T. CHIVERS and J. PROCTOR. Can. J. Chem. 57, 1286(1979). Pentasulfur hexanitride, S5N6, has been prepared in good yield by the reaction of [n-Bu4N+][S4N5-] with bromine (or iodine) in methylene chloride at 0°C. In contrast, the tetrasulfur pentanitride(-1) ion reacts smoothly with chlorine to give S4N5CI, while the reaction with sulfuryl chloride produces S4N5C1 and S5N6 and the reaction with thionyl chloride produces a mixture of S3N20, S3N202, S4N4, and S5N6. Pentasulfur hexanitride is an air-sensitive, explosive, yellow-orange solid which sublimes at ca. 45DC/10-2 Torr without significant decomposition. It has been characterised by infrared, Raman, uv-visible, and mass spectra and by a single crystal X-ray structure determination. The crystals are monoclinic and belong to the space group C2/c, a = 8.787 (2) [Traduit par le journal]