#------------------------------------------------------------------------------ #$Date: 2019-01-16 05:25:37 +0200 (Wed, 16 Jan 2019) $ #$Revision: 213117 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/28/2242819.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_2242819 loop_ _publ_author_name 'Anitha, Azhagan Ganapathi' 'Arunagiri, Chidambaram' 'Subashini, Annamalai' _publ_section_title ; Synthesis, X-ray crystal structure, Hirshfeld surface analysis and DFT studies of (E)-N'-(2-bromobenzylidene)-4-methylbenzohydrazide ; _journal_coeditor_code LH5887 _journal_issue 2 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 109 _journal_page_last 114 _journal_paper_doi 10.1107/S2056989018017978 _journal_volume 75 _journal_year 2019 _chemical_formula_iupac 'C15 H13 Br N2 O' _chemical_formula_moiety 'C15 H13 Br N2 O' _chemical_formula_sum 'C15 H13 Br N2 O' _chemical_formula_weight 317.18 _chemical_name_common ; (E)-N'-(2-Bromobenzylidene)-4-methylbenzohydrazide ; _chemical_name_systematic ; (E)-4-Methyl-N'-(2-bromobenzylidene)benzohydrazide ; _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' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 9.6002(10) _cell_length_b 11.5584(13) _cell_length_c 12.5823(12) _cell_measurement_reflns_used 6594 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 26.00 _cell_measurement_theta_min 2.39 _cell_volume 1396.2(3) _computing_cell_refinement ; APEX2 and SAINT (Bruker, 2004) ; _computing_data_collection ; APEX2 (Bruker, 2004) ; _computing_data_reduction ; SAINT and XPREP (Bruker, 2004) ; _computing_molecular_graphics ; ORTEP3 for Windows (Farrugia, 2012) ; _computing_publication_material ; SHELXL2014 (Sheldrick, 2015) ; _computing_structure_refinement ; SHELXL014 (Sheldrick, 2015) ; _computing_structure_solution ; SIR97 (Altomare et al., 1999) ; _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker Kappa APEXII CCD' _diffrn_measurement_method '\w and \f scan' _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 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 17816 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 2.39 _exptl_absorpt_coefficient_mu 2.937 _exptl_absorpt_correction_T_max 0.5911 _exptl_absorpt_correction_T_min 0.4728 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2004) ; _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 640 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.424 _refine_diff_density_min -0.468 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 176 _refine_ls_number_reflns 2744 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.094 _refine_ls_R_factor_all 0.0763 _refine_ls_R_factor_gt 0.0365 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0208P)^2^+2.2419P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0723 _refine_ls_wR_factor_ref 0.0974 _reflns_number_gt 1837 _reflns_number_total 2744 _reflns_threshold_expression >2sigma(I) _iucr_refine_instructions_details ; TITL 3 in Pna21 CELL 0.71073 9.6002 11.5584 12.5823 90.000 90.000 90.000 ZERR 4.00 0.0010 0.0013 0.0012 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, Z SYMM 1/2 - X, 1/2 + Y, 1/2 + Z SFAC C H N O BR UNIT 60 52 8 4 4 MERG 2 OMIT -3.00 52.00 EQIV $1 x-1/2, -y-1/2, z HTAB C9 O1_$1 HTAB N1 O1_$1 dfix 0.85 0.02 n1 h1 FMAP 2 PLAN 20 SIZE 0.20 0.25 0.30 ACTA BOND BOND $H CONF L.S. 10 TEMP 23.00 WGHT 0.020600 2.252200 FVAR 0.61843 BR1 5 0.274121 0.498464 0.502668 11.00000 0.06728 0.06244 = 0.06693 -0.00059 0.01179 0.00559 O1 4 0.780729 0.196103 0.204825 11.00000 0.03006 0.11118 = 0.04875 0.00144 -0.00694 0.00633 N1 3 0.564264 0.264149 0.233714 11.00000 0.03347 0.06073 = 0.03469 -0.00293 -0.00906 -0.00059 N2 3 0.596509 0.292460 0.337283 11.00000 0.04547 0.05825 = 0.03547 -0.00156 -0.00866 -0.00031 C1 1 0.617398 0.174966 0.064946 11.00000 0.03501 0.04901 = 0.03299 0.00302 0.00080 -0.00418 C2 1 0.688602 0.084642 0.019135 11.00000 0.04598 0.05807 = 0.05476 0.00582 0.00325 0.01050 AFIX 43 H2 2 0.763162 0.051383 0.055099 11.00000 -1.20000 AFIX 0 C3 1 0.651200 0.042731 -0.079108 11.00000 0.06723 0.05935 = 0.06316 -0.00776 0.00848 0.00217 AFIX 43 H3 2 0.700012 -0.019254 -0.107986 11.00000 -1.20000 AFIX 0 C4 1 0.543296 0.090660 -0.135221 11.00000 0.06058 0.06181 = 0.04134 -0.00659 0.00502 -0.01257 C5 1 0.472133 0.182701 -0.090154 11.00000 0.05174 0.06562 = 0.04031 -0.00055 -0.01318 -0.00115 AFIX 43 H5 2 0.398738 0.216505 -0.127072 11.00000 -1.20000 AFIX 0 C6 1 0.508455 0.225147 0.008855 11.00000 0.03786 0.05477 = 0.04120 -0.00315 -0.00511 0.00257 AFIX 43 H6 2 0.459943 0.287244 0.037823 11.00000 -1.20000 AFIX 0 C7 1 0.499833 0.044732 -0.242425 11.00000 0.09740 0.09490 = 0.05783 -0.02064 -0.00893 -0.01613 AFIX 33 H7C 2 0.422960 0.089378 -0.268863 11.00000 -1.50000 H7A 2 0.472252 -0.034758 -0.235618 11.00000 -1.50000 H7B 2 0.576628 0.050346 -0.291021 11.00000 -1.50000 AFIX 0 C8 1 0.662093 0.213005 0.172416 11.00000 0.02907 0.05941 = 0.04013 0.00790 0.00008 -0.00283 C9 1 0.496407 0.329642 0.393696 11.00000 0.04865 0.04595 = 0.03905 -0.00215 -0.01257 -0.00262 AFIX 43 H9 2 0.409252 0.341271 0.363250 11.00000 -1.20000 AFIX 0 C10 1 0.518169 0.354330 0.507133 11.00000 0.05724 