#------------------------------------------------------------------------------ #$Date: 2011-09-28 17:24:46 +0300 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/22/93/2229361.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_2229361 loop_ _publ_author_name 'Saraswathi, B. S.' 'Foro, Sabine' 'Gowda, B. Thimme' _publ_section_title ; N,N'-Bis(2-methylphenyl)succinamide ; _journal_coeditor_code DS2092 _journal_issue 3 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o607 _journal_volume 67 _journal_year 2011 _chemical_formula_iupac 'C18 H20 N2 O2' _chemical_formula_moiety 'C18 H20 N2 O2' _chemical_formula_sum 'C18 H20 N2 O2' _chemical_formula_weight 296.36 _chemical_name_systematic ; N,N'-Bis(2-methylphenyl)succinamide ; _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 SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 101.97(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 11.586(2) _cell_length_b 7.9550(10) _cell_length_c 8.8030(10) _cell_measurement_reflns_used 887 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.61 _cell_measurement_theta_min 2.56 _cell_volume 793.7(2) _computing_cell_refinement ; CrysAlis RED (Oxford Diffraction, 2009) ; _computing_data_collection ; CrysAlis CCD (Oxford Diffraction, 2009) ; _computing_data_reduction ; CrysAlis RED (Oxford Diffraction, 2009) ; _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'SHELXL97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur diffractometer with a Sapphire CCD detector ; _diffrn_measurement_method ; Rotation method data acquisition using \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 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0557 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_number 3109 _diffrn_reflns_theta_full 26.37 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 3.13 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_T_max 0.9976 _exptl_absorpt_correction_T_min 0.9681 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlis RED; Oxford Diffraction, 2009) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.240 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 316 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.188 _refine_diff_density_min -0.210 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 104 _refine_ls_number_reflns 1615 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 0.969 _refine_ls_R_factor_all 0.1202 _refine_ls_R_factor_gt 0.0656 _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^+0.5489P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1345 _refine_ls_wR_factor_ref 0.1626 _reflns_number_gt 987 _reflns_number_total 1615 _reflns_threshold_expression I>2sigma(I) _[local]_cod_data_source_file ds2092.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_original_cell_volume 793.70(19) _cod_database_code 2229361 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 _atom_site_disorder_assembly _atom_site_disorder_group C C1 0.2287(2) 0.4159(3) 0.4527(3) 0.0332(6) Uani d . 1 . . C C2 0.3283(2) 0.3765(4) 0.3956(3) 0.0375(7) Uani d . 1 . . C C3 0.3804(3) 0.5058(4) 0.3267(4) 0.0509(8) Uani d . 1 . . H H3 0.4469 0.4828 0.2866 0.061 Uiso calc R 1 . . C C4 0.3357(3) 0.6671(4) 0.3168(4) 0.0572(9) Uani d . 1 . . H H4 0.3712 0.7505 0.2682 0.069 Uiso calc R 1 . . C C5 0.2395(3) 0.7053(4) 0.3778(4) 0.0544(9) Uani d . 1 . . H H5 0.2106 0.8147 0.3732 0.065 Uiso calc R 1 . . C C6 0.1859(3) 0.5800(4) 0.4459(4) 0.0468(8) Uani d . 