#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2224582.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_2224582 loop_ _publ_author_name 'Zhang, Li-Ping' 'Yang, Ming' 'Fang, Yun' _publ_section_title ; (Z)-3-(4-Methoxyanilino)-1-phenylbut-2-en-1-one ; _journal_coeditor_code CI2973 _journal_issue 1 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o7 _journal_volume 66 _journal_year 2010 _chemical_formula_iupac 'C17 H17 N O2' _chemical_formula_moiety 'C17 H17 N O2' _chemical_formula_sum 'C17 H17 N O2' _chemical_formula_weight 267.32 _chemical_name_systematic ; (Z)-3-(4-Methoxyanilino)-1-phenylbut-2-en-1-one ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 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 94.954(6) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 6.435(2) _cell_length_b 7.287(3) _cell_length_c 30.919(12) _cell_measurement_reflns_used 2333 _cell_measurement_temperature 294(2) _cell_measurement_theta_max 26.25 _cell_measurement_theta_min 2.64 _cell_volume 1444.4(9) _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_collection 'SMART (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 294(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker SMART CCD area-detector' _diffrn_measurement_method '\f and \w scans' _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 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_number 7729 _diffrn_reflns_theta_full 26.40 _diffrn_reflns_theta_max 26.40 _diffrn_reflns_theta_min 1.32 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7390 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.229 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 568 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _refine_diff_density_max 0.180 _refine_diff_density_min -0.166 _refine_ls_extinction_coef 0.035(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 2008)' _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 184 _refine_ls_number_reflns 2931 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.002 _refine_ls_R_factor_all 0.0802 _refine_ls_R_factor_gt 0.0459 _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^)+(0.0645P)^2^+0.2627P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1153 _refine_ls_wR_factor_ref 0.1351 _reflns_number_gt 1900 _reflns_number_total 2931 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ci2973.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/n' _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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 1444.5(9) _cod_database_code 2224582 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -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 O O1 0.0332(2) 0.1669(2) 0.45901(4) 0.0621(4) Uani d . 1 O O2 -0.17087(19) 0.1729(2) 0.20705(4) 0.0552(4) Uani d . 1 N N1 0.0723(2) 0.1693(2) 0.27987(4) 0.0417(4) Uani d . 1 H H1 -0.0489 0.1722 0.2658 0.050 Uiso calc R 1 C C1 0.0705(2) 0.1739(2) 0.32573(5) 0.0364(4) Uani d . 