CRYSTAL AND MOLECULAR STRUCTURE OF ADDUCT FROM 3-DIAZOBUTANONE AND CARBON DISULFIDE

An X-ray single-crystal structure analysis of the adduct C9H12O2S2 derived from the thermal decomposition of 3-diazobutanone in carbon disulfide has shown it to be a 2-methylene-l,3-dithiacyclobutane. The crystals are monoclinic, a = 12.82, b = 13.48, c = 12.98, β = 104° 45’, and the space group is C2/c with eight molecules in the unit cell. The structure was determined from photographic data, using a combination of Patterson, Fourier, and symbolic addition methods; the final R factor on 1517 nonzero independent structure amplitudes was 0.097. The geometry of the molecule is discussed, with special emphasis on the planar system formed by the substituted 2-methylene-l,3-dithiacyclobutane unit. © 1968, American Chemical Society. All rights reserved.