Crystal structure of 4-benzoyl-3-methyl-1-phenyl-2-pyrazolin-5-one sulfadiazine dimethylformamide monosolvate, C30H29N7O4S (original) (raw)

2014, Zeitschrift für Kristallographie - New Crystal Structures

C 30 H 29 N 7 O 4 S, triclinic, P1 (no. 2), a =7.7793(3) Å, b =9.1053(4) Å, c =21.7108(9)Å,a=97.433(2)°, b =93.025(2)°, g =111.055(2)°, V =1414.9 Å 3 , Z =2, R gt (F) =0.0399, wR ref (F 2) =0.1084, T =200 K. Source of material The reagents were of analytical grade and wereused as obtained. To as olution of synthesized4-benzoyl-3-methyl-1-phenyl-2pyrazolin-5-one (2.0 mmol,0 .56g)i nm ethanol(10 mL)w as addedslowlytosulfadiazine(2.0mmol, 0.50 g) in methanol(10 mL)while stirring, and the mixture was refluxed for 3h.The pale yellow precipitate obtained was filtered, washed with methanol, dried at room temperature and stored over fused CaCl 2 .Yellow cubic single crystals of the titled ketoimine Schiff base good enough for x-ray diffraction were grown at room temperature from slow evaporation of dimethylformamide solution. Experimental details Carbon-bound Hatoms were placed in calculated positions and were included in the refinement in the riding model approximation, with U iso (H) sett o1 .2U eq (C). The Ha toms of the methyl groups were allowed to rotate with afixed angle around the CC bond to best fit the experimental electron density (HFIX 137 in the SHELX program suite [11]), with U iso (H) sett o1 .5U eq (C).