0.04052 = 0.03273 -0.00188 -0.00629 -0.00787 C11 1 0.429026 0.423635 0.565113 11.00000 0.07010 0.04542 = 0.04342 -0.00212 -0.00039 -0.01429 C12 1 0.451417 0.441890 0.672564 11.00000 0.11620 0.05939 = 0.04223 -0.00578 0.01569 -0.02056 AFIX 43 H12 2 0.390833 0.488245 0.711462 11.00000 -1.20000 AFIX 0 C13 1 0.564211 0.390783 0.721305 11.00000 0.15199 0.05931 = 0.03437 -0.00272 -0.02079 -0.03045 AFIX 43 H13 2 0.580658 0.403868 0.793147 11.00000 -1.20000 AFIX 0 C14 1 0.650389 0.322359 0.665953 11.00000 0.11709 0.08219 = 0.04951 0.00163 -0.04257 -0.00059 AFIX 43 H14 2 0.723854 0.285685 0.700395 11.00000 -1.20000 AFIX 0 C15 1 0.631343 0.305892 0.559116 11.00000 0.07537 0.05396 = 0.05297 0.00295 -0.01965 -0.00186 AFIX 43 H15 2 0.695074 0.261707 0.521021 11.00000 -1.20000 AFIX 0 H1 2 0.480097 0.267763 0.216704 11.00000 0.05068 HKLF 4 REM 3 in Pna21 REM R1 = 0.0365 for 1837 Fo > 4sig(Fo) and 0.0763 for all 2744 data REM 176 parameters refined using 2 restraints END WGHT 0.0205 2.2518 REM Highest difference peak 0.424, deepest hole -0.468, 1-sigma level 0.074 Q1 1 0.3981 0.2947 -0.1579 11.00000 0.05 0.42 Q2 1 0.2480 0.4218 0.4918 11.00000 0.05 0.35 Q3 1 0.4218 0.2609 -0.2687 11.00000 0.05 0.35 Q4 1 0.8412 0.2908 0.6773 11.00000 0.05 0.32 Q5 1 0.2285 0.4347 0.4699 11.00000 0.05 0.31 Q6 1 0.4093 0.0207 -0.2198 11.00000 0.05 0.30 Q7 1 0.4800 0.3594 0.0115 11.00000 0.05 0.30 Q8 1 0.1736 0.4915 0.5051 11.00000 0.05 0.29 Q9 1 0.4512 0.5590 0.6769 11.00000 0.05 0.27 Q10 1 0.5808 -0.0151 -0.2752 11.00000 0.05 0.26 Q11 1 0.4846 0.1330 -0.4205 11.00000 0.05 0.26 Q12 1 0.4045 0.3068 0.1717 11.00000 0.05 0.25 Q13 1 0.6256 -0.1413 -0.1161 11.00000 0.05 0.25 Q14 1 0.4370 0.5727 0.5767 11.00000 0.05 0.24 Q15 1 0.3628 0.5802 0.5019 11.00000 0.05 0.24 Q16 1 0.5054 0.3333 0.8960 11.00000 0.05 0.24 Q17 1 0.7553 0.0433 0.2341 11.00000 0.05 0.23 Q18 1 0.4605 0.1743 0.2039 11.00000 0.05 0.23 Q19 1 0.8698 0.1115 0.0156 11.00000 0.05 0.23 Q20 1 0.4088 0.2948 0.0718 11.00000 0.05 0.23 ; _cod_data_source_file lh5887sup1.cif _cod_data_source_block I _cod_database_code 2242819 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_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 _atom_site_symmetry_multiplicity Br Br1 0.27412(5) 0.49846(5) 0.50267(12) 0.06555(18) Uani d . 1 1 O O1 0.7807(3) 0.1961(4) 0.2048(3) 0.0633(11) Uani d . 1 1 N N1 0.5643(4) 0.2641(4) 0.2337(3) 0.0430(10) Uani d D 1 1 N N2 0.5965(5) 0.2925(4) 0.3373(3) 0.0464(11) Uani d . 1 1 C C1 0.6174(5) 0.1750(4) 0.0649(3) 0.0390(10) Uani d . 1 1 C C2 0.6886(5) 0.0846(4) 0.0191(5) 0.0529(14) Uani d . 