Syntheses and x-ray crystal structures of [MoO(SCH2CH2-CH2S)2]- and [Mo2O2(μ-N3)(SCH2CH2CH2S)3]-. A study of the redox behaviour of [MoO(SCH2CH2S)2]- by cyclic voltammetry using convolution analysis

Peter T. Bishop, Jonathan R. Dilworth, John P. Hutchinson, Jon A. Zubieta

Research output: Contribution to journalArticle

6 Scopus citations

Abstract

The complexes [PPh4][MoO{S(CH2)nS}2], n=2 (1) n=3 (3), were synthesised from the MoVI dioxoprecursor complex [MoO2(butane-2,3-diolato)2] and the appropriate thiol in the presence of base. Complex (3) exhibits a square pyramidal geometry. Crystal Data: P21,0, Z=4, a=9.612(2), b=21.202(4), c=15.462(3) Å, β=103.06(1)°, V=3043.3Å3, F(000)=1364.0, 3687 reflections collected, and 1957 used in solution with R=0.058. [MoO(SCH2CH2CH2S)2]- reacts with hydrazoic acid in methanol to produce [Mo2O2(μ-N3)-(SCH2CH2CH2S)3] (5), crystal data: {Mathematical expression}a=9.398(3), b=14.650(2), c=27.42(2) (Å), α=β=γ=90°, Z=4 V=3775.8Å3, F(000)=1872.0, 2563 reflections collected and 1244 were used in the solution with R=0.058. The complex is an asymmetric dimer with a triple bridge comprising two dithiolate sulphurs and a nitrogen of the azide ligand. Convolution analysis of the cyclic voltammetric response of complex (1) confirmed a diffusion controlled one electron reversible reduction process.

Original languageEnglish (US)
Pages (from-to)177-182
Number of pages6
JournalTransition Metal Chemistry
Volume15
Issue number3
DOIs
StatePublished - Jun 1990

ASJC Scopus subject areas

  • Inorganic Chemistry
  • Metals and Alloys
  • Materials Chemistry

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