#------------------------------------------------------------------------------ #$Date: 2013-08-29 18:37:19 +0300 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/00/57/2005764.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2005764 loop_ _publ_author_name 'Lubini, P.' 'Wouters, J.' _publ_section_title ; 6-Bromo-2H-3,1-benzoxazine-2,4(1H)-dione at 153K ; _journal_issue 12 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 3108 _journal_page_last 3110 _journal_volume 52 _journal_year 1996 _chemical_formula_sum 'C8 H4 Br N O3' _chemical_formula_weight 242.03 _chemical_name_systematic ; 4-Bromo-2H-1,3-Benzoxazine-2,4(1H)-dione ; _space_group_IT_number 33 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_space_group_name_H-M 'P n a 21' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 24.904(5) _cell_length_b 6.0290(12) _cell_length_c 5.1640(10) _cell_measurement_reflns_used 68 _cell_measurement_temperature 153(2) _cell_measurement_theta_max 12.5 _cell_measurement_theta_min 10 _cell_volume 775.4(3) _diffrn_ambient_temperature 153(2) _diffrn_measurement_device 'Stoe P4' _diffrn_measurement_method \q/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.061 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_number 1514 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_min 3.27 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 90 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 5.268 _exptl_absorpt_correction_T_max 0.813 _exptl_absorpt_correction_T_min 0.295 _exptl_absorpt_correction_type '\y scan (North, Phillips & Mathews, 1968)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 2.073 _exptl_crystal_density_meas 'not measured' _exptl_crystal_description 'thin plate' _exptl_crystal_F_000 472 _exptl_crystal_size_max .65 _exptl_crystal_size_mid .45 _exptl_crystal_size_min .04 _refine_diff_density_max 0.476 _refine_diff_density_min -0.422 _refine_ls_abs_structure_details 'Flack (1983) parameter = -0.01(3)' _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.026 _refine_ls_goodness_of_fit_obs 1.020 _refine_ls_hydrogen_treatment 'H atoms riding' _refine_ls_matrix_type full _refine_ls_number_parameters 118 _refine_ls_number_reflns 1348 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.026 _refine_ls_restrained_S_obs 1.019 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_obs 0.0559 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1126P)^2^+0.7760P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.1424 _refine_ls_wR_factor_obs 0.1343 _reflns_number_observed 1223 _reflns_number_total 1348 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file du1159.cif _[local]_cod_data_source_block br _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2005764 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' 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 _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_type_symbol Br 1 0.73941(3) 0.55628(11) 0.9741(3) 0.0278(3) Uani d . Br N 1 0.5494(3) 0.1898(9) 1.5616(11) 0.0204(14) Uani d . N H1 1 0.5350 0.0633 1.5128 0.024 Uiso calc R H O1 1 0.5491(2) 0.4954(8) 1.8364(11) 0.0233(12) Uani d . O C1 1 0.5274(3) 0.2966(11) 1.7646(14) 0.0182(15) Uani d . C O2 1 0.4905(2) 0.2278(8) 1.8923(11) 0.0283(14) Uani d . O C2 1 0.5909(3) 0.5987(12) 1.7063(13) 0.0187(16) Uani d . C C3 1 0.6588(3) 0.5592(11) 1.3602(15) 0.0197(16) Uani d . C H3 1 0.6736 0.6992 1.4054 0.024 Uiso calc R H O3 1 0.6045(2) 0.7777(8) 1.7822(11) 0.0258(13) Uani d . O C4 1 0.6798(3) 0.4385(10) 1.1602(15) 0.0185(15) Uani d . C C5 1 0.6593(3) 0.2313(12) 1.0897(13) 0.0178(15) Uani d . C H5 1 0.6751 0.1497 0.9523 0.021 Uiso calc R H C6 1 0.6156(3) 0.1465(12) 1.2221(14) 0.0198(16) Uani d . C H6 1 0.6008 0.0068 1.1752 0.024 Uiso calc R H C7 1 0.5934(3) 0.2683(10) 1.4252(13) 0.0150(15) Uani d . C C8 1 0.6151(3) 0.4728(10) 1.4968(17) 0.0167(14) Uani d . C loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br 0.0216(5) 0.0328(4) 0.0289(4) -0.0033(3) 0.0048(5) 0.0034(5) N 0.021(3) 0.015(3) 0.025(3) -0.002(3) 0.004(2) 0.000(2) O1 0.026(3) 0.022(2) 0.022(3) 0.003(3) 0.006(2) 0.000(2) C1 0.020(4) 0.015(3) 0.020(3) 0.003(3) -0.001(3) 0.001(3) O2 0.025(3) 0.029(3) 0.031(3) 0.003(3) 0.013(2) 0.007(2) C2 0.021(4) 0.019(3) 0.016(4) 0.005(3) 0.001(3) 0.001(3) C3 0.019(4) 0.018(3) 0.022(3) 0.000(3) -0.007(3) -0.002(3) O3 0.028(3) 0.021(3) 0.028(3) 0.003(2) -0.003(2) -0.008(2) C4 0.012(4) 0.026(4) 0.018(3) 0.001(3) -0.002(3) 0.005(3) C5 0.013(3) 0.022(3) 0.018(3) 0.006(3) -0.002(3) -0.003(3) C6 0.021(4) 0.016(3) 0.023(4) 0.003(3) -0.006(3) -0.001(3) C7 0.007(3) 0.015(3) 0.023(4) -0.001(2) 0.000(3) 0.001(3) C8 0.021(3) 0.019(3) 0.011(4) 0.003(3) -0.002(4) 0.001(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C1 N C7 123.6(6) yes C1 O1 C2 124.0(6) yes O2 C1 N 124.9(7) yes O2 C1 O1 117.1(7) yes N C1 O1 118.0(7) yes O3 C2 O1 117.3(7) yes O3 C2 C8 126.7(7) yes O1 C2 C8 116.0(6) yes C4 C3 C8 118.8(6) yes C3 C4 C5 122.1(7) yes C3 C4 Br 118.8(5) yes C5 C4 Br 119.1(6) yes C6 C5 C4 119.3(7) yes C5 C6 C7 119.2(6) yes N C7 C6 121.0(6) yes N C7 C8 118.2(6) yes C6 C7 C8 120.8(7) yes C7 C8 C3 119.7(7) yes C7 C8 C2 119.9(7) yes C3 C8 C2 120.3(6) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Br C4 1.905(8) yes N C1 1.346(9) yes N C7 1.387(9) yes O1 C1 1.366(9) yes O1 C2 1.386(10) yes C1 O2 1.206(9) yes C2 O3 1.197(9) yes C2 C8 1.452(10) yes C3 C4 1.368(11) yes C3 C8 1.397(11) yes C4 C5 1.398(10) yes C5 C6 1.383(11) yes C6 C7 1.394(10) yes C7 C8 1.396(9) yes _cod_database_fobs_code 2005764