#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003504.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_2003504 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 944 _journal_page_last 946 _publ_section_title ; 3-Methyl-4H-pyrido[3,2-e][1,2,4]thiadiazine 1,1-Dioxide ; _chemical_formula_sum 'C7 H7 N3 O2 S' _chemical_formula_weight 197.22 _space_group_IT_number 9 _symmetry_space_group_name_Hall 'C -2yc' _symmetry_space_group_name_H-M 'C 1 c 1' _[local]_cod_cif_authors_sg_H-M 'C c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 20.709(3) _cell_length_b 7.7770(14) _cell_length_c 17.276(3) _cell_angle_alpha 90.00 _cell_angle_beta 143.279(5) _cell_angle_gamma 90.00 _cell_volume 1663.6(5) _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54180 _cell_measurement_reflns_used 39 _cell_measurement_theta_min 11.43 _cell_measurement_theta_max 39.45 _exptl_absorpt_coefficient_mu 3.237 _cell_measurement_temperature 293(2) _exptl_crystal_description prism _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.25 _exptl_crystal_colour colourless _chemical_compound_source 'Lab. of Medicinal Chemistry, Li\`ege' _diffrn_measurement_device 'Stoe-Siemens AED 4-circle diffractometer' _diffrn_measurement_method '\w' _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.3892 _exptl_absorpt_correction_T_max 0.5141 _diffrn_reflns_number 1049 _reflns_number_total 1049 _reflns_number_observed 1032 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_theta_max 54.99 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 10 _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '60' _diffrn_standards_decay_% 5.0 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0268 _refine_ls_wR_factor_obs 0.0691 _refine_ls_wR_factor_all 0.0693 _refine_ls_goodness_of_fit_obs 1.117 _refine_ls_goodness_of_fit_all 1.108 _refine_ls_number_reflns 1049 _refine_ls_number_parameters 240 _refine_ls_hydrogen_treatment ;H-atoms included as riding atoms at calculated positions, H atoms were constrained ; _refine_ls_weighting_scheme ;calc w = 1/[\s^2^(F~o~^2^)+(0.0461P)^2^+1.2809P] where P = (F~o~^2^+2F~c~^2^)/3 ; _refine_ls_shift/esd_max 0.000 _refine_diff_density_max 0.178 _refine_diff_density_min -0.223 _refine_ls_extinction_method 'F~c~^*^ = kF~c~[1+0.001xF~c~^2^\l^3^/sin(2\q)]' _refine_ls_extinction_coef 0.0056(3) 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 _refine_ls_abs_structure_details 'Flack (1983), h = 0.09(2)' _refine_ls_abs_structure_Flack 0.09(2) 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 0.26022(8) 0.06330(15) 0.82916(9) 0.0441(4) N2 1 0.1610(4) -0.0669(5) 0.7277(5) 0.0543(12) C3 1 0.0618(4) -0.0189(7) 0.6465(6) 0.0481(15) N4 1 0.0312(3) 0.1350(5) 0.6422(4) 0.0427(9) H4 1 -0.0364(3) 0.1600(5) 0.5756(4) 0.061(6) C5 1 0.1018(3) 0.2573(6) 0.7384(4) 0.0365(10) C6 1 0.0659(4) 0.4028(6) 0.7434(5) 0.0461(12) H6 1 -0.0076(4) 0.4234(6) 0.6789(5) 0.061(6) C7 1 0.1394(5) 0.5136(6) 0.8433(6) 0.0527(13) H7 1 0.1170(5) 0.6127(6) 0.8472(6) 0.061(6) C8 1 0.2488(4) 