#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003485.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2003485 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 946 _journal_page_last 948 _publ_section_title ; 3-Methyl-4H-pyrido[4,3-e][1,2,4]thiadiazine 1,1-Dioxide Monohydrate ; _chemical_formula_moiety 'C7 H7 N3 O2 S, H2 O' _chemical_formula_sum 'C7 H9 N3 O3 S1' _chemical_formula_weight 215.23 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.3055(6) _cell_length_b 8.4118(6) _cell_length_c 12.3965(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.731(7) _cell_angle_gamma 90.00 _cell_volume 959.10(11) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54180 _cell_measurement_reflns_used 52 _cell_measurement_theta_min 18.72 _cell_measurement_theta_max 37.15 _exptl_absorpt_coefficient_mu 2.934 _cell_measurement_temperature 293(2) _exptl_crystal_description prism _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.34 _exptl_crystal_colour colourless _chemical_compound_source ; Laboratory of Medicinal Chemistry, Li\`ege ; _diffrn_measurement_device 'Stoe-Siemens AED four-circle' _diffrn_measurement_method '\w-scan' _exptl_absorpt_correction_type 'semi-empirical via \y scans' _exptl_absorpt_correction_T_min 0.3486 _exptl_absorpt_correction_T_max 0.4475 _diffrn_reflns_number 1202 _reflns_number_total 1202 _reflns_number_observed 1119 _reflns_observed_criterion I>2sigma(I) _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_theta_max 55.01 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '60 min' _diffrn_standards_decay_% 2.5 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0375 _refine_ls_wR_factor_obs 0.1012 _refine_ls_wR_factor_all 0.1020 _refine_ls_goodness_of_fit_obs 1.125 _refine_ls_goodness_of_fit_all 1.089 _refine_ls_number_reflns 1202 _refine_ls_number_parameters 134 _refine_ls_hydrogen_treatment ? _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(F~o~^2^) + (0.0618P)^2^ + 0.4223P] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_shift/esd_max 0.000 _refine_diff_density_max 0.23 _refine_diff_density_min -0.34 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.086(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0181 0.009 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.000 'N' 'N' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0311 0.018 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0492 0.032 'S' 'S' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.3331 0.556 loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv S1 1 0.83365(6) 0.02798(8) 0.13155(5) 0.0508(4) N2 1 0.7520(3) 0.0549(3) 0.2350(2) 0.0618(7) C3 1 0.6257(3) -0.0067(3) 0.2441(2) 0.0485(7) N4 1 0.5489(2) -0.1031(3) 0.1715(2) 0.0448(6) H4 1 0.4671(38) -0.1421(40) 0.1802(26) 0.077(4) C5 1 0.5946(2) -0.1568(3) 0.0775(2) 0.0405(6) C6 1 0.5122(3) -0.2632(3) 0.0083(2) 0.0507(7) H6 1 0.4245(3) -0.3015(3) 0.0251(2) 0.077(4) C7 1 0.5616(3) -0.3108(3) -0.0846(2) 0.0580(8) H7 1 0.5050(3) -0.3822(3) -0.1300(2) 0.077(4) N8 1 0.6869(3) -0.2610(3) -0.1148(2) 0.0614(7) C9 1 0.7656(3) -0.1607(3) -0.0483(2) 0.0572(8) H9 1 0.8532(3) -0.1255(3) -0.0672(2) 0.077(4) C10 1 0.7254(2) -0.1049(3) 0.0480(2) 0.0435(7) C11 1 0.5587(4) 0.0318(3) 0.3438(2) 0.0636(8) H111 1 0.6319(8) 0.0270(37) 0.4072(4) 0.148(11) H112 1 0.4835(23) -0.0439(23) 0.3509(14) 0.148(11) H113 1 0.5178(31) 0.1367(15) 0.3369(12) 0.148(11) O12 1 0.9714(2) -0.0436(3) 0.1676(2) 0.0671(6) O13 1 0.8381(2) 0.1747(2) 0.0739(2) 0.0737(7) O14 1 0.2734(2) -0.2085(3) 0.1817(2) 0.0781(8) H141 1 0.2037 -0.1896 0.1221 0.077(4) H142 1 0.2406 -0.2185 0.2556 0.077(4) loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 S1 0.0380(5) -0.0092(3) 0.0057(3) 0.0552(6) 0.0061(3) 0.0588(5) N2 0.0531(14) -0.0165(11) 0.0128(11) 0.0642(15) -0.0153(12) 0.069(2) C3 0.050(2) 0.0040(12) 0.0107(12) 0.0414(14) 0.0015(12) 0.055(2) N4 0.0376(11) -0.0052(9) 0.0118(9) 0.0513(13) 0.0016(10) 0.0473(12) C5 0.0362(13) 0.0009(10) 0.0077(10) 0.0434(14) 0.0085(11) 0.0424(13) C6 0.0463(14) -0.0114(12) 0.0108(11) 0.056(2) 0.0019(12) 0.0508(15) C7 0.062(2) -0.0103(14) 0.0080(13) 0.065(2) -0.0034(13) 0.048(2) N8 0.0623(15) -0.0048(12) 0.0190(11) 0.071(2) -0.0052(12) 0.0543(14) C9 0.0463(15) -0.0036(13) 0.0229(13) 0.066(2) 0.0044(14) 0.064(2) C10 0.0352(13) -0.0010(11) 0.0092(11) 0.0459(14) 0.0087(11) 0.0502(14) C11 0.071(2) 0.0015(14) 0.0234(15) 0.060(2) -0.0113(14) 0.064(2) O12 0.0385(11) -0.0017(9) 0.0003(9) 0.090(2) 0.0083(11) 0.0703(13) O13 0.0728(14) -0.0199(10) 0.0029(11) 0.0587(13) 0.0155(11) 0.0867(14) O14 0.0469(11) -0.0081(11) 0.0138(9) 0.125(2) 0.0270(12) 0.0639(13)