#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2223373.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_2223373 loop_ _publ_author_name 'Saeed, Aamer' 'Khera, Rasheed Ahmad' 'Rafique, Hummera' 'Simpson, Jim' 'Stanley, Roderick G.' _publ_section_title ; 2,4-Dichloro-N-p-tolylbenzamide ; _journal_coeditor_code FL2252 _journal_issue 10 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o2527 _journal_volume 65 _journal_year 2009 _chemical_formula_iupac 'C14 H11 Cl2 N O' _chemical_formula_moiety 'C14 H11 Cl2 N O' _chemical_formula_sum 'C14 H11 Cl2 N O' _chemical_formula_weight 280.14 _chemical_name_systematic ; 2,4-Dichloro-N-p-tolylbenzamide ; _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 _cell_angle_alpha 90.00 _cell_angle_beta 94.208(9) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.0884(18) _cell_length_b 9.825(2) _cell_length_c 14.167(3) _cell_measurement_reflns_used 5859 _cell_measurement_temperature 89(2) _cell_measurement_theta_max 33.00 _cell_measurement_theta_min 2.52 _cell_volume 1261.6(4) _computing_cell_refinement 'APEX2 and SAINT (Bruker, 2006)' _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_data_reduction 'SAINT (Bruker, 2006)' _computing_molecular_graphics ; SHELXTL (Sheldrick, 2008) and Mercury (Macrae et al., 2006) ; _computing_publication_material ; SHELXL97 (Sheldrick, 2008), enCIFer (Allen et al., 2004), PLATON (Spek, 2009) and publCIF (Westrip, 2009) ; _computing_structure_refinement ; SHELXL97 (Sheldrick, 2008) and TITAN2000 (Hunter & Simpson, 1999) ; _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 89(2) _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.929 _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method \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 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 20982 _diffrn_reflns_theta_full 31.50 _diffrn_reflns_theta_max 33.12 _diffrn_reflns_theta_min 2.88 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.500 _exptl_absorpt_correction_T_max 0.970 _exptl_absorpt_correction_T_min 0.753 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2006)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'irregular fragment' _exptl_crystal_F_000 576 _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.06 _refine_diff_density_max 0.569 _refine_diff_density_min -0.485 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 167 _refine_ls_number_reflns 4465 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.149 _refine_ls_R_factor_all 0.0600 _refine_ls_R_factor_gt 0.0411 _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^)+(0.0688P)^2^+0.2064P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1146 _refine_ls_wR_factor_ref 0.1319 _reflns_number_gt 3463 _reflns_number_total 4465 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file fl2252.