#------------------------------------------------------------------------------ #$Date: 2025-08-19 12:52:15 +0100 (Tue, 19 Aug 2025) $ #$Revision: 301804 $ #$URL: svn://www.crystallography.net/cod/cif/2/21/43/2214307.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_2214307 loop_ _publ_author_name 'Kwak, Han' 'Kim, Sea-Hyun' 'Kim, Pan-Gi' 'Kim, Cheal' 'Kim, Youngmee' _publ_section_title ; N,N'-(4,5-Dichloro-o-phenylene)dibenzamide ; _journal_coeditor_code LH2410 _journal_issue 7 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o3141 _journal_page_last o3141 _journal_paper_doi 10.1107/S160053680702733X _journal_volume 63 _journal_year 2007 _chemical_formula_iupac 'C20 H14 Cl2 N2 O2' _chemical_formula_moiety 'C20 H14 Cl2 N2 O2' _chemical_formula_sum 'C20 H14 Cl2 N2 O2' _chemical_formula_weight 385.23 _chemical_name_systematic ; N,N'-(4,5-Dichloro-o-phenylene)dibenzamide ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXTL _cell_angle_alpha 90.00 _cell_angle_beta 102.630(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 8.3024(8) _cell_length_b 11.8571(11) _cell_length_c 18.7334(18) _cell_measurement_reflns_used 986 _cell_measurement_temperature 288(2) _cell_measurement_theta_max 18.83 _cell_measurement_theta_min 2.23 _cell_volume 1799.5(3) _computing_cell_refinement 'SAINT (Bruker, 1997)' _computing_data_collection 'SMART (Bruker, 1997)' _computing_data_reduction SAINT _computing_molecular_graphics 'SHELXTL (Bruker, 1998)' _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 288(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method '\f and \w' _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 0.0478 _diffrn_reflns_av_sigmaI/netI 0.0863 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 9881 _diffrn_reflns_theta_full 25.98 _diffrn_reflns_theta_max 25.98 _diffrn_reflns_theta_min 2.05 _exptl_absorpt_coefficient_mu 0.378 _exptl_absorpt_correction_T_max 0.989 _exptl_absorpt_correction_T_min 0.986 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 1997)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_description rod _exptl_crystal_F_000 792 _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.157 _refine_diff_density_min -0.193 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 243 _refine_ls_number_reflns 3518 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.002 _refine_ls_R_factor_all 0.1052 _refine_ls_R_factor_gt 0.0485 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0183P)^2^+0.2774P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0974 _refine_ls_wR_factor_ref 0.1144 _reflns_number_gt 1936 _reflns_number_total 3518 _reflns_threshold_expression I>2\s(I) _cod_data_source_file lh2410.