0.4778(8) 0.9400(6) 0.062(2) H8 1 0.2984(4) 0.5527(8) 1.0100(6) 0.061(6) N9 1 0.2860(3) 0.3421(6) 0.9374(4) 0.0525(11) C10 1 0.2130(3) 0.2377(6) 0.8371(4) 0.0379(10) C11 1 -0.0245(5) -0.1502(8) 0.5519(7) 0.074(2) H111 1 -0.0868(12) -0.0966(12) 0.4695(11) 0.094(9) H112 1 -0.0438(22) -0.1996(36) 0.5824(19) 0.094(9) H113 1 0.0015(12) -0.2389(26) 0.5431(29) 0.094(9) O12 1 0.2861(3) 0.1236(5) 0.7772(4) 0.0593(10) O13 1 0.3461(4) -0.0172(6) 0.9522(4) 0.0832(15) S21 1 0.03733(7) 0.03070(13) 0.88108(8) 0.0383(3) N22 1 0.1458(3) -0.0644(5) 0.9548(4) 0.0465(11) C23 1 0.2431(4) -0.0119(6) 1.0665(5) 0.0360(11) N24 1 0.2678(3) 0.1352(5) 1.1237(3) 0.0369(9) H24 1 0.3349(3) 0.1561(5) 1.1969(3) 0.061(6) C25 1 0.1927(3) 0.2591(5) 1.0735(4) 0.0334(10) C26 1 0.2240(4) 0.4173(6) 1.1345(4) 0.0413(11) H26 1 0.2966(4) 0.4411(6) 1.2129(4) 0.061(6) C27 1 0.1475(4) 0.5357(7) 1.0781(5) 0.0464(12) H27 1 0.1671(4) 0.6420(7) 1.1172(5) 0.061(6) C28 1 0.0390(4) 0.4967(6) 0.9609(5) 0.0466(12) H28 1 -0.0127(4) 0.5788(6) 0.9237(5) 0.061(6) N29 1 0.0063(3) 0.3481(5) 0.9003(4) 0.0413(9) C30 1 0.0828(3) 0.2312(6) 0.9575(4) 0.0359(11) C31 1 0.3343(4) -0.1270(7) 1.1316(5) 0.0540(14) H311 1 0.4017(4) -0.0707(22) 1.2071(22) 0.094(9) H312 1 0.3298(19) -0.1521(42) 1.0730(14) 0.094(9) H313 1 0.3302(19) -0.2321(22) 1.1566(35) 0.094(9) O32 1 -0.0054(3) -0.0625(4) 0.9030(4) 0.0539(9) O33 1 -0.0333(3) 0.0571(5) 0.7483(3) 0.0604(10) 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 0.0362(7) 0.0136(5) 0.0273(6) 0.0414(7) 0.0061(5) 0.0402(7) N2 0.061(3) -0.001(2) 0.056(3) 0.035(2) -0.008(2) 0.075(3) C3 0.059(4) -0.009(3) 0.052(4) 0.033(3) -0.010(3) 0.064(4) N4 0.028(2) -0.006(2) 0.022(2) 0.043(2) -0.009(2) 0.038(2) C5 0.029(2) 0.005(2) 0.022(2) 0.039(3) 0.002(2) 0.032(2) C6 0.031(3) 0.007(2) 0.024(2) 0.045(3) 0.000(2) 0.042(3) C7 0.044(3) 0.000(3) 0.034(3) 0.045(3) -0.014(3) 0.051(3) C8 0.041(3) -0.006(3) 0.032(3) 0.062(4) -0.024(3) 0.055(3) N9 0.028(2) 0.002(2) 0.019(2) 0.059(3) -0.011(2) 0.037(2) C10 0.033(2) 0.005(2) 0.025(2) 0.037(2) 0.000(2) 0.035(2) C11 0.069(4) -0.032(3) 0.069(4) 0.062(4) -0.036(3) 0.099(5) O12 0.054(2) 0.004(2) 0.056(2) 0.064(2) 0.001(2) 0.076(2) O13 0.079(3) 0.049(3) 0.043(2) 0.077(3) 0.028(2) 0.052(2) S21 0.0263(6) -0.0065(5) 0.0178(5) 0.0337(6) -0.0058(5) 0.0314(6) N22 0.034(2) -0.004(2) 0.028(2) 0.042(2) -0.012(2) 0.046(3) C23 0.033(3) -0.001(2) 0.029(3) 0.033(2) -0.002(2) 0.040(3) N24 0.021(2) 0.000(2) 0.015(2) 0.033(2) -0.001(2) 0.031(2) C25 0.026(2) -0.002(2) 0.020(2) 0.032(2) 0.001(2) 0.031(2) C26 0.029(2) -0.011(2) 0.020(2) 0.037(3) -0.011(2) 0.035(2) C27 0.042(3) -0.005(2) 0.033(2) 0.035(3) -0.009(2) 0.049(3) C28 0.036(3) 0.005(2) 0.032(3) 0.038(3) 0.002(2) 0.051(3) N29 0.029(2) 0.001(2) 0.025(2) 0.031(2) 0.002(2) 0.044(2) C30 0.028(2) -0.003(2) 0.022(2) 0.035(3) 0.002(2) 0.034(2) C31 0.040(3) 0.005(2) 0.042(3) 0.046(3) -0.001(3) 0.068(4) O32 0.047(2) -0.014(2) 0.044(2) 0.043(2) -0.009(2) 0.065(2) O33 0.044(2) -0.009(2) 0.020(2) 0.063(2) -0.007(2) 0.030(2)