J. Gopalakrishnan et al., CYCLIC S-N COMPOUNDS AND PHOSPHORUS REAGENTS - XVII - SYNTHESIS AND X-RAY STRUCTURAL CHARACTERIZATION OF (PH)(DCA)(ME2N)P=N-S3N3 HETEROCYCLE, Proceedings of the Indian Academy of Sciences. Chemical sciences, 110(2), 1998, pp. 89-95
The phosphiniminocyclotrithiazene, (Ph)(DCA) (Me2N)PN-S3N3 (II) [DCA =
dicyclohexylamino] was obtained in approximate to 70% yield from room
temperature reaction of S4N4 with the corresponding phosphine, (Ph)(D
CA)(Me2N)P (I). Single crystal X-ray structure determination of (II) r
eveals slightly different P-N bond lengths around phosphorus [P-N(4):
1.607; P-N(5): 1.645 and P-N(6): 1.638 Angstrom] and almost planar con
figuration around both N(5) and N(6). The tricoordinate sulphur [S(1)]
substantially deviates (0.663 Angstrom) from the mean plane of the he
terocycle. The structural parameters of(II) are compared with the rece
ntly reported diethylamino and di-n-butylamino analogues. (II) affords
(Ph)(DCA)(Me2N)P = N-S3N (IV) in approximate to 60% yield on thermoly
sis in solution.