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' 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 'Monoclinic' changed to 'monoclinic' 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_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2214307 _cod_database_fobs_code 2214307 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy Cl Cl1 0.28862(10) 1.37684(6) 1.07001(5) 0.0748(3) Uani d . 1 Cl Cl2 0.00258(11) 1.37867(6) 0.92701(5) 0.0839(3) Uani d . 1 N N1 0.3210(3) 0.95030(19) 1.04178(14) 0.0450(6) Uani d . 1 H H1N 0.345(3) 0.906(2) 1.0091(15) 0.047(8) Uiso d . 1 N N2 0.0736(3) 0.95613(18) 0.90593(12) 0.0415(6) Uani d . 1 H H2N -0.029(4) 0.962(2) 0.8863(16) 0.080(11) Uiso d . 1 O O1 0.2756(2) 0.97875(15) 1.15499(10) 0.0522(5) Uani d . 1 O O2 0.3166(2) 0.87012(16) 0.90634(11) 0.0608(6) Uani d . 1 C C1 0.4721(3) 0.7357(2) 1.09042(16) 0.0566(8) Uani d . 1 H H1 0.4859 0.7618 1.0453 0.068 Uiso calc R 1 C C2 0.5274(4) 0.6296(2) 1.11447(19) 0.0664(9) Uani d . 1 H H2 0.5786 0.5845 1.0854 0.080 Uiso calc R 1 C C3 0.5076(4) 0.5901(3) 1.18068(19) 0.0642(9) Uani d . 1 H H3 0.5452 0.5185 1.1963 0.077 Uiso calc R 1 C C4 0.4320(4) 0.6564(3) 1.22422(17) 0.0617(8) Uani d . 1 H H4 0.4183 0.6300 1.2693 0.074 Uiso calc R 1 C C5 0.3768(3) 0.7627(2) 1.19999(15) 0.0550(8) Uani d . 1 H H5 0.3258 0.8076 1.2293 0.066 Uiso calc R 1 C C6 0.3958(3) 0.8035(2) 1.13373(14) 0.0411(6) Uani d . 1 C C7 0.3283(3) 0.9185(2) 1.11169(15) 0.0422(7) Uani d . 1 C C8 0.2518(3) 1.0535(2) 1.01112(14) 0.0391(6) Uani d . 1 C C9 0.2980(3) 1.1534(2) 1.04811(15) 0.0457(7) Uani d . 1 H H9 0.3801 1.1528 1.0908 0.055 Uiso calc R 1 C C10 0.2238(3) 1.2540(2) 1.02250(15) 0.0481(7) Uani d . 1 C C11 0.1031(3) 1.2557(2) 0.95916(16) 0.0487(7) Uani d . 1 C C12 0.0627(3) 1.1572(2) 0.92025(15) 0.0461(7) Uani d . 1 H H12 -0.0140 1.1594 0.8759 0.055 Uiso calc R 1 C C13 0.1339(3) 1.0549(2) 0.94576(14) 0.0400(6) Uani d . 1 C C14 0.1654(3) 0.8714(2) 0.88694(14) 0.0433(7) Uani d . 1 C C15 0.0737(3) 0.7775(2) 0.84321(14) 0.0432(7) Uani d . 1 C C16 -0.0825(3) 0.7881(2) 0.79916(15) 0.0555(8) Uani d . 1 H H16 -0.1371 0.8570 0.7957 0.067 Uiso calc R 1 C C17 -0.1572(4) 0.6964(3) 0.76037(17) 0.0688(9) Uani d . 1 H H17 -0.2616 0.7043 0.7302 0.083 Uiso calc R 1 C C18 -0.0799(4) 0.5938(3) 0.76558(18) 0.0667(9) Uani d . 1 H H18 -0.1325 0.5320 0.7400 0.080 Uiso calc R 1 C C19 0.0747(4) 0.5828(3) 0.80849(19) 0.0678(9) Uani d . 1 H H19 0.1280 0.5134 0.8118 0.081 Uiso calc R 1 C C20 0.1520(4) 0.6736(2) 0.84674(16) 0.0588(8) Uani d . 