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Salts of the Dithionitryl Ion (1+), [S=N=S]+

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S Sulfur-Nitrogen Compounds

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Abstract

The title compound was prepared by reacting S4N4 with sulfur and ASF, in SO2 in the presence of a trace amount of bromine via 1/2 S8 + S4N4 + 6 ASF5→4 S2N+ AsF -6 + 2 AsF3. This is the only route which gives high yields of a crystalline, soluble S2N+ salt. The synthesis was carried out in flame-dried, three-bulb Pyrex glass vessels incorporating a medium sintered glass frit and closed with a Teflon-stemmed glass valve. It is important to use a well-dried apparatus and reagents, and to add the required amount of ASF, and traces of bromine before the reaction mixture warms up to room temperature. SO2, AsF5 (2% [1] or 10% [2] excess), and a trace amount of Br2 were successively condensed onto a mixture of S8 (10% deficit) and S4N4. The mixture was stirred for 12 h (20 h [3]) at room temperature [1 to 3]. After removing the volatiles, the brownish yellow solid was treated with S8 in SO2 for another 12 h to convert SN+ AsF -6 (a minor product of the reaction) to S2N+ AsF -6 [1, 2]. In comparison to earlier papers [2, 3] the purification was improved. After filtration the soluble product was recrystallized four times by slowly removing the solvent. CCI3F and SO2 were added and the solution cooled to -78°C. After filtration the solvent was recondensed onto the solid (this process was repeated five times). Removal of the solvent gave highly crystalline S2N+ AsF -6 (90% yield based on S4N4). The remaining traces of sulfur were removed by sublimation at ca. 60°C/10-3 Torr after 14 h [1]. In another paper a different purification procedure was published: After stirring the reaction mixture for 12 h the solvent was removed, and the crude olive green product was stirred in CH2Cl2 for 24 h. Washing with CH2Cl2 increased the yield by 20%. The impurities were filtered off, and the product was washed briefly with more CH2Cl2 by back condensation. The yield was 95% [4].

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  1. Frankfurt am Main, Germany

    Alfons Kubny

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  1. Norbert Baumann
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  2. Hans-Jürgen Fachmann
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  3. Reimund Jotter
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Baumann, N., Fachmann, HJ., Jotter, R., Kubny, A. (1994). Salts of the Dithionitryl Ion (1+), [S=N=S]+. In: Baumann, N., Fachmann, HJ., Jotter, R., Kubny, A. (eds) S Sulfur-Nitrogen Compounds. Gmelin Handbook of Inorganic and Organometallic Chemistry / Gmelin Handbuch der Anorganischen Chemie, vol S / S-N / 10 / a. Springer, Berlin, Heidelberg. https://doi.org/10.1007/978-3-662-06351-4_4

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