1 1 H H2 0.7632 0.0514 0.0551 0.064 Uiso calc R 1 1 C C3 0.6512(7) 0.0427(5) -0.0791(5) 0.0632(15) Uani d . 1 1 H H3 0.7000 -0.0193 -0.1080 0.076 Uiso calc R 1 1 C C4 0.5433(6) 0.0907(5) -0.1352(4) 0.0546(14) Uani d . 1 1 C C5 0.4721(6) 0.1827(5) -0.0902(4) 0.0526(13) Uani d . 1 1 H H5 0.3987 0.2165 -0.1271 0.063 Uiso calc R 1 1 C C6 0.5085(4) 0.2251(4) 0.0089(5) 0.0446(10) Uani d . 1 1 H H6 0.4599 0.2872 0.0378 0.054 Uiso calc R 1 1 C C7 0.4998(11) 0.0447(6) -0.2424(6) 0.0834(19) Uani d . 1 1 H H7C 0.4230 0.0894 -0.2689 0.125 Uiso calc R 1 1 H H7A 0.4723 -0.0348 -0.2356 0.125 Uiso calc R 1 1 H H7B 0.5766 0.0503 -0.2910 0.125 Uiso calc R 1 1 C C8 0.6621(5) 0.2130(4) 0.1724(4) 0.0429(11) Uani d . 1 1 C C9 0.4964(5) 0.3296(4) 0.3937(4) 0.0446(12) Uani d . 1 1 H H9 0.4093 0.3413 0.3632 0.053 Uiso calc R 1 1 C C10 0.5182(5) 0.3543(3) 0.5071(5) 0.0435(10) Uani d . 1 1 C C11 0.4290(6) 0.4236(4) 0.5651(4) 0.0530(13) Uani d . 1 1 C C12 0.4514(8) 0.4419(5) 0.6726(4) 0.0726(19) Uani d . 1 1 H H12 0.3908 0.4882 0.7115 0.087 Uiso calc R 1 1 C C13 0.5642(9) 0.3908(6) 0.7213(5) 0.082(2) Uani d . 1 1 H H13 0.5807 0.4039 0.7931 0.098 Uiso calc R 1 1 C C14 0.6504(9) 0.3224(6) 0.6660(5) 0.083(2) Uani d . 1 1 H H14 0.7239 0.2857 0.7004 0.100 Uiso calc R 1 1 C C15 0.6313(7) 0.3059(5) 0.5591(4) 0.0608(15) Uani d . 1 1 H H15 0.6951 0.2617 0.5210 0.073 Uiso calc R 1 1 H H1 0.480(3) 0.268(5) 0.217(4) 0.051(16) Uiso d D 1 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 Br1 0.0673(3) 0.0624(3) 0.0669(3) 0.0056(3) 0.0118(6) -0.0006(3) O1 0.0301(18) 0.111(3) 0.049(2) 0.006(2) -0.0069(16) 0.001(2) N1 0.033(2) 0.061(3) 0.035(2) -0.001(2) -0.0091(19) -0.003(2) N2 0.045(3) 0.058(3) 0.035(2) 0.000(2) -0.009(2) -0.002(2) C1 0.035(2) 0.049(3) 0.033(2) -0.004(2) 0.001(2) 0.003(2) C2 0.046(3) 0.058(3) 0.055(4) 0.011(2) 0.003(3) 0.006(3) C3 0.067(4) 0.059(3) 0.063(4) 0.002(3) 0.008(3) -0.008(3) C4 0.061(3) 0.062(3) 0.041(3) -0.013(3) 0.005(3) -0.007(3) C5 0.052(3) 0.066(3) 0.040(3) -0.001(3) -0.013(2) -0.001(3) C6 0.038(2) 0.055(3) 0.041(2) 0.0026(19) -0.005(3) -0.003(3) C7 0.097(4) 0.095(5) 0.058(3) -0.016(6) -0.009(3) -0.021(5) C8 0.029(2) 0.059(3) 0.040(3) -0.003(2) 0.000(2) 0.008(2) C9 0.049(3) 0.046(3) 0.039(3) -0.003(2) -0.013(2) -0.002(2) C10 0.057(3) 0.041(2) 0.033(2) -0.008(2) -0.006(3) -0.002(3) C11 0.070(4) 0.045(3) 0.043(3) -0.014(3) 0.000(3) -0.002(2) C12 0.116(6) 0.059(4) 0.042(4) -0.021(4) 0.016(4) -0.006(3) C13 0.152(7) 0.059(4) 0.034(3) -0.030(4) -0.021(4) -0.003(3) C14 0.117(6) 0.082(5) 0.050(4) -0.001(5) -0.043(4) 0.002(4) C15 