1 H H20 0.2580 0.6654 0.8753 0.071 Uiso calc R 1 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 Cl1 0.0886(6) 0.0492(5) 0.0825(7) -0.0102(4) 0.0100(5) -0.0145(4) Cl2 0.0950(7) 0.0447(5) 0.1010(8) 0.0163(4) -0.0021(5) 0.0086(4) N1 0.0476(13) 0.0463(14) 0.0398(15) 0.0096(11) 0.0062(11) -0.0015(12) N2 0.0345(13) 0.0432(14) 0.0456(14) 0.0054(11) 0.0061(11) -0.0046(10) O1 0.0583(12) 0.0532(12) 0.0451(12) 0.0122(10) 0.0113(9) -0.0043(9) O2 0.0371(11) 0.0836(15) 0.0612(14) 0.0104(10) 0.0098(9) -0.0184(11) C1 0.0627(19) 0.0547(19) 0.055(2) 0.0142(15) 0.0176(15) 0.0111(15) C2 0.075(2) 0.0536(19) 0.072(2) 0.0180(16) 0.0178(18) -0.0005(17) C3 0.065(2) 0.0484(19) 0.075(3) 0.0049(16) 0.0065(18) 0.0147(17) C4 0.064(2) 0.065(2) 0.053(2) 0.0011(17) 0.0072(16) 0.0160(16) C5 0.0531(18) 0.064(2) 0.0459(19) 0.0053(15) 0.0075(14) 0.0056(15) C6 0.0344(14) 0.0453(16) 0.0415(17) 0.0027(12) 0.0040(12) -0.0013(13) C7 0.0342(14) 0.0461(16) 0.0429(19) 0.0006(12) 0.0011(12) -0.0009(13) C8 0.0357(14) 0.0394(16) 0.0436(16) 0.0043(12) 0.0116(12) 0.0015(12) C9 0.0382(15) 0.0507(18) 0.0468(17) -0.0040(13) 0.0064(12) -0.0026(13) C10 0.0486(16) 0.0390(16) 0.058(2) -0.0072(13) 0.0152(14) -0.0034(13) C11 0.0479(16) 0.0378(16) 0.061(2) 0.0049(13) 0.0126(14) 0.0054(14) C12 0.0410(15) 0.0490(18) 0.0465(18) 0.0026(13) 0.0058(12) 0.0087(13) C13 0.0343(14) 0.0406(16) 0.0463(17) -0.0003(12) 0.0115(12) 0.0020(13) C14 0.0414(17) 0.0494(17) 0.0402(17) 0.0047(14) 0.0113(13) 0.0040(13) C15 0.0462(15) 0.0437(16) 0.0420(17) 0.0087(13) 0.0145(13) 0.0000(13) C16 0.0533(17) 0.0503(18) 0.059(2) 0.0106(14) 0.0044(15) -0.0095(15) C17 0.0600(19) 0.074(2) 0.068(2) 0.0023(18) 0.0029(16) -0.0243(18) C18 0.080(2) 0.054(2) 0.072(2) -0.0077(18) 0.0290(19) -0.0220(17) C19 0.086(2) 0.0473(19) 0.076(2) 0.0143(18) 0.0301(19) -0.0018(17) C20 0.0610(19) 0.0539(19) 0.062(2) 0.0148(16) 0.0133(15) 0.0027(16) 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' N N 0.0061 0.0033 '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' Cl Cl 0.1484 0.1585 '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 C7 N1 C8 124.2(2) n C7 N1 H1N 123.0(17) ? C8 N1 H1N 112.3(17) ? C14 N2 C13 126.5(2) n C14 N2 H2N 121(2) ? C13 N2 H2N 112(2) ? C2 C1 C6 119.9(3) ? C2 C1 H1 120.1 ? C6 C1 H1 120.1 ? C3 C2 C1 120.7(3) ? C3 C2 H2 119.7 ? C1 C2 H2 119.7 ? C2 C3 C4 120.1(3) ? C2 C3 H3 120.0 ? C4 C3 H3 120.0 ? C3 C4 C5 119.1(3) ? C3 C4 H4 120.5 ? C5 C4 H4 120.5 ? C6 C5 C4 121.5(3) ? C6 C5 H5 119.3 ? C4 C5 H5 119.3 ? C5 C6 C1 118.8(3) ? C5 C6 C7 117.4(2) ? C1 C6 C7 123.8(3) ? O1 C7 N1 121.9(2) n O1 C7 C6 120.8(3) n N1 C7 C6 117.2(2) n C9 C8 C13 119.7(2) ? C9 C8 N1 119.5(2) n C13 C8 N1 120.8(2) n C10 C9 C8 120.8(2) ? C10 C9 H9 119.6 ? C8 C9 H9 119.6 ? C11 C10 C9 119.9(2) ? C11 C10 Cl1 121.1(2) ? C9 C10 Cl1 118.9(2) ? C10 C11 C12 119.4(2) ? C10 C11 Cl2 121.3(2) ? C12 C11 Cl2 119.3(2) ? C11 C12 C13 121.5(2) ? C11 C12 H12 119.3 ? C13 C12 H12 119.3 ? C12 C13 C8 118.6(2) ? C12 C13 N2 117.7(2) n C8 C13 N2 123.5(2) n O2 C14 N2 121.9(2) n O2 C14 C15 121.3(2) ? N2 C14 C15 116.7(2) n C16 C15 C20 118.5(3) ? C16 C15 C14 124.1(2) ? C20 C15 C14 117.4(2) ? C17 C16 C15 120.0(3) ? C17 C16 H16 120.0 ? C15 C16 H16 120.0 ? C18 C17 C16 120.9(3) ? C18 C17 H17 119.5 ? C16 C17 H17 119.5 ? C19 C18 C17 119.5(3) ? C19 C18 H18 120.2 ? C17 C18 H18 120.2 ? C18 C19 C20 120.4(3) ? C18 C19 H19 119.8 ? C20 C19 H19 119.8 ? C19 C20 C15 120.7(3) ? C19 C20 H20 119.6 ? C15 C20 H20 119.6 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Cl1 C10 1.731(3) n Cl2 C11 1.722(3) n N1 C7 1.351(3) n N1 C8 1.418(3) n N1 H1N 0.87(3) ? N2 C14 1.355(3) n N2 C13 1.419(3) n N2 H2N 0.85(3) ? O1 C7 1.231(3) n O2 C14 1.228(3) n C1 C2 1.381(4) ? C1 C6 1.389(4) ? C1 H1 0.9300 ? C2 C3 1.369(4) ? C2 H2 0.9300 ? C3 C4 1.379(4) ? C3 H3 0.9300 ? C4 C5 1.383(4) ? C4 H4 0.9300 ? C5 C6 1.373(3) ? C5 H5 0.9300 ? C6 C7 1.498(3) ? C8 C9 1.384(3) ? C8 C13 1.391(3) ? C9 C10 1.379(3) ? C9 H9 0.9300 ? C10 C11 1.376(4) ? C11 C12 1.379(3) ? C12 C13 1.388(3) ? C12 H12 0.9300 ? C14 C15 1.489(3) ? C15 C16 1.382(3) ? C15 C20 1.388(3) ? C16 C17 1.377(4) ? C16 H16 0.9300 ? C17 C18 1.369(4) ? C17 H17 0.9300 ? C18 C19 1.364(4) ? C18 H18 0.9300 ? C19 C20 1.372(4) ? C19 H19 0.9300 ? C20 H20 0.9300 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N2 H2N O1 3_577 0.85(3) 2.15(3) 2.976(3) 165(3) C5 H5 O1 . 0.93 2.44 2.769(3) 100.5 N1 H1N O2 . 0.87(3) 1.93(3) 2.702(3) 147(2) loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion C6 C1 C2 C3 0.1(5) C1 C2 C3 C4 -0.1(5) C2 C3 C4 C5 0.0(5) C3 C4 C5 C6 0.0(4) C4 C5 C6 C1 0.0(4) C4 C5 C6 C7 178.6(2) C2 C1 C6 C5 -0.1(4) C2 C1 C6 C7 -178.6(2) C8 N1 C7 O1 -0.7(4) C8 N1 C7 C6 176.2(2) C5 C6 C7 O1 8.2(4) C1 C6 C7 O1 -173.3(3) C5 C6 C7 N1 -168.7(2) C1 C6 C7 N1 9.8(4) C7 N1 C8 C9 49.1(4) C7 N1 C8 C13 -128.6(3) C13 C8 C9 C10 2.6(4) N1 C8 C9 C10 -175.1(2) C8 C9 C10 C11 -0.5(4) C8 C9 C10 Cl1 -178.9(2) C9 C10 C11 C12 -2.8(4) Cl1 C10 C11 C12 175.6(2) C9 C10 C11 Cl2 177.8(2) Cl1 C10 C11 Cl2 -3.8(4) C10 C11 C12 C13 3.9(4) Cl2 C11 C12 C13 -176.6(2) C11 C12 C13 C8 -1.8(4) C11 C12 C13 N2 174.0(2) C9 C8 C13 C12 -1.5(4) N1 C8 C13 C12 176.2(2) C9 C8 C13 N2 -177.0(2) N1 C8 C13 N2 0.7(4) C14 N2 C13 C12 134.9(3) C14 N2 C13 C8 -49.5(4) C13 N2 C14 O2 3.5(4) C13 N2 C14 C15 -178.4(2) O2 C14 C15 C16 -157.0(3) N2 C14 C15 C16 24.9(4) O2 C14 C15 C20 22.3(4) N2 C14 C15 C20 -155.8(2) C20 C15 C16 C17 0.4(4) C14 C15 C16 C17 179.7(3) C15 C16 C17 C18 1.0(5) C16 C17 C18 C19 -1.5(5) C17 C18 C19 C20 0.6(5) C18 C19 C20 C15 0.8(5) C16 C15 C20 C19 -1.3(4) C14 C15 C20 C19 179.4(3) loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 ChemSpider 21124135 2 PubChem 139072507