Crystal structure of (4bS,9S)4b-hydroxy-11,13-dioxo-4b,7,8,9,10,11,12,13-octahydro-5H-6-thia-10,12a-diaza-cyclodeca[a]indene-9-carboxylic acid methyl ester, C16H18N2O5S, with a remarkable short S···H contact of 2.61 Å

A. G. Griesbeck, M. Oelgemöller, J. Lex
2002 Zeitschrift für Kristallographie - New Crystal Structures  
C 16H18N2O5S, monoclinic, P21 (No. 4), a = 10.390(1) Å, b = 7.105(1) Å, c = 11.639(1) Å, b = 109.95(1)°, V = 807.7 Å 3 , Z = 2, R gt(F) = 0.036, wRref(F 2 ) = 0.068, T = 293 K. Source of material The title compound was prepared from the N-phthaloyl derivative of the dipeptide glycyl L-methionine by irradiation (300 nm wavelength, 27 hours, 2 mmol in 100 ml of acetone at room temperature). The crude product was purified by column chromatography on silica (methanol / methylene chloride 1:20)
more » ... chloride 1:20) which yielded 54% of the diastereoisomerically pure cis compound. The resulting material was dissolved in acetone and after slow evaporation of the solvent, a colorless oil resulted from which tiny and air-sensitive colorless needles crystallized with mp of 468 K -469 K (cf. 471 K -473 K [1]).
doi:10.1524/ncrs.2002.217.2.235 fatcat:uwgzxm5jcbetxkoudbhgxaw64m