#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2002939.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_2002939 _journal_name_full 'Acta Crystallographica, Section B' _journal_year 1999 _journal_volume B55 _journal_page_first 530 _journal_page_last 542 _publ_section_title ; Packing similarities of 3 isosteric molecules: 5,6-dichlorophthalic anhydride, 5,6-dibromophthalic anhydride, and 5,6-dichlorobenzfurazan-1-oxide including three polymorphs of 5,6-dichlorobenzfurazan-1-oxide ; _chemical_name_common '4,5-dibromophthalic anhydride' _chemical_formula_moiety ? _chemical_formula_sum 'C8 H2 Br2 O3' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_weight 305.92 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'C-1' 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 12.923(3) _cell_length_b 9.209(2) _cell_length_c 7.6280(15) _cell_angle_alpha 105.08(3) _cell_angle_beta 99.20(3) _cell_angle_gamma 81.29(3) _cell_volume 859.5(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13 _cell_measurement_theta_max 22 _cell_measurement_temperature 297(2) _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 2.364 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 9.40 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_process_details ; North, A. C. T., Phillips, D. C., and Mathews, F. S. (1968). Acta Cryst., A24, 351-359. ; _exptl_absorpt_correction_T_min 0.23 _exptl_absorpt_correction_T_max 0.52 _diffrn_ambient_temperature 297(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'CAD-4' _diffrn_measurement_method '\w-2\q' _diffrn_reflns_number 4009 _diffrn_reflns_av_R_equivalents 0.050 _diffrn_reflns_av_sigmaI/netI 0.085 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 28 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% '<1' _reflns_number_total 2058 _reflns_number_observed 1284 _reflns_observed_criterion >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.099 _refine_ls_R_factor_obs 0.050 _refine_ls_wR_factor_all 0.139 _refine_ls_wR_factor_obs 0.117 _refine_ls_goodness_of_fit_all 1.028 _refine_ls_goodness_of_fit_obs 1.120 _refine_ls_restrained_S_all 1.035 _refine_ls_restrained_S_obs 1.120 _refine_ls_number_reflns 2057 _refine_ls_number_parameters 119 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment 'idealized positions' _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.064P)^2^+0.18P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/esd_max 0.01 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.80 _refine_diff_density_min -0.74 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0047(9) 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' loop_ _atom_site_label _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_occupancy _atom_site_disorder_group _atom_site_type_symbol C1 0.5553(5) 0.2655(8) 0.2842(9) 0.0378(14) Uani d . 1 . C C2 0.4529(5) 0.2683(8) 0.1995(10) 0.0399(15) Uani d . 1 . C C3 0.3955(5) 0.3988(8) 0.1619(9) 0.0368(14) Uani d . 1 . C H3 0.3259(5) 0.4010(8) 0.1070(9) 0.044 Uiso calc R 1 . H C4 0.4498(5) 0.5276(7) 0.2125(9) 0.0377(14) Uani d . 1 . C C5 0.5523(5) 0.5250(7) 0.2963(10) 0.0382(14) Uani d . 1 . C C6 0.6090(5) 0.3925(7) 0.3352(9) 0.0356(13) Uani d . 1 . C H6 0.6783(5) 0.3898(7) 0.3918(9) 0.043 Uiso calc R 1 . H C7 0.5912(6) 0.1096(8) 0.3068(11) 0.044(2) Uani d . 1 . C C8 0.4208(6) 0.1150(8) 0.1613(11) 0.044(2) Uani d . 1 . C O1 0.6722(5) 0.0542(6) 0.3695(9) 0.063(2) Uani d . 1 . O O2 0.5069(4) 0.0238(5) 0.2304(8) 0.0509(13) Uani d . 1 . O O3 0.3416(5) 0.0645(6) 0.0907(9) 0.061(2) Uani d . 1 . O Br4 0.37379(6) 0.70771(8) 0.16374(12) 0.0508(3) Uani d . 1 . Br Br5 0.62425(6) 0.69818(9) 0.35590(12) 0.0518(3) Uani d . 1 . Br 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 C1 0.031(3) 0.043(3) 0.038(4) -0.004(3) -0.005(3) 0.013(3) C2 0.036(4) 0.044(3) 0.039(4) -0.002(3) 0.005(3) 0.011(3) C3 0.027(3) 0.045(3) 0.036(3) -0.005(2) -0.004(3) 0.009(3) C4 0.038(4) 0.035(3) 0.040(4) 0.002(3) 0.004(3) 0.013(3) C5 0.039(4) 0.038(3) 0.036(4) -0.008(3) -0.001(3) 0.008(3) C6 0.027(3) 0.038(3) 0.039(4) -0.004(2) -0.002(3) 0.007(3) C7 0.045(4) 0.038(3) 0.047(4) -0.006(3) 0.000(3) 0.010(3) C8 0.035(4) 0.042(3) 0.052(5) -0.004(3) 0.002(3) 0.011(3) O1 0.050(3) 0.050(3) 0.081(4) 0.001(2) -0.020(3) 0.024(3) O2 0.040(3) 0.037(2) 0.068(4) -0.006(2) -0.013(3) 0.012(2) O3 0.045(3) 0.052(3) 0.082(4) -0.018(2) -0.017(3) 0.019(3) Br4 0.0495(5) 0.0434(4) 0.0597(6) 0.0052(3) 0.0031(4) 0.0211(4) Br5 0.0517(5) 0.0473(4) 0.0586(5) -0.0184(3) 0.0002(4) 0.0137(3)