Abstract
Crystalline (S3N2)2NAsF6 was prepared in ca. 60% yield from a 1 : 1 mixture of S4N4 and S2NAsF6 in liquid SO2 at 0 °C, and its structure determined by X-ray crystallography. The compound crystallises in the monoclinic space group C2/c with unit-cell dimensions a= 17.343(6), b= 17.103(6), c= 16.737(9)A, β= 98.29(3)°, and Z= 16. The structure was solved by direct methods and refined by least-squares techniques to a final R of 0.11 for 2 308 observed reflections. (S3N2)2NAsF6 is essentially ionic with sulphur–fluorine cation–anion contacts. The (S3N2)2N+ cation is the first example of a monobridged bicyclic sulphur–nitrogen cation, and consists of two thiodithiazyl (S3N2) groups connected together by a bridging nitrogen atom attached to a sulphur atom of each S3N2 ring. The S3N2 rings are cis with respect to the bridging nitrogen atom, and are essentially eclipsed with respect to the SNS bridge. (S3N2)2NAsF6 reacts with CsN3 in liquid SO2 solution yielding impure poly(sulphur nitride) and CsAsF6. Solutions of (S3N2)2NAsF6 in liquid SO2 slowly disproportionate to S4N2AsF6 and S4N4. The i.r. spectrum of (S3N2)2NAsF6 is also reported.
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