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Reactivity of tetrathiometalates with alkynes. Synthesis and characterisation of dithiolene complexes of Mo, W, and V by ESMS and XRD

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Abstract

The reaction of DMA (C2(CO2Me)2) with MoS 2−4 , WS 2−4 , and VS 3−4 led to six dithiolene compounds. (NEt4)2[Mo2(X)2(μ-S) 2(η2-S2C2(CO2Me)2)2] 1, (X = O or S), (NEt4)2[V(η2-S2C2(CO2Me)2)3] 2a, (NEt4)2[V(O)(η2-S2C2(CO2Me)2)2] 2b, (NEt4)2[W2(S)2(μ-S)2(η2-S2C2(CO2Me)2)2] 3, (NEt4)2[W(O)(η2-S2C2(CO2Me)2)2] 4 and (NEt4)2[W2(μ-S)2(η2 -S2C2(CO2Me)2)4] 5 were isolated in the solid state. The structures of 2a, 3, 4 and 5 were determined by single crystal X-ray diffraction study. The compounds 1 and 2b were characterised in solution by ESMS (Electrospray Mass Spectrometry) and in the solid state by IR spectroscopy. ESMS data also allowed proposal of a reaction scheme which rationalizes the formation of the different species present in solution.

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Authors and Affiliations

  1. Institut Lavoisier de Versailles, UMR CNRS 8180, Université de Versailles-St-Quentin, 45, avenue des Etats-Unis, Versailles, 78035, France

    Alain Mallard, Corine Simonnet-Jégat, Jérôme Marrot & Francis Sécheresse

  2. Laboratoire de Spectrométrie de Masse Bioorganique, UMR CNRS 6014, Université de Rouen, Mont St Aignan, 76821, France

    Hélène Lavanant

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  1. Alain Mallard
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  2. Corine Simonnet-Jégat
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  3. Hélène Lavanant
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  4. Jérôme Marrot
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  5. Francis Sécheresse
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Correspondence to Corine Simonnet-Jégat.

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Mallard, A., Simonnet-Jégat, C., Lavanant, H. et al. Reactivity of tetrathiometalates with alkynes. Synthesis and characterisation of dithiolene complexes of Mo, W, and V by ESMS and XRD. Transition Met Chem 33, 143–152 (2008). https://doi.org/10.1007/s11243-007-9005-3

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  • DOI: https://doi.org/10.1007/s11243-007-9005-3

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