#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2008415.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_2008415 loop_ _publ_author_name 'Hoshina, G.' 'Ohba, S.' 'Tsuchimoto, M.' _publ_section_title ; (RS,SR)-N,N'-Bis(2-hydroxybenzyl)-1,2-diphenylethylenediamine ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first IUC9900030 _journal_volume 55 _journal_year 1999 _chemical_formula_moiety 'C28 H28 N2 O2' _chemical_formula_sum 'C28 H28 N2 O2' _chemical_formula_weight 424.54 _chemical_name_common N,N'-bis(2-hydroxybenzyl)-1,2-diphenylethylenediamine _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yab' _symmetry_space_group_name_H-M 'P 1 21/a 1' _audit_creation_method 'from TEXRAY.INF file' _cell_angle_alpha 90 _cell_angle_beta 97.60(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 7.361(3) _cell_length_b 16.269(4) _cell_length_c 9.622(3) _cell_measurement_reflns_used 25 _cell_measurement_temperature 299 _cell_measurement_theta_max 14.2 _cell_measurement_theta_min 12.8 _cell_volume 1142.2(7) _computing_cell_refinement 'MSC/AFC Diffractometer Control Software' _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation & Rigaku Corporation, 1993) ; _computing_data_reduction 'TEXSAN (Molecular Structure Corporation & Rigaku Corporation, 1998)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material TEXSAN _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _diffrn_ambient_temperature 299 _diffrn_measurement_device_type 'Rigaku AFC-5' _diffrn_measurement_method \q-2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Rigaku shield tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.023 _diffrn_reflns_av_sigmaI/netI 0.040 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 2419 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_reflns_theta_max 26.0 _diffrn_reflns_theta_min 2.13 _diffrn_standards_decay_% none _diffrn_standards_interval_count 100 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.078 _exptl_absorpt_correction_T_max 0.985 _exptl_absorpt_correction_T_min 0.904 _exptl_absorpt_correction_type \Y-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prismatic _exptl_crystal_F_000 452.00 _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.56 _exptl_crystal_size_min 0.17 _refine_diff_density_max 0.56 _refine_diff_density_min -0.35 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 145 _refine_ls_number_reflns 2239 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.048 _refine_ls_R_factor_all 0.125 _refine_ls_R_factor_gt 0.066 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.0843P)^2^+0.7660P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.201 _reflns_number_gt 1338 _reflns_number_total 2239 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file qb0084.cif _[local]_cod_data_source_block H4-salen _[local]_cod_cif_authors_sg_H-M 'P 21/a' _cod_original_cell_volume 1142.2(6) _cod_database_code 2008415 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,-z -x,-y,-z 1/2+x,1/2-y,z loop_ _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_occupancy _atom_site_type_symbol O1 0.0337(3) -0.1317(2) 0.4935(3) 0.0747(8) Uani 1.00 O N2 0.2985(3) -0.0451(2) 0.3901(3) 0.0510(7) Uani 1.00 N C3 -0.0449(4) -0.1377(2) 0.3581(3) 0.0479(8) Uani 1.00 C C4 -0.1899(5) -0.1927(2) 0.3268(4) 0.0550(9) Uani 1.00 C C5 -0.2761(5) -0.1994(2) 0.1915(4) 0.0617(10) Uani 1.00 C C6 -0.2183(5) -0.1540(2) 0.0849(4) 0.0567(9) Uani 1.00 C C7 -0.0735(4) -0.1008(2) 0.1160(3) 0.0477(7) Uani 1.00 C C8 0.0127(4) -0.0900(2) 0.2507(3) 0.0462(8) Uani 1.00 C C9 0.1516(5) -0.0218(3) 0.2852(4) 0.0710(10) Uani 1.00 C C10 0.4293(5) 0.0160(2) 0.4440(3) 0.0536(9) Uani 1.00 C C11 0.5070(4) 0.0694(2) 0.3371(3) 0.0412(7) Uani 1.00 C C12 0.5938(5) 0.0358(2) 0.2321(4) 0.0576(9) Uani 1.00 C C13 0.6658(6) 0.0839(3) 0.1381(4) 0.0750(10) Uani 1.00 C C14 0.6571(6) 0.1672(3) 0.1464(5) 0.0790(10) Uani 1.00 C C15 0.5711(6) 0.2032(2) 0.2488(5) 0.0760(10) Uani 1.00 C C16 