The crystal structure of [NSON(CF 3) 2] 4 has been determined by single crystal X-ray diffraction. The crystals are tetragonal, I 4 - , a = b = 16.73(1), c = 4.73(1) Ā, Z = 2. The molecule possesses an eight-membered N 4S 4 ring with a crystallographic inverse tetrad axis at its centre; the nitroxyl radicals are attached to the sulphur atoms. The two independent SN bond lengths are 1.56(1) and 1.62(1) Ā; the geometry of the N 4S 4O 4 moiety is similar to that of N 4S 4F 4.