Abstract
The reactions between 1,2,4-thiadiazol-3,5-dicarbonitrile, S(CN)4, and sulfur chlorides (SCl2 and S2Cl2) in the presence of Adogen® 464 (Aldrich) proceeds with formation of S3(CN)4Cl2 (1) and S3(CN)8Cl2 (2). These main products were characterized by X-ray structure determination of an adduct 1a and of 2. This adduct 1a was obtained by addition of the Lewis acid AsF5 in liquid SO2. 1a crystallizes with one SO2 molecule in the space group P21/n with a = 1177.3(2), b = 1082.8(1), c = 1255.3(5) pm, β = 109.73(3)°, Z = 4, V = 1.5061 nm3. It contains two five-membered rings connected by a nitrogen atom. AsF5 is coordinated to one of the ring nitrogen atoms [N(1)] adjacent to the sulfur atom S(1) and C(1)Cl-group. The other ring contains an S(2)-S(3) bond of length 207.7(4) pm. The rings are planar within experimental error. 2 crystallizes in the space group P21/n with a = 782.12(6), b = 1498.1(5), c = 1217.8(2) pm, β = 102.43(1)°, Z = 4, V = 1.3934 nm3. 2 is formed by addition of one molecule of SCl2 to two molecules of S(CN)4.
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