Oxidation of [Li4{(NBut)3S}2]: a new route to sulfur triimides ‡

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Abstract
The oxidation reactions of [Li4{(NBut)3S}2] with oxygen and halogens (bromine and iodine) were investigated. In all these reactions a radical intermediate [Li3{(NBut)3S}2]˙ was observed, which was investigated by ESR spectroscopy. While the reaction with oxygen leads to the dianionic sulfur(VI) species [Li2(NBut)3SO], oxidation with halogens yields N,N′,N″-tris(tert-butyl)sulfur triimide S(NBut)3. The latter reaction provides an easy access to sulfur triimides. Some intermediates from the reaction of [Li4{(NBut)3S}2] with halogens could be isolated and characterised by X-ray structure analyses. The intermediates can be rationalised as adducts of a lithium halide and a monomeric [Li2(NBut)2S] unit to give [(thf)3Li3(µ3-X){(NBut)3S}] (X = Br or I). In the presence of oxygen the oxidation reaction of [Li4{(NBut)3S}2] with iodine affords an adduct of lithium iodide and the sulfate analogue [(thf)3Li3(µ3-I){(NBut)3SO}] is obtained. As revealed by X-ray structure analysis, this adduct is very similar to [(thf)3Li3(µ3-I){(NBut)3S}] in the solid state.

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