2) Å, V = 1304.10(3) Å3, and Z = 4. EPR experiments on the solid compound showed a g value of 1.94 at 347.46 mT, which accords to a Mo(V) species. The electronic structure of the title compound was investigated with DFT methods.

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Authors and Affiliations

  1. Institut für Anorganische Chemie, Universität Regensburg, Regensburg, Germany

    Christoph Vitzthumecker, Fred Robinson & Arno Pfitzner

  2. Institute of Chemistry, University of Bath, Bath, UK

    Fred Robinson

Authors
  1. Christoph Vitzthumecker
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  2. Fred Robinson
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  3. Arno Pfitzner
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Correspondence to Arno Pfitzner.

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Vitzthumecker, C., Robinson, F. & Pfitzner, A. Structural characterization of MoOCl3(THF)2, the pre-reagent for Kauffmann olefination reactions. Monatsh Chem 148, 629–633 (2017). https://doi.org/10.1007/s00706-016-1881-9

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  • DOI: https://doi.org/10.1007/s00706-016-1881-9

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