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      Further studies on the chemistry of molybdenyl adducts of [Pt₂(μ-S)₂(PPh₃)₄]: Hydrolysis, condensation and ligand exchange processes

      Henderson, William; Nicholson, Brian K.; Bridson, James Hadley; Kueh, Jui Thiang
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      Molybdenum manuscript final bl.pdf
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      DOI
       10.1016/j.ica.2011.04.050
      Link
       www.sciencedirect.com
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      Henderson, W., Nicholson, B.K., Bridson, J.H. & Kueh, J.T. (2011). Further studies on the chemistry of molybdenyl adducts of [Pt₂(μ-S)₂(PPh₃)₄]: Hydrolysis, condensation and ligand exchange processes. Inorganica Chimica Acta, available online 7 May 2011.
      Permanent Research Commons link: https://hdl.handle.net/10289/5468
      Abstract
      Reaction of [Pt₂(μ-S)₂(PPh₃)₄] with [MoO₂(acac)₂] in methanol gives the known five-coordinate Mo(VI) adduct [Pt₂(μ-S)₂(PPh₃)₄MoO₂(OMe)]⁺ isolated as its PF₆⁻, BPh₄⁻ and [Mo₈O₂₆]₄⁻ salts; the latter was structurally characterised, the polymolybdate anion being the uncommon γ form. Hydrolysis of [Pt₂(μ-S)₂(PPh₃)₄MoO₂(OMe)]⁺ in wet dichloromethane initially produces [Pt₂(μ-S)₂(PPh₃)₄MoO₂(OH)]⁺ and subsequently the bright yellow oxo-bridged dimolybdenum species [{Pt₂(μ-S)₂(PPh₃)₄MoO₂}₂O]₂⁺, structurally characterised as its tetraphenylborate salt, and found to contain two five-coordinate molybdenum centres. [{Pt₂(μ-S)₂(PPh₃)₄MoO₂}₂O]₂⁺ can be prepared directly from [Pt₂(μ-S)₂(PPh₃)₄] and [MoO₂(acac)₂] in wet MeCN. Slow reconversion to [Pt₂(μ-S)₂(PPh₃)₄MoO₂(OMe)]⁺ occurs when [{Pt₂(μ-S)₂(PPh₃)₄MoO₂}₂O]₂⁺ is dissolved in methanol. [Pt₂(μ-S)₂(PPh₃)₄MoO₂(OMe)]⁺ undergoes alkoxide exchange in dichloromethane-alcohol solutions to give [Pt₂(μ-S)₂(PPh₃)₄MoO₂(OR)]⁺ species (R = e.g. n-octyl). These reactions are easily monitored using electrospray ionisation mass spectrometry.
      Date
      2011
      Type
      Journal Article
      Publisher
      Elsevier
      Rights
      This is an author’s accepted version of an article published in the journal: Inorganica Chimica Acta. © 2011 Elsevier.
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      • Science and Engineering Papers [3069]
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