0.075(4) 0.054(3) 0.053(3) -0.002(3) -0.020(3) 0.003(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' 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' 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 C8 N1 N2 119.2(4) C8 N1 H1 123(4) N2 N1 H1 117(4) C9 N2 N1 116.0(4) C2 C1 C6 118.6(5) C2 C1 C8 117.6(4) C6 C1 C8 123.8(5) C1 C2 C3 121.0(5) C1 C2 H2 119.5 C3 C2 H2 119.5 C4 C3 C2 121.2(5) C4 C3 H3 119.4 C2 C3 H3 119.4 C3 C4 C5 118.2(5) C3 C4 C7 121.8(6) C5 C4 C7 120.0(6) C6 C5 C4 121.1(5) C6 C5 H5 119.5 C4 C5 H5 119.5 C5 C6 C1 120.0(5) C5 C6 H6 120.0 C1 C6 H6 120.0 C4 C7 H7C 109.5 C4 C7 H7A 109.5 H7C C7 H7A 109.5 C4 C7 H7B 109.5 H7C C7 H7B 109.5 H7A C7 H7B 109.5 O1 C8 N1 121.7(4) O1 C8 C1 121.6(4) N1 C8 C1 116.6(4) N2 C9 C10 120.1(4) N2 C9 H9 120.0 C10 C9 H9 120.0 C11 C10 C15 118.1(5) C11 C10 C9 122.5(5) C15 C10 C9 119.4(5) C10 C11 C12 120.5(6) C10 C11 Br1 122.2(4) C12 C11 Br1 117.2(5) C13 C12 C11 119.4(6) C13 C12 H12 120.3 C11 C12 H12 120.3 C14 C13 C12 120.5(6) C14 C13 H13 119.8 C12 C13 H13 119.8 C13 C14 C15 120.6(7) C13 C14 H14 119.7 C15 C14 H14 119.7 C14 C15 C10 120.8(6) C14 C15 H15 119.6 C10 C15 H15 119.6 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Br1 C11 1.891(6) O1 C8 1.225(6) N1 C8 1.351(6) N1 N2 1.379(5) N1 H1 0.837(19) N2 C9 1.270(6) C1 C2 1.375(7) C1 C6 1.389(6) C1 C8 1.485(6) C2 C3 1.375(8) C2 H2 0.9300 C3 C4 1.371(8) C3 H3 0.9300 C4 C5 1.386(7) C4 C7 1.508(9) C5 C6 1.384(8) C5 H5 0.9300 C6 H6 0.9300 C7 H7C 0.9600 C7 H7A 0.9600 C7 H7B 0.9600 C9 C10 1.470(8) C9 H9 0.9300 C10 C11 1.381(7) C10 C15 1.386(7) C11 C12 1.385(7) C12 C13 1.378(10) C12 H12 0.9300 C13 C14 1.340(10) C13 H13 0.9300 C14 C15 1.370(8) C14 H14 0.9300 C15 H15 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 N1 H1 O1 3_455 0.84(3) 1.96(3) 2.785(5) 167(5) C9 H9 O1 3_455 0.93 2.38 3.166(6) 142 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 C8 N1 N2 C9 -173.3(5) C6 C1 C2 C3 -1.5(7) C8 C1 C2 C3 178.4(5) C1 C2 C3 C4 1.0(8) C2 C3 C4 C5 -0.2(8) C2 C3 C4 C7 -179.2(6) C3 C4 C5 C6 -0.1(8) C7 C4 C5 C6 178.9(6) C4 C5 C6 C1 -0.3(8) C2 C1 C6 C5 1.1(7) C8 C1 C6 C5 -178.8(5) N2 N1 C8 O1 -3.5(7) N2 N1 C8 C1 174.6(4) C2 C1 C8 O1 24.6(7) C6 C1 C8 O1 -155.5(5) C2 C1 C8 N1 -153.6(5) C6 C1 C8 N1 26.3(7) N1 N2 C9 C10 175.7(4) N2 C9 C10 C11 161.4(5) N2 C9 C10 C15 -19.2(7) C15 C10 C11 C12 -1.2(7) C9 C10 C11 C12 178.2(5) C15 C10 C11 Br1 178.1(4) C9 C10 C11 Br1 -2.5(6) C10 C11 C12 C13 0.4(8) Br1 C11 C12 C13 -178.9(5) C11 C12 C13 C14 -1.1(10) C12 C13 C14 C15 2.8(11) C13 C14 C15 C10 -3.6(10) C11 C10 C15 C14 2.8(8) C9 C10 C15 C14 -176.6(6)