1 C C2 -0.0759(3) 0.2824(3) 0.34338(5) 0.0412(4) Uani d . 1 H H2 -0.1639 0.3558 0.3253 0.049 Uiso calc R 1 C C3 -0.0940(3) 0.2835(3) 0.38775(5) 0.0445(5) Uani d . 1 H H3 -0.1947 0.3560 0.3992 0.053 Uiso calc R 1 C C4 0.0378(3) 0.1768(2) 0.41473(5) 0.0423(4) Uani d . 1 C C5 0.1869(3) 0.0706(3) 0.39734(6) 0.0515(5) Uani d . 1 H H5 0.2780 0.0005 0.4156 0.062 Uiso calc R 1 C C6 0.2022(3) 0.0673(3) 0.35319(6) 0.0480(5) Uani d . 1 H H6 0.3015 -0.0069 0.3418 0.058 Uiso calc R 1 C C7 -0.1412(4) 0.2438(4) 0.47712(6) 0.0798(8) Uani d . 1 H H7A -0.1385 0.3749 0.4740 0.120 Uiso calc R 1 H H7B -0.1366 0.2126 0.5074 0.120 Uiso calc R 1 H H7C -0.2670 0.1963 0.4623 0.120 Uiso calc R 1 C C8 0.4516(3) 0.1682(3) 0.27522(6) 0.0504(5) Uani d . 1 H H8A 0.4579 0.2429 0.3009 0.076 Uiso calc R 1 H H8B 0.5399 0.2199 0.2549 0.076 Uiso calc R 1 H H8C 0.4981 0.0463 0.2828 0.076 Uiso calc R 1 C C9 0.2316(3) 0.1612(2) 0.25509(5) 0.0384(4) Uani d . 1 C C10 0.1947(3) 0.1546(2) 0.21040(5) 0.0397(4) Uani d . 1 H H10 0.3087 0.1449 0.1940 0.048 Uiso calc R 1 C C11 -0.0069(3) 0.1616(2) 0.18819(5) 0.0386(4) Uani d . 1 C C12 -0.0272(3) 0.1643(2) 0.13949(5) 0.0390(4) Uani d . 1 C C13 0.1114(3) 0.0745(3) 0.11502(5) 0.0485(5) Uani d . 1 H H13 0.2218 0.0086 0.1288 0.058 Uiso calc R 1 C C14 0.0869(3) 0.0820(3) 0.07020(6) 0.0592(6) Uani d . 1 H H14 0.1797 0.0195 0.0540 0.071 Uiso calc R 1 C C15 -0.0728(4) 0.1807(3) 0.04946(6) 0.0612(6) Uani d . 1 H H15 -0.0872 0.1869 0.0193 0.073 Uiso calc R 1 C C16 -0.2117(4) 0.2703(3) 0.07320(6) 0.0621(6) Uani d . 1 H H16 -0.3203 0.3375 0.0591 0.075 Uiso calc R 1 C C17 -0.1908(3) 0.2612(3) 0.11809(6) 0.0525(5) Uani d . 1 H H17 -0.2871 0.3205 0.1340 0.063 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 O1 0.0685(10) 0.0814(11) 0.0370(7) 0.0231(8) 0.0080(6) 0.0056(7) O2 0.0377(7) 0.0836(11) 0.0449(7) -0.0037(7) 0.0074(6) -0.0087(7) N1 0.0333(8) 0.0548(10) 0.0370(8) -0.0018(7) 0.0037(6) -0.0034(7) C1 0.0366(9) 0.0376(10) 0.0348(9) -0.0016(7) 0.0027(7) -0.0008(7) C2 0.0355(9) 0.0476(11) 0.0399(10) 0.0068(8) -0.0001(7) 0.0040(8) C3 0.0426(10) 0.0488(12) 0.0429(10) 0.0107(8) 0.0082(8) -0.0013(8) C4 0.0476(10) 0.0462(11) 0.0329(9) 0.0030(8) 0.0031(8) 0.0010(8) C5 0.0565(12) 0.0516(12) 0.0463(11) 0.0195(10) 0.0038(9) 0.0093(9) C6 0.0557(11) 0.0438(11) 0.0456(11) 0.0178(9) 0.0100(8) 0.0023(9) C7 0.0960(18) 0.102(2) 0.0442(12) 0.0378(15) 0.0206(12) 0.0024(12) C8 0.0375(10) 0.0637(13) 0.0498(11) 0.0002(9) 0.0039(8) 0.0037(9) C9 0.0368(9) 0.0355(10) 0.0434(10) -0.0023(7) 0.0066(7) 0.0012(8) C10 0.0372(9) 0.0442(11) 0.0388(9) -0.0009(8) 0.0098(7) 0.0003(8) C11 0.0404(10) 0.0363(10) 0.0398(9) -0.0036(8) 0.0082(8) -0.0024(8) C12 0.0424(10) 0.0361(10) 0.0384(9) -0.0062(8) 0.0023(7) -0.0024(8) C13 0.0552(12) 0.0484(12) 0.0425(11) 0.0028(9) 0.0071(8) -0.0012(9) C14 0.0729(14) 0.0622(14) 0.0439(11) -0.0019(11) 0.0137(10) -0.0078(10) C15 0.0862(16) 0.0605(14) 