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_database_code 2223373 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 C C1 0.52742(16) 0.71474(14) 0.71812(10) 0.0111(3) Uani d . 1 C C2 0.43510(16) 0.67111(13) 0.63071(10) 0.0105(3) Uani d . 1 C C3 0.29263(16) 0.61878(14) 0.63334(10) 0.0121(3) Uani d . 1 C C4 0.21096(16) 0.57806(14) 0.55106(10) 0.0126(3) Uani d . 1 H H4 0.1147 0.5414 0.5539 0.015 Uiso calc R 1 C C5 0.27317(16) 0.59219(14) 0.46479(10) 0.0125(3) Uani d . 1 C C6 0.41328(16) 0.64737(14) 0.45883(10) 0.0130(3) Uani d . 1 H H6 0.4536 0.6584 0.3993 0.016 Uiso calc R 1 C C7 0.49281(16) 0.68595(14) 0.54224(11) 0.0125(3) Uani d . 1 H H7 0.5887 0.7233 0.5391 0.015 Uiso calc R 1 C C8 0.66786(16) 0.62192(14) 0.86070(10) 0.0109(3) Uani d . 1 C C9 0.77909(17) 0.71922(15) 0.87165(11) 0.0141(3) Uani d . 1 H H9 0.7902 0.7855 0.8239 0.017 Uiso calc R 1 C C10 0.87396(17) 0.71820(15) 0.95361(11) 0.0153(3) Uani d . 1 H H10 0.9498 0.7847 0.9607 0.018 Uiso calc R 1 C C11 0.86130(16) 0.62256(14) 1.02572(11) 0.0131(3) Uani d . 1 C C12 0.74965(17) 0.52520(15) 1.01274(11) 0.0142(3) Uani d . 1 H H12 0.7388 0.4585 1.0603 0.017 Uiso calc R 1 C C13 0.65393(16) 0.52412(14) 0.93137(10) 0.0123(3) Uani d . 1 H H13 0.5789 0.4568 0.9238 0.015 Uiso calc R 1 C C14 0.96308(18) 0.62590(17) 1.11523(11) 0.0184(3) Uani d . 1 H H14A 0.9120 0.6683 1.1662 0.028 Uiso calc R 1 H H14B 1.0515 0.6788 1.1040 0.028 Uiso calc R 1 H H14C 0.9916 0.5328 1.1334 0.028 Uiso calc R 1 N N1 0.56897(14) 0.61267(12) 0.77821(9) 0.0120(2) Uani d . 1 O O1 0.56444(13) 0.83472(10) 0.72985(8) 0.0168(2) Uani d . 1 Cl Cl1 0.20933(4) 0.60815(4) 0.73967(3) 0.01815(11) Uani d . 1 Cl Cl2 0.17246(4) 0.53821(4) 0.36221(3) 0.01910(11) Uani d . 1 H H1N 0.530(2) 0.534(2) 0.7672(16) 0.023 Uiso d . 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 C1 0.0116(6) 0.0104(6) 0.0112(6) 0.0005(5) 0.0004(5) 0.0007(5) C2 0.0122(6) 0.0073(6) 0.0117(6) 0.0008(4) -0.0010(5) 0.0009(4) C3 0.0135(6) 0.0120(6) 0.0107(6) 0.0020(5) 0.0011(5) 0.0023(5) C4 0.0108(6) 0.0127(6) 0.0141(7) -0.0008(5) -0.0005(5) 0.0009(5) C5 0.0145(6) 0.0111(6) 0.0115(6) 0.0015(5) -0.0020(5) -0.0012(5) C6 0.0154(6) 0.0114(6) 0.0123(6) 0.0003(5) 0.0022(5) 0.0005(5) C7 0.0127(6) 0.0095(6) 0.0153(7) -0.0011(5) 0.0005(5) 0.0005(5) C8 0.0121(6) 0.0091(6) 0.0112(6) 0.0016(4) -0.0006(5) -0.0013(4) C9 0.0154(6) 0.0127(6) 0.0137(6) -0.0026(5) -0.0014(5) 0.0035(5) C10 0.0141(7) 0.0134(6) 0.0179(7) -0.0031(5) -0.0015(6) 0.0003(5) C11 0.0117(6) 0.0141(6) 0.0133(6) 0.0011(5) -0.0008(5) -0.0002(5) C12 0.0166(7) 0.0131(6) 0.0125(6) -0.0014(5) -0.0008(5) 0.0026(5) C13 0.0130(6) 0.0103(6) 0.0134(6) -0.0019(5) -0.0001(5) 0.0005(5) C14 0.0182(7) 0.0217(7) 0.0145(7) -0.0031(6) -0.0037(6) 0.0012(6) N1 