An improved synthesis and purification, and some properties, of powdered (SN)X are reported. Gram quantities can be prepared by reacting (NSCl)3 and Me3SiN3(molar ratio 1:7.5) in acetonitrile, followed by the liquid-SO2 extraction of impurities. The product polymers are fine black powders; surface areas (14–22 m2 g–1) were measured by the B.E.T. method. Freshly prepared and purified samples readily converted to S4N4 both photolytically and by thermal activation; a rapid solid-state conversion to S4N4 occurred at ca. 120 °C (under N2). Differential scanning calorimetry gave ΔH(conversion)=–(20 ± 1) kJ mol–1 of S4N4. Aged samples of powdered polymer were sublimed in vacuo at 110 °C to give gold-bronze conductive layers, σ(bulk)≈ 5 Ω–1 cm–1. A new mode of growth of (SN)X single crystals during high-vacuum sublimation was observed.
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Journal of the Chemical Society, Dalton Transactions
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