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Issue 12, 2002
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Reactions of tetrathiotungstate and tetrathiomolybdate with substituted haloalkanes

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Abstract

Reactions of [PPh4]2[WS4] in CH3CN with excess n-hexylbromide, 1,4-dichlorobutane, 2-(bromomethyl)tetrahydro-2H-pyran) (bmthp), and 2-(bromoethyl)-1,3-dioxane (bedo) followed by extraction with THF afforded a series of alkylthiolatotrithiotungstate complexes, [PPh4][(RS)WS3] (1: R = n-hexyl; 2: R = ClCH2CH2CH2CH2; 3: R = mthp; 4: R = edo), and the analogous reactions of [PPh4]2[MoS4] in CH3CN–THF with excess bmthp and bedo also generated [PPh4][(RS)MoS3] (5: R = mthp; 6: R = edo), albeit in low yields. Treatment of [PPh4]2[WS4] in CH3CN with excess (S)-(+)-3-bromo-2-methyl-1-propanol turned out to give a trinuclear, [PPh4]2[W3S8((S)-(+)-OCH2CH(Me)CH2Br)2] (7). Compounds 1–7 were characterized spectroscopically and the crystal structures of 2–7 were determined by X-ray analysis. All the mononuclear complexes 2–6 assume tetrahedral structures, being coordinated by one thiolate sulfur and three terminal sulfido ligands, and no additional coordination was observed by the O-donor portions of mthp or edo. The structure of 7 consists of a linear W3 spine and two (S)-(+)-OCH2CH(Me)CH2Br ligands are coordinated at the central W atom.

Graphical abstract: Reactions of tetrathiotungstate and tetrathiomolybdate with substituted haloalkanes

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Publication details

The article was received on 23 Jul 2001, accepted on 23 Apr 2002 and first published on 16 May 2002


Article type: Paper
DOI: 10.1039/B106572F
Citation: J. Chem. Soc., Dalton Trans., 2002,0, 2573-2580
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    Reactions of tetrathiotungstate and tetrathiomolybdate with substituted haloalkanes

    J. Lang, H. Kawaguchi and K. Tatsumi, J. Chem. Soc., Dalton Trans., 2002, 0, 2573
    DOI: 10.1039/B106572F

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