#------------------------------------------------------------------------------ #$Date: 2008-01-26 17:25:03 +0000 (Sat, 26 Jan 2008) $ #$Revision: 20 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003626.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_2003626 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 1385 _journal_page_last 1388 _publ_section_title ; 3-Amino-4H-pyrido[4,3-e]-1,2,4-thiadiazine 1,1-Dioxide Monohydrate and 3-tert-Butyl-4H-pyrido[4,3-e]-1,2,4-thiadiazine 1,1-Dioxide ; _chemical_formula_sum 'C10 H13 N3 O2 S' _chemical_formula_weight 239.29 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _symmetry_space_group_name_H-M 'P 21/a' _cell_length_a 9.802(9) _cell_length_b 11.682(9) _cell_length_c 10.384(16) _cell_angle_alpha 90.00 _cell_angle_beta 108.00(10) _cell_angle_gamma 90.00 _cell_volume 1130.9(23) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.5418 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 24.47 _cell_measurement_theta_max 39.93 _exptl_absorpt_coefficient_mu 2.477 _cell_measurement_temperature 293(2) _exptl_crystal_description prism _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.15 _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 (\y scan)' _exptl_absorpt_correction_T_min 0.3774 _exptl_absorpt_correction_T_max 0.6191 _diffrn_reflns_number 1566 _reflns_number_total 1566 _reflns_number_observed 1388 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0 _diffrn_reflns_theta_max 59.08 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '60 min' _diffrn_standards_decay_% 3.5 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0443 _refine_ls_wR_factor_obs 0.1276 _refine_ls_wR_factor_all 0.1297 _refine_ls_goodness_of_fit_obs 1.160 _refine_ls_goodness_of_fit_all 1.103 _refine_ls_number_reflns 1566 _refine_ls_number_parameters 151 _refine_ls_hydrogen_treatment ;H atoms were constrained and included as riding atoms, except for the 4H- atom, which was kept fixed ; _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)+(0.0785P)^2^+0.6684P] _refine_ls_shift/esd_max 0.000 _refine_diff_density_max 0.348 _refine_diff_density_min -0.379 _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)' _refine_ls_extinction_coef 0.0151(13) 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 0.03391(7) 0.74648(6) 0.47417(7) 0.0379(3) N2 1 0.1468(2) 0.7118(2) 0.6157(2) 0.0425(6) C3 1 0.2240(3) 0.6198(2) 0.6332(3) 0.0360(6) N4 1 0.2310(2) 0.5483(2) 0.5326(2) 0.0422(6) H4 1 0.2928 0.4837 0.5600 0.072(6) C5 1 0.1687(3) 0.5710(2) 0.3972(3) 0.0370(7) C6 1 0.1943(3) 0.5007(3) 0.2987(3) 0.0505(8) H6 1 0.2498(3) 0.4349(3) 0.3223(3) 0.072(6) C7 1 0.1354(3) 0.5315(3) 0.1669(3) 0.0569(9) H7 1 0.1514(3) 0.4835(3) 0.1016(3) 0.072(6) N8 1 0.0563(3) 0.6251(3) 0.1236(2) 0.0582(7) C9 1 0.0312(3) 0.6893(3) 0.2179(3) 0.0504(8) H9 1 -0.0241(3) 0.7549(3) 0.1906(3) 0.072(6) C10 1 0.0818(3) 0.6656(2) 0.3552(3) 0.0362(7) C11 1 0.3170(3) 0.5889(2) 0.7748(3) 0.0414(7) C12 1 0.4725(4) 0.5908(5) 0.7787(4) 0.099(2) H121 1 0.4989(13) 0.6673(8) 0.7623(41) 0.154(8) H122 1 0.4854(10) 0.5405(27) 0.7102(29) 0.154(8) H123 1 0.5320(5) 0.5657(35) 0.8661(15) 0.154(8) C13 1 0.2895(6) 0.6703(4) 0.8771(4) 0.108(2) H131 1 0.3284(38) 0.7442(11) 0.8679(28) 0.154(8) H132 1 0.3346(39) 0.6416(19) 0.9668(4) 0.154(8) H133 1 0.1881(7) 0.6769(27) 0.8616(27) 0.154(8) C14 1 0.2787(5) 0.4693(4) 0.8082(4) 0.0890(14) H141 1 0.1860(18) 0.4704(7) 0.8215(36) 0.154(8) H142 1 0.3491(22) 0.4432(13) 0.8895(21) 0.154(8) H143 1 0.2767(38) 0.4186(7) 0.7349(17) 0.154(8) O1 1 0.0519(2) 0.8658(2) 0.4514(2) 0.0516(6) O2 1 -0.1059(2) 0.7128(2) 0.4749(2) 0.0527(6) 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 0.0340(5) 0.0020(3) 0.0064(3) 0.0382(5) -0.0012(3) 0.0382(5) N2 0.0430(13) 0.0046(11) 0.0090(11) 0.0489(14) -0.0038(11) 0.0336(13) C3 0.0351(14) -0.0017(12) 0.0079(11) 0.0386(15) -0.0018(12) 0.0327(14) N4 0.0486(14) 0.0087(10) 0.0035(10) 0.0404(13) -0.0021(10) 0.0316(13) C5 0.0359(14) -0.0003(12) 0.0046(11) 0.043(2) -0.0017(11) 0.0286(14) C6 0.054(2) 0.0123(15) 0.0061(13) 0.055(2) -0.0047(14) 0.037(2) C7 0.064(2) 0.011(2) 0.0116(15) 0.070(2) -0.006(2) 0.034(2) N8 0.069(2) 0.0062(14) 0.0094(12) 0.067(2) 0.0003(13) 0.0337(13) C9 0.052(2) 0.0060(14) 0.0038(14) 0.053(2) 0.0062(14) 0.039(2) C10 0.0332(14) -0.0028(11) 0.0038(11) 0.0401(15) 0.0000(12) 0.0311(14) C11 0.043(2) 0.0005(13) 0.0059(12) 0.049(2) 0.0005(12) 0.0282(14) C12 0.048(2) -0.022(3) -0.003(2) 0.188(5) 0.020(3) 0.049(2) C13 0.155(5) 0.059(3) -0.002(2) 0.113(4) -0.014(2) 0.036(2) C14 0.124(4) -0.025(3) 0.000(2) 0.078(3) 0.017(2) 0.047(2) O1 0.0571(13) 0.0010(9) 0.0083(10) 0.0392(12) -0.0011(9) 0.0526(12) O2 0.0367(11) -0.0008(10) 0.0159(10) 0.0618(13) -0.0053(11) 0.0603(13)