Abstract
The title compound, C14H16N2S3, crystallized with two independent mol-ecules [(1 a ) and (1 b )] in the asymmetric unit. Both mol-ecules display a pseudo-trans conformation. The two consecutive S-S bond lengths of the tris-ulfane unit of mol-ecule (1 a ) are 2.06 (3) and 2.08 (3) Å, and 2.08 (3) and 2.07 (2) Å for mol-ecule (1 b ). Torsion angles about each of the two S-S bonds are 86.6 (2) and 87.0 (2)° for (1 a ), and -84.6 (2) and -85.9 (2)° for (1 b ). The core atoms, viz. the N-S-S-S-N moiety, of the two mol-ecules superimpose well if one is inverted on the other, but the phenyl groups do not. Thus, the two units are essentially conformational enanti-omers. In mol-ecule (1 a ), the two phenyl rings are inclined to one another by 86.7 (3)°, and in mol-ecule (1 b ), by 81.1 (3)°. In the crystal, mol-ecules are linked via C-H⋯π inter-actions, forming sheets lying parallel to (010).
Highlights
N—S—S—S—N moiety, of the two molecules superimpose well if one is inverted on the other, but the phenyl groups do not
Molecules are linked via C—H interactions, forming sheets lying parallel to (010)
The reactions of substrates with one or two sulfanyl chloride, acid chloride, and/orsulfanyl moieties have been of interest to our laboratory for some time (Barany et al, 1983; Barany & Mott, 1984; Schroll & Barany, 1986; Schroll et al, 1990; Schroll et al, 2012)
Summary
The reactions of substrates with one or two sulfanyl chloride, acid chloride, and/or (alkoxydichloromethyl)sulfanyl moieties have been of interest to our laboratory for some time (Barany et al, 1983; Barany & Mott, 1984; Schroll & Barany, 1986; Schroll et al, 1990; Schroll et al, 2012) In some of these experiments, bis[methyl(phenyl)amino]trisulfane was a component of more complicated mixtures of polysulfanes with varying numbers of S atoms. One such mixture was separated by preparative HPLC at 298 K, eluting with methanol–water (17:3). The fraction containing the title compound (dissolved in the eluting solvent) was cooled to 277 K, after which the trisulfane was obtained directly in crystalline form
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