0.0154(6) 0.0084(5) 0.0115(6) -0.0014(4) -0.0034(5) 0.0006(4) O1 0.0210(6) 0.0084(5) 0.0199(5) -0.0009(4) -0.0056(4) 0.0009(4) Cl1 0.01473(18) 0.0284(2) 0.01157(18) 0.00040(13) 0.00261(13) 0.00371(13) Cl2 0.01772(19) 0.0254(2) 0.01362(18) -0.00149(13) -0.00263(14) -0.00494(13) 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 O1 C1 N1 124.29(13) O1 C1 C2 120.84(12) N1 C1 C2 114.82(12) C3 C2 C7 118.10(13) C3 C2 C1 122.99(13) C7 C2 C1 118.90(13) C4 C3 C2 121.42(14) C4 C3 Cl1 117.94(12) C2 C3 Cl1 120.61(11) C5 C4 C3 118.71(14) C5 C4 H4 120.6 C3 C4 H4 120.6 C4 C5 C6 121.66(13) C4 C5 Cl2 118.69(11) C6 C5 Cl2 119.65(12) C7 C6 C5 118.36(14) C7 C6 H6 120.8 C5 C6 H6 120.8 C6 C7 C2 121.72(13) C6 C7 H7 119.1 C2 C7 H7 119.1 C9 C8 C13 119.66(13) C9 C8 N1 123.01(13) C13 C8 N1 117.28(12) C8 C9 C10 119.17(13) C8 C9 H9 120.4 C10 C9 H9 120.4 C9 C10 C11 122.27(14) C9 C10 H10 118.9 C11 C10 H10 118.9 C12 C11 C10 117.50(13) C12 C11 C14 121.22(14) C10 C11 C14 121.27(13) C13 C12 C11 121.19(14) C13 C12 H12 119.4 C11 C12 H12 119.4 C12 C13 C8 120.20(13) C12 C13 H13 119.9 C8 C13 H13 119.9 C11 C14 H14A 109.5 C11 C14 H14B 109.5 H14A C14 H14B 109.5 C11 C14 H14C 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 C1 N1 C8 126.87(12) C1 N1 H1N 117.5(14) C8 N1 H1N 115.6(14) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 O1 1.2338(17) C1 N1 1.3512(18) C1 C2 1.5062(19) C2 C3 1.396(2) C2 C7 1.401(2) C3 C4 1.394(2) C3 Cl1 1.7379(16) C4 C5 1.391(2) C4 H4 0.9500 C5 C6 1.392(2) C5 Cl2 1.7423(15) C6 C7 1.392(2) C6 H6 0.9500 C7 H7 0.9500 C8 C9 1.392(2) C8 C13 1.400(2) C8 N1 1.4240(18) C9 C10 1.395(2) C9 H9 0.9500 C10 C11 1.399(2) C10 H10 0.9500 C11 C12 1.397(2) C11 C14 1.514(2) C12 C13 1.392(2) C12 H12 0.9500 C13 H13 0.9500 C14 H14A 0.9800 C14 H14B 0.9800 C14 H14C 0.9800 N1 H1N 0.86(2) 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 N1 H1N O1 2_646 0.86(2) 2.14(2) 2.9867(17) 168(2) C12 H12 Cl1 3_667 0.95 2.91 3.7372(17) 145.8 C6 H6 O1 4_575 0.95 2.67 3.619(2) 174.8 C7 H7 Cg2 4_576 0.95 2.65 3.4865(17) 147 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 O1 C1 C2 C3 -115.79(17) N1 C1 C2 C3 66.64(18) O1 C1 C2 C7 62.85(19) N1 C1 C2 C7 -114.72(15) C7 C2 C3 C4 2.0(2) C1 C2 C3 C4 -179.31(13) C7 C2 C3 Cl1 -175.69(10) C1 C2 C3 Cl1 2.96(19) C2 C3 C4 C5 -0.9(2) Cl1 C3 C4 C5 176.86(11) C3 C4 C5 C6 -0.9(2) C3 C4 C5 Cl2 178.77(11) C4 C5 C6 C7 1.5(2) Cl2 C5 C6 C7 -178.17(11) C5 C6 C7 C2 -0.3(2) C3 C2 C7 C6 -1.4(2) C1 C2 C7 C6 179.87(12) C13 C8 C9 C10 -0.6(2) N1 C8 C9 C10 -178.01(14) C8 C9 C10 C11 -0.1(2) C9 C10 C11 C12 0.6(2) C9 C10 C11 C14 -178.33(15) C10 C11 C12 C13 -0.5(2) C14 C11 C12 C13 178.50(14) C11 C12 C13 C8 -0.2(2) C9 C8 C13 C12 0.8(2) N1 C8 C13 C12 178.32(13) O1 C1 N1 C8 -4.3(2) C2 C1 N1 C8 173.21(13) C9 C8 N1 C1 -26.7(2) C13 C8 N1 C1 155.92(15)