. Can. J. Chem. 67, 1788 (1989). The reaction of (Me2N)3S+NSO-with sulphur has been investigated by ultraviolet-visible, infrared, Raman, and I4N, 170, and 33S nuclear magnetic resonance spectroscopies. The red species (A,,, 501 nm) formed initially is tentatively identified as SSNSO-. This anion is thermally unstable with respect to the formation of S4N-and sulphur oxyanions. Previously reported salts of the "NS02-" ion have been reinvestigated by infrared, Raman, and ' 4~ nmr spectroscopies, which indicate that the major component of these salts is the NSO-ion. The reaction of (Me2N)$S+NSO-with S4N4 is shown by 1 4~ nInr spectroscopy to produce both S3N3Op, the major product, and S3N3-.Key words: nitrogen-sulphur-oxygen (N-S-0) anions, I4N NMR spectroscopy.TR~STRAM CHIVERS, KENNETH J. SCHMIDT, DEANE D. MCINTYRE et HANS J. VOGEL. Can. J. Chem. 67, 1788 (1989). Faisant a pel aux mCthodes spectroscopiques ultraviolet-visible, infrarouge, Raman et rksonance magnttique nuclCaire du "N, "0 et h , on a Ctudie la rCaction du (Me2N)3S'NSO-avec le soufre. En premiere approximation, on a attribuC la structure SSNSO-aux especes rouges (A,,, de 501 nm) qui se foment initialement. Cet anion est thermiquement stable par rapport i la formation d'ions S4N-et d'oxyanions du soufre. Utilisant les mCthodes spectroscopiques ir, Raman et rmn du I4N, on a rCexaminC la structure de l'ion ((NS02-n dont la formation avait Ct C rapportte antkrieurement; ces rtsultats indiquent que la composante principale de ces sels est l'ion NSO-. En se basant sur la rmn du 1 4~, on dCmontre que la reaction du ( M~~N )~+ N S Oavec le S4N4 conduit ti la formation tant de S3N30-, le produit principal, que de S3N3-. Mots cle's : anions de nitrogene-soufre-oxygkne (N-S-0), spectroscopie RMN du 1 4~.[Traduit par la revue] Introduction Several nitrogen-sulphur-oxygen (N-S-0) anions that contain a sulphoxy group have been characterized. These include the acyclic species NSO-, 1 (1 -3), the ring system S3N30-, 2 (4), and the cage anion S4N50-, 3 (5). Recently we discovered that electrochemically generated solutions of 1 in acetonitrile (ca. 0.3 mM) react with elemental sulphur to give a red anion