#------------------------------------------------------------------------------ #$Date: 2016-03-26 14:26:29 +0200 (Sat, 26 Mar 2016) $ #$Revision: 180262 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/11/48/7114849.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_7114849 loop_ _publ_author_name 'Vasilyev, Aleksandr V.' 'Lindeman, Sergey V.' 'Kochi, Jay K.' _publ_section_title ; Noncovalent binding of the halogens to aromatic donors. Discrete structures of labile Br2 complexes with benzene and toluene ; _journal_issue 10 _journal_name_full 'Chemical Communications' _journal_page_first 909 _journal_paper_doi 10.1039/b102148f _journal_year 2001 _chemical_compound_source 'chemical synthesis' _chemical_formula_sum 'C6 H6 Br2' _chemical_formula_weight 237.93 _chemical_melting_point 'below -15C' _chemical_name_systematic ; Benzene/Dibromine Molecular Complex 1:1 ; _space_group_IT_number 154 _symmetry_cell_setting trigonal _symmetry_space_group_name_Hall 'P 32 2"' _symmetry_space_group_name_H-M 'P 32 2 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 3 _cell_length_a 8.721(2) _cell_length_b 8.721(2) _cell_length_c 8.701(2) _cell_measurement_reflns_used 4035 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 28.6 _cell_measurement_theta_min 2.6 _cell_volume 573.1(2) _computing_cell_refinement 'SAINT V6.01 (BrukerAXS, 1997-99)' _computing_data_collection 'SMART V5.054 (BrukerAXS, 1997-98)' _computing_data_reduction 'SAINT & SADABS V2.06 (Sheldrick, 2000)' _computing_molecular_graphics 'XP V5.06 (BrukerAXS, 1997-99)' _computing_publication_material 'SHELXL-93, XCIF V5.05 (BrukerAXS, 1997-99)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _diffrn_ambient_temperature 123(2) _diffrn_measurement_device 'Siemens/Bruker SMART 1K' _diffrn_measurement_method ; omega-scan, frame range 0.3 deg, hemisphere + two additional phi-scans ; _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_sigmaI/netI 0.0187 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 7294 _diffrn_reflns_theta_max 29.03 _diffrn_reflns_theta_min 2.70 _diffrn_standards_decay_% none _diffrn_standards_number none _exptl_absorpt_coefficient_mu 10.508 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_correction_T_min 0.11 _exptl_absorpt_correction_type 'Semi-empirical (SADABS procedure)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 2.068 _exptl_crystal_density_method none _exptl_crystal_description 'crystal grown along capillary' _exptl_crystal_F_000 336 _exptl_crystal_size_max 7.0 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _refine_diff_density_max 0.985 _refine_diff_density_min -2.206 _refine_diff_density_rms 0.220 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.15(26) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.171 _refine_ls_goodness_of_fit_obs 1.180 _refine_ls_hydrogen_treatment ; riding model with Uiso=1.2Uiso/eq of an adjacent carbon atom ; _refine_ls_matrix_type full _refine_ls_number_parameters 22 _refine_ls_number_reflns 581 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.409 _refine_ls_restrained_S_obs 1.180 _refine_ls_R_factor_all 0.0759 _refine_ls_R_factor_obs 0.0634 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+8.9084P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.1781 _refine_ls_wR_factor_obs 0.1438 _reflns_number_observed 549 _reflns_number_total 597 _reflns_observed_criterion >2sigma(I) _cod_data_source_file b102148f.txt _cod_data_source_block alexasx _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+8.9084P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+8.9084P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_sg_symbol_H-M P3(2)21 _cod_database_code 7114849 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'y, x, -z' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0303(6) 0.0264(6) 0.0270(5) -0.0007(4) 0.0009(5) -0.0103(5) loop_ _atom_site_label _atom_site_type_symbol _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_occupancy _atom_site_calc_flag _atom_site_refinement_flags Br1 Br 0.6260(2) 0.9635(2) 0.03832(11) 0.0388(5) Uani 1 d . C1 C 0.5440(27) 1.0000 -0.3333 0.030(4) Uiso 1 d S H1 H 0.4351(27) 1.0000 -0.3333 0.035 Uiso 1 calc SR C2 C 0.5412(24) 0.8451(21) -0.3120(15) 0.036(3) Uiso 1 d . H2 H 0.4314(24) 0.7393(21) -0.2965(15) 0.043 Uiso 1 calc R C3 C 0.7025(19) 0.8389(22) -0.3125(16) 0.033(3) Uiso 1 d . H3 H 0.7033(19) 0.7312(22) -0.2993(16) 0.039 Uiso 1 calc R C4 C 0.8579(32) 1.0000 -0.3333 0.041(5) Uiso 1 d S H4 H 0.9669(32) 1.0000 -0.3333 0.049 Uiso 1 calc SR 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' Br Br -0.2901 2.4595 '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_site_symmetry_1 Br1 Br1 C2 175.3(3) 5_675 C2 C1 C2 122.4(29) 5_674 C1 C2 C3 120.6(22) . C1 C2 Br1 85.5(6) . C3 C2 Br1 86.7(9) . C4 C3 C2 116.1(23) . C3 C4 C3 124.1(31) 5_674 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Br1 Br1 2.301(2) 5_675 Br1 C2 3.184(13) . C1 C2 1.35(2) 5_674 C1 C2 1.35(2) . C2 C3 1.43(2) . C3 C4 1.39(2) . C4 C3 1.39(2) 5_674