0.0358(10) -0.0136(12) -0.0008(10) -0.0006(10) C16 0.0730(14) 0.0571(14) 0.0526(12) 0.0022(11) -0.0148(10) 0.0031(10) C17 0.0555(12) 0.0505(12) 0.0505(12) 0.0040(10) -0.0016(9) -0.0073(10) 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 C4 O1 C7 117.43(15) C9 N1 C1 130.43(15) C9 N1 H1 114.8 C1 N1 H1 114.8 C2 C1 C6 118.82(15) C2 C1 N1 118.30(15) C6 C1 N1 122.79(15) C1 C2 C3 120.92(16) C1 C2 H2 119.5 C3 C2 H2 119.5 C4 C3 C2 119.71(16) C4 C3 H3 120.1 C2 C3 H3 120.1 O1 C4 C5 115.81(15) O1 C4 C3 124.58(16) C5 C4 C3 119.61(16) C6 C5 C4 120.56(17) C6 C5 H5 119.7 C4 C5 H5 119.7 C5 C6 C1 120.36(17) C5 C6 H6 119.8 C1 C6 H6 119.8 O1 C7 H7A 109.5 O1 C7 H7B 109.5 H7A C7 H7B 109.5 O1 C7 H7C 109.5 H7A C7 H7C 109.5 H7B C7 H7C 109.5 C9 C8 H8A 109.5 C9 C8 H8B 109.5 H8A C8 H8B 109.5 C9 C8 H8C 109.5 H8A C8 H8C 109.5 H8B C8 H8C 109.5 N1 C9 C10 120.13(16) N1 C9 C8 120.40(15) C10 C9 C8 119.40(15) C9 C10 C11 123.68(15) C9 C10 H10 118.2 C11 C10 H10 118.2 O2 C11 C10 123.41(16) O2 C11 C12 117.59(15) C10 C11 C12 118.94(14) C13 C12 C17 118.60(16) C13 C12 C11 122.58(16) C17 C12 C11 118.82(16) C14 C13 C12 120.45(18) C14 C13 H13 119.8 C12 C13 H13 119.8 C15 C14 C13 120.44(19) C15 C14 H14 119.8 C13 C14 H14 119.8 C14 C15 C16 119.87(18) C14 C15 H15 120.1 C16 C15 H15 120.1 C15 C16 C17 120.2(2) C15 C16 H16 119.9 C17 C16 H16 119.9 C16 C17 C12 120.42(18) C16 C17 H17 119.8 C12 C17 H17 119.8 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C4 1.374(2) O1 C7 1.413(2) O2 C11 1.251(2) N1 C9 1.333(2) N1 C1 1.419(2) N1 H1 0.86 C1 C2 1.378(2) C1 C6 1.385(2) C2 C3 1.387(2) C2 H2 0.93 C3 C4 1.378(2) C3 H3 0.93 C4 C5 1.378(2) C5 C6 1.377(2) C5 H5 0.93 C6 H6 0.93 C7 H7A 0.96 C7 H7B 0.96 C7 H7C 0.96 C8 C9 1.497(2) C8 H8A 0.96 C8 H8B 0.96 C8 H8C 0.96 C9 C10 1.383(2) C10 C11 1.415(2) C10 H10 0.93 C11 C12 1.500(2) C12 C13 1.383(2) C12 C17 1.387(3) C13 C14 1.382(2) C13 H13 0.93 C14 C15 1.368(3) C14 H14 0.93 C15 C16 1.370(3) C15 H15 0.93 C16 C17 1.385(3) C16 H16 0.93 C17 H17 0.93 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 O2 . 0.86 1.91 2.629(2) 139 C8 H8B O2 1_655 0.96 2.49 3.351(3) 148 C3 H3 Cg2 2_455 0.93 2.84 3.712(3) 156 C13 H13 Cg1 2_545 0.93 2.82 3.619(3) 145 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 C9 N1 C1 C2 142.48(19) C9 N1 C1 C6 -40.9(3) C6 C1 C2 C3 -0.9(3) N1 C1 C2 C3 175.86(16) C1 C2 C3 C4 0.9(3) C7 O1 C4 C5 -167.8(2) C7 O1 C4 C3 12.2(3) C2 C3 C4 O1 -179.76(17) C2 C3 C4 C5 0.3(3) O1 C4 C5 C6 178.64(18) C3 C4 C5 C6 -1.4(3) C4 C5 C6 C1 1.4(3) C2 C1 C6 C5 -0.2(3) N1 C1 C6 C5 -176.83(17) C1 N1 C9 C10 178.77(16) C1 N1 C9 C8 -4.1(3) N1 C9 C10 C11 2.1(3) C8 C9 C10 C11 -175.06(16) C9 C10 C11 O2 -0.6(3) C9 C10 C11 C12 176.46(16) O2 C11 C12 C13 -149.89(18) C10 C11 C12 C13 32.8(2) O2 C11 C12 C17 30.3(2) C10 C11 C12 C17 -146.95(18) C17 C12 C13 C14 0.2(3) C11 C12 C13 C14 -179.60(17) C12 C13 C14 C15 1.0(3) C13 C14 C15 C16 -1.1(3) C14 C15 C16 C17 0.0(3) C15 C16 C17 C12 1.2(3) C13 C12 C17 C16 -1.3(3) C11 C12 C17 C16 178.51(17)