0.4936(5) 0.1540(2) 0.3439(4) 0.0551(8) Uani 1.00 C H1 0.1496 -0.1061 0.4928 0.0907 Uiso 1.00 H H2 0.3463 -0.0842 0.3312 0.0907 Uiso 1.00 H H4 -0.2296 -0.2253 0.3990 0.0663 Uiso 1.00 H H5 -0.3768 -0.2358 0.1723 0.0735 Uiso 1.00 H H6 -0.2778 -0.1593 -0.0087 0.0686 Uiso 1.00 H H7 -0.0311 -0.0707 0.0417 0.0572 Uiso 1.00 H H9A 0.0918 0.0244 0.3174 0.0859 Uiso 1.00 H H9B 0.2019 -0.0079 0.2019 0.0859 Uiso 1.00 H H10 0.3726 0.0509 0.5038 0.0648 Uiso 1.00 H H12 0.6031 -0.0220 0.2249 0.0696 Uiso 1.00 H H13 0.7243 0.0595 0.0660 0.0910 Uiso 1.00 H H14 0.7095 0.2008 0.0821 0.0945 Uiso 1.00 H H15 0.5640 0.2616 0.2554 0.0877 Uiso 1.00 H H16 0.4313 0.1786 0.4137 0.0672 Uiso 1.00 H 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 0.070(2) 0.100(2) 0.0530(10) -0.035(2) 0.0040(10) 0.0090(10) N2 0.0440(10) 0.060(2) 0.0460(10) -0.0180(10) -0.0050(10) 0.0040(10) C3 0.041(2) 0.050(2) 0.052(2) -0.0050(10) 0.0050(10) -0.0020(10) C4 0.046(2) 0.048(2) 0.074(2) -0.0090(10) 0.019(2) -0.003(2) C5 0.043(2) 0.054(2) 0.087(3) -0.013(2) 0.005(2) -0.019(2) C6 0.049(2) 0.053(2) 0.065(2) -0.001(2) -0.007(2) -0.017(2) C7 0.043(2) 0.047(2) 0.052(2) 0.0030(10) 0.0010(10) 0.0000(10) C8 0.035(2) 0.049(2) 0.053(2) -0.0070(10) 0.0000(10) 0.0020(10) C9 0.059(2) 0.082(3) 0.066(2) -0.027(2) -0.013(2) 0.017(2) C10 0.049(2) 0.059(2) 0.050(2) -0.019(2) -0.0020(10) 0.005(2) C11 0.0340(10) 0.042(2) 0.046(2) -0.0050(10) -0.0010(10) 0.0020(10) C12 0.057(2) 0.054(2) 0.063(2) 0.008(2) 0.014(2) 0.002(2) C13 0.063(2) 0.092(3) 0.074(3) 0.004(2) 0.026(2) 0.013(2) C14 0.058(2) 0.100(3) 0.077(3) -0.022(2) 0.004(2) 0.039(3) C15 0.074(3) 0.045(2) 0.101(3) -0.013(2) -0.022(2) 0.020(2) C16 0.051(2) 0.048(2) 0.064(2) 0.002(2) 0.001(2) -0.007(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 1 0 2 -1 0 1 3 1 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 C3 O1 H1 . . 107 no C9 N2 C10 . . 118.8(3) yes C9 N2 H2 . . 93 no C10 N2 H2 . . 113 no O1 C3 C4 . . 118.1(3) yes O1 C3 C8 . . 122.4(3) yes C4 C3 C8 . . 119.6(3) yes C3 C4 C5 . . 119.9(3) yes C3 C4 H4 . . 120.1 no C5 C4 H4 . . 120.0 no C4 C5 C6 . . 120.9(3) yes C4 C5 H5 . . 119.0 no C6 C5 H5 . . 120.0 no C5 C6 C7 . . 118.8(3) yes C5 C6 H6 . . 120.5 no C7 C6 H6 . . 120.7 no C6 C7 C8 . . 122.3(3) yes C6 C7 H7 . . 118.8 no C8 C7 H7 . . 119.0 no C3 C8 C7 . . 118.4(3) yes C3 C8 C9 . . 120.3(3) yes C7 C8 C9 . . 120.9(3) yes N2 C9 C8 . . 112.7(3) yes N2 C9 H9A . . 108.7 no N2 C9 H9B . . 108.3 no C8 C9 H9A . . 108.9 no C8 C9 H9B . . 108.4 no H9A C9 H9B . . 109.7 no N2 C10 C10 . 3_656 113.0(4) yes N2 C10 C11 . . 116.6(3) yes N2 C10 H10 . . 107.9 no C10 C10 C11 3_656 . 113.7(3) yes C10 C10 H10 3_656 . 95.3 no C11 C10 H10 . . 107.8 no C10 C11 C12 . . 121.6(3) yes C10 C11 C16 . . 120.2(3) yes C12 C11 C16 . . 118.2(3) yes C11 C12 C13 . . 121.4(3) yes C11 C12 H12 . . 119.6 no C13 C12 H12 . . 119.1 no C12 C13 C14 . . 120.7(4) yes C12 C13 H13 . . 120.0 no C14 C13 H13 . . 119.3 no C13 C14 C15 . . 119.9(4) yes C13 C14 H14 . . 120.8 no C15 C14 H14 . . 119.3 no C14 C15 C16 . . 119.6(4) yes C14 C15 H15 . . 120.5 no C16 C15 H15 . . 119.9 no C11 C16 C15 . . 120.2(3) yes C11 C16 H16 . . 119.8 no C15 C16 H16 . . 120.0 no 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 O1 C3 . 1.357(4) yes O1 H1 . 0.950 no N2 C9 . 1.429(4) yes N2 C10 . 1.433(4) yes N2 H2 . 0.950 no C3 C4 . 1.395(4) yes C3 C8 . 1.403(4) yes C4 C5 . 1.375(5) yes C4 H4 . 0.950 no C5 C6 . 1.376(5) yes C5 H5 . 0.948 no C6 C7 . 1.375(5) yes C6 H6 . 0.951 no C7 C8 . 1.377(4) yes C7 H7 . 0.953 no C8 C9 . 1.515(5) yes C9 H9A . 0.944 no C9 H9B . 0.953 no C10 C10 3_656 1.489(6) yes C10 C11 . 1.515(4) yes C10 H10 . 0.944 no C11 C12 . 1.377(5) yes C11 C16 . 1.382(4) yes C12 C13 . 1.356(6) yes C12 H12 . 0.946 no C13 C14 . 1.358(7) yes C13 H13 . 0.951 no C14 C15 . 1.371(7) yes C14 H14 . 0.946 no C15 C16 . 1.394(6) yes C15 H15 . 0.953 no C16 H16 . 0.950 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O1 H1 N2 0.95 1.86 2.699(4) 146