The compound S3N2+AsF6− has been prepared by the reaction of S4N4 with AsF5. The crystal structure has been determined from three-dimensional X-ray counter data. Crystals are monoclinic, space group P21/c with a = 8.499(4), b = 8.298(4), c = 11.069(8), β = 94.59(5), V = 778.1 Å3, Z = 4, and Dc = 2.67 g cm−3. The structure was solved by Patterson methods and refined to a conventional R factor of 0.028 for 798 independent reflections with I ≥ 3σ(I). The structure consists of discrete AsF6− ions and planar cyclic S3N2+ ions. Solutions of S3N2+AsF6− in methylene chloride gave a five-line electron spin resonance spectrum with an intensity ratio of 1:2:3:2:1 showing that the unpaired electron in S3N2+ is coupled to two equivalent nitrogen atoms in full accord with the results of the crystal structure determination.
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Gillespie et al. (1975) studied this question.