1 . . H H6 0.1206 0.6051 0.4879 0.056 Uiso calc R 1 . . C C7 0.1138(2) 0.1563(3) 0.4500(3) 0.0299(6) Uani d . 1 . . C C8 0.0525(2) 0.0450(4) 0.5479(3) 0.0356(7) Uani d . 1 . . H H8A 0.1082 -0.0375 0.6013 0.043 Uiso calc R 1 . . H H8B 0.0266 0.1130 0.6259 0.043 Uiso calc R 1 . . C C9 0.3816(3) 0.2030(4) 0.4074(4) 0.0540(9) Uani d . 1 . . H H9A 0.3508 0.1415 0.3140 0.065 Uiso calc R 1 . . H H9B 0.3622 0.1452 0.4946 0.065 Uiso calc R 1 . . H H9C 0.4658 0.2118 0.4212 0.065 Uiso calc R 1 . . N N1 0.1685(2) 0.2917(3) 0.5239(2) 0.0355(6) Uani d D 1 . . H H1N 0.155(2) 0.310(3) 0.614(2) 0.043 Uiso d D 1 . . O O1 0.11453(17) 0.1214(2) 0.31422(19) 0.0414(6) Uani 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 0.0376(14) 0.0357(16) 0.0271(13) -0.0083(12) 0.0085(11) -0.0046(12) C2 0.0355(14) 0.0414(17) 0.0352(15) -0.0055(13) 0.0065(12) -0.0030(13) C3 0.0444(17) 0.061(2) 0.0507(19) -0.0170(17) 0.0179(15) 0.0004(17) C4 0.068(2) 0.047(2) 0.057(2) -0.0246(17) 0.0158(17) 0.0051(17) C5 0.070(2) 0.0332(18) 0.062(2) -0.0114(16) 0.0176(18) -0.0029(16) C6 0.0522(18) 0.0400(18) 0.0511(19) -0.0041(14) 0.0171(15) -0.0092(15) C7 0.0344(14) 0.0312(14) 0.0249(13) -0.0012(12) 0.0078(10) 0.0012(12) C8 0.0444(16) 0.0378(16) 0.0259(14) -0.0092(12) 0.0105(12) 0.0028(12) C9 0.0439(17) 0.058(2) 0.062(2) 0.0057(16) 0.0154(15) 0.0040(17) N1 0.0465(13) 0.0373(13) 0.0262(11) -0.0094(11) 0.0158(10) -0.0048(10) O1 0.0570(13) 0.0437(12) 0.0264(10) -0.0154(10) 0.0157(9) -0.0039(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' 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 C1 C6 . . 120.8(3) ? C2 C1 N1 . . 121.5(2) ? C6 C1 N1 . . 117.7(2) ? C1 C2 C3 . . 117.3(3) ? C1 C2 C9 . . 122.8(2) ? C3 C2 C9 . . 119.9(3) ? C4 C3 C2 . . 121.6(3) ? C4 C3 H3 . . 119.2 ? C2 C3 H3 . . 119.2 ? C5 C4 C3 . . 120.5(3) ? C5 C4 H4 . . 119.8 ? C3 C4 H4 . . 119.8 ? C4 C5 C6 . . 119.2(3) ? C4 C5 H5 . . 120.4 ? C6 C5 H5 . . 120.4 ? C5 C6 C1 . . 120.6(3) ? C5 C6 H6 . . 119.7 ? C1 C6 H6 . . 119.7 ? O1 C7 N1 . . 123.6(2) ? O1 C7 C8 . . 121.4(2) ? N1 C7 C8 . . 115.0(2) ? C8 C8 C7 3_556 . 112.3(3) ? C8 C8 H8A 3_556 . 109.2 ? C7 C8 H8A . . 109.2 ? C8 C8 H8B 3_556 . 109.2 ? C7 C8 H8B . . 109.2 ? H8A C8 H8B . . 107.9 ? C2 C9 H9A . . 109.5 ? C2 C9 H9B . . 109.5 ? H9A C9 H9B . . 109.5 ? C2 C9 H9C . . 109.5 ? H9A C9 H9C . . 109.5 ? H9B C9 H9C . . 109.5 ? C7 N1 C1 . . 124.5(2) ? C7 N1 H1N . . 115.1(19) ? C1 N1 H1N . . 119.6(19) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 C2 . 1.387(4) ? C1 C6 . 1.393(4) ? C1 N1 . 1.427(3) ? C2 C3 . 1.393(4) ? C2 C9 . 1.507(4) ? C3 C4 . 1.380(5) ? C3 H3 . 0.9300 ? C4 C5 . 1.368(4) ? C4 H4 . 0.9300 ? C5 C6 . 1.376(4) ? C5 H5 . 0.9300 ? C6 H6 . 0.9300 ? C7 O1 . 1.229(3) ? C7 N1 . 1.347(3) ? C7 C8 . 1.512(3) ? C8 C8 3_556 1.509(5) ? C8 H8A . 0.9700 ? C8 H8B . 0.9700 ? C9 H9A . 0.9600 ? C9 H9B . 0.9600 ? C9 H9C . 0.9600 ? N1 H1N . 0.853(17) ? 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 4_566 0.853(17) 1.991(18) 2.840(3) 173(3) 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C6 C1 C2 C3 . . . . -2.3(4) ? N1 C1 C2 C3 . . . . 179.4(2) ? C6 C1 C2 C9 . . . . 176.8(3) ? N1 C1 C2 C9 . . . . -1.5(4) ? C1 C2 C3 C4 . . . . 0.6(4) ? C9 C2 C3 C4 . . . . -178.6(3) ? C2 C3 C4 C5 . . . . 1.4(5) ? C3 C4 C5 C6 . . . . -1.6(5) ? C4 C5 C6 C1 . . . . -0.1(5) ? C2 C1 C6 C5 . . . . 2.1(4) ? N1 C1 C6 C5 . . . . -179.5(3) ? O1 C7 C8 C8 . . . 3_556 -30.5(4) ? N1 C7 C8 C8 . . . 3_556 150.9(3) ? O1 C7 N1 C1 . . . . 3.3(4) ? C8 C7 N1 C1 . . . . -178.1(2) ? C2 C1 N1 C7 . . . . -64.0(4) ? C6 C1 N1 C7 . . . . 117.6(3) ?