Direct synthesis from MoCl3(THF)3 of a complex containing the [Mo3S4]4+ core |
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| Affiliation: | 1. University of Patras, Department of Chemistry, GR-26504 Patras, Greece;2. Hellenic Open University, School of Science and Technology, GR-26222 Patras, Greece;3. Foundation for Research and Technology Hellas—Institute of Chemical Engineering Sciences (FORTH/ICE-HT), GR-26504 Rio, Patras, Greece;4. Institute of Catalysis and Petrochemistry, CSIC, Marie Curie 2, 28049 Madrid, Spain;1. Department of Physics, Virginia Commonwealth University, Richmond, VA 23284, United States;2. H.E.J. Research Institute of Chemistry, University of Karachi, Karachi 75270, Pakistan;3. Department of Surgery, Virginia Commonwealth University, School of Medicine, Richmond, VA 23298, United States;4. National Institute of Standards and Technology, Materials Measurement Science Division, Gaithersburg, MD 20899-8520, United States;1. Faculty of Chemistry, Jagiellonian University, Gronostajowa 2, 30-387 Kraków, Poland;2. Department of Molecular Biophysics, Faculty of Biochemistry, Biophysics and Biotechnology, Jagiellonian University, Gronostajowa 7, 30-387 Kraków, Poland;3. Department of Chemistry, Michigan State University, 578 South Shaw Lane, East Lansing, MI 48824, USA;1. Muhlenberg College, 2400 Chew St., Allentown, PA 18104, USA;2. Colgate University, 13 Oak Dr., Hamilton, NY 13346, USA;3. Bucknell University, 701 Moore Ave, Lewisburg, PA 17837, USA;4. The College of William and Mary, 200 Stadium Dr., Williamsburg, VA 23186, USA;5. The University of Virginia, Charlottesville, VA 22904, USA;2. Dipartimento di Fisica, Università degli Studi di Cagliari, and Istituto Officina dei Materiali (CNR-IOM), UOS Cagliari, Cittadella Universitaria di Monserrato, S.P. Monserrato-Sestu, Km. 0.700, 09042 Monserrato (CA), Italy |
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| Abstract: | By reaction of MoCl3(THF)3 with NaSH in tetrahydrofuran, followed by addition of Me2PCH2CH2PMe2(dmpe), then chromatography on silica-gel, and finally addition of NH4PF6, the compound [Mo3S4Cl3(dmpe)3]PF6·CH3OH was prepared in moderate yield. X-ray crystallography showed the presence of a chiral cation based on a Mo3S4 core with chelating dmpe units arranged like the blades of a ship's screw. The three Cl atoms fill the remaining octahedral sites on each metal atom. The compound crystallizes in space group R3c with (hexagonal) cell dimensions of a = 15.310(7) Å, c = 30.640(3) Å and Z = 6. The [Mo3S4Cl3(dmpe)3]+ ion and the PF6− ion each have crystallographic C3 symmetry. The principal distances and theirs esds are: MoMo, 2.766(4) Å; Mo(μ3-S), 2.360(9) Å; Mo(μ2-S), 2.290(7) Å, 2.336(7) Å; MoP, 2.534(8) Å, 2.605(8) Å; MoCl, 2.473(7) Å; PF, 1.56(2) Å, 1.64(3) Å. The correct enantiomer was obtained by refining both to convergence, which give R = 0.059 and R = 0.064. |
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