INVESTIGATION AND RATIONALIZATION OF HYDROGEN-BONDING PATTERNS IN SULFONYLAMINO COMPOUNDS AND RELATED MATERIALS - CRYSTAL-STRUCTURE DETERMINATION OF MICROCRYSTALLINE SOLIDS FROM POWDER X-RAY-DIFFRACTION DATA

The crystal structures of three sulfonylamino compounds have been solv ed ab initio using powder diffraction data collected using a conventio nal laboratory X-ray diffractometer, and refined using Rietveld profil e-refinement techniques. 4-Toluenesulfonamide (1) is monoclinic, P2(1) /n, with a = 7.7030(3), b = 16.4656(7), c = 6.5861 (3) angstrom, beta = 92.411 (2)degrees; benzenesulfonylhydrazine (2) is monoclinic, P2(1) /c, with a = 8.0924(2), b = 8.6082(2), c = 11.7122(4) angstrom, beta = 108.591 (2)degrees; and 4-toluenesulfonylhydrazine (3) is monoclinic, P2(1)/n, with a = 18.6021(6), b = 5.6406(2), c = 8.5356(3) angstrom, beta = 106.222(2)degrees. The structures of 1 and 2 were solved from p owder X-ray diffraction data by direct methods, using the SHELXS and S IR88 programs respectively; the structure of 3 was solved from powder X-ray diffraction data by the combined maximum entropy and likelihood method. The hydrogen bonding patterns in these crystals, and in the cr ystal structures of some related sulfonylamino compounds, are analysed and classified according to recently developed methods based on graph set analysis. For 1, the hydrogen bonding is described by the graph s et C(4)C(4); for 2, the graph set for the first-order network is N1 = C(5)S(5)C(4), and there are second-order networks R4(4)(14) and R4(4)( 18); for 3, the first-order network is N1 = C(5)S(5)C(4).