#------------------------------------------------------------------------------ #$Date: 2011-09-28 15:24:46 +0100 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/36/2003625.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_2003625 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _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_moiety 'C6 H6 N4 O2 S, H2 O' _chemical_formula_sum 'C6 H8 N4 O3 S' _chemical_formula_weight 216.22 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yab' _symmetry_space_group_name_H-M 'P 1 21/a 1' _[local]_cod_cif_authors_sg_H-M 'P 21/a' 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' _cell_length_a 7.487(2) _cell_length_b 15.470(7) _cell_length_c 8.131(7) _cell_angle_alpha 90.00 _cell_angle_beta 109.55(3) _cell_angle_gamma 90.00 _cell_volume 887.5(9) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.5418 _cell_measurement_reflns_used 21 _cell_measurement_theta_min 18.55 _cell_measurement_theta_max 34.66 _exptl_absorpt_coefficient_mu 3.208 _cell_measurement_temperature 293(2) _exptl_crystal_description prism _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _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 0.5820 _exptl_absorpt_correction_T_max 0.7014 _diffrn_reflns_number 1219 _reflns_number_total 1219 _reflns_number_observed 964 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0 _diffrn_reflns_theta_max 59.19 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '60 min' _diffrn_standards_decay_% 2.6 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0342 _refine_ls_wR_factor_obs 0.1002 _refine_ls_wR_factor_all 0.1035 _refine_ls_goodness_of_fit_obs 1.173 _refine_ls_goodness_of_fit_all 1.062 _refine_ls_number_reflns 1219 _refine_ls_number_parameters 130 _refine_ls_hydrogen_treatment ; H atoms were constrained and included as riding atoms, except for the 4H- atom and water H atoms, which were kept fixed ; _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)+(0.0686P)^2^+0.1258P]' _refine_ls_shift/esd_max 0.000 _refine_diff_density_max 0.179 _refine_diff_density_min -0.260 _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)' _refine_ls_extinction_coef 0.0104(11) 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 0.24943(9) 0.12782(4) 0.16130(9) 0.0456(3) N2 1 0.2255(3) 0.04719(13) 0.0360(3) 0.0490(6) C3 1 0.3235(4) -0.0248(2) 0.0870(3) 0.0420(6) N4 1 0.4828(3) -0.03139(12) 0.2284(3) 0.0447(6) H4 1 0.5538 -0.0874 0.2528 0.073(4) C5 1 0.5669(3) 0.0382(2) 0.3308(3) 0.0405(6) C6 1 0.7434(4) 0.0300(2) 0.4585(3) 0.0491(7) H6 1 0.8077(4) -0.0225(2) 0.4756(3) 0.073(4) C7 1 0.8217(4) 0.1002(2) 0.5587(4) 0.0543(7) H7 1 0.9389(4) 0.0935(2) 0.6455(4) 0.073(4) N8 1 0.7384(3) 0.1786(2) 0.5387(3) 0.0587(7) C9 1 0.5699(4) 0.1862(2) 0.4157(4) 0.0524(7) H9 1 0.5111(4) 0.2400(2) 0.3986(4) 0.073(4) C10 1 0.4773(4) 0.1181(2) 0.3118(3) 0.0425(6) N11 1 0.2716(3) -0.09588(14) -0.0086(3) 0.0537(6) H111 1 0.3353 -0.1466 0.0211 0.073(4) H112 1 0.1655 -0.0941 -0.0919 0.073(4) O1 1 0.1171(3) 0.12294(12) 0.2549(2) 0.0559(6) O2 1 0.2377(3) 0.20555(12) 0.0616(3) 0.0625(6) O3 1 0.6519(4) -0.18460(15) 0.2380(3) 0.0813(8) H31 1 0.7014 -0.1917 0.1425 0.073(4) H32 1 0.6912 -0.2332 0.3177 0.073(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 0.0453(5) 0.0056(3) 0.0130(3) 0.0298(4) 0.0024(3) 0.0583(4) N2 0.0474(13) 0.0039(10) 0.0100(10) 0.0321(12) -0.0030(11) 0.0613(13) C3 0.0411(15) -0.0025(11) 0.0162(13) 0.0320(15) -0.0009(12) 0.0531(15) N4 0.0440(13) 0.0011(9) 0.0121(10) 0.0283(11) -0.0012(10) 0.0580(13) C5 0.0385(14) -0.0006(11) 0.0180(12) 0.0318(14) 0.0015(12) 0.0531(14) C6 0.041(2) 0.0026(12) 0.0158(13) 0.044(2) 0.0014(13) 0.061(2) C7 0.042(2) -0.0029(13) 0.0144(13) 0.052(2) -0.0070(15) 0.066(2) N8 0.0479(14) -0.0106(11) 0.0172(12) 0.0492(15) -0.0128(12) 0.076(2) C9 0.049(2) -0.0034(12) 0.0222(15) 0.037(2) -0.0059(13) 0.073(2) C10 0.0408(15) -0.0010(11) 0.0174(12) 0.0330(14) 0.0012(11) 0.0547(14) N11 0.0495(14) 0.0002(10) 0.0107(11) 0.0348(12) -0.0080(12) 0.0697(14) O1 0.0426(11) 0.0072(8) 0.0184(9) 0.0586(13) -0.0015(10) 0.0665(12) O2 0.0767(14) 0.0072(9) 0.0171(11) 0.0321(11) 0.0132(10) 0.0728(13) O3 0.122(2) 0.0408(13) 0.0457(14) 0.0518(15) 0.0206(11) 0.0794(15) _cod_database_code 2003625