#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2008282.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_2008282 loop_ _publ_author_name 'Okuyama, K.' 'Rozhanskii, I.' 'Goto, K.' _publ_contact_author ; Prof. Kenji Okuyama Faculty of Technology Tokyo University of Agriculture and Technology Koganei, Tokyo 184-8588 Japan ; _publ_section_title ; Bilayered structure of N,N'-diphenyl-4,4'-biphthalimide ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 424 _journal_page_last 425 _journal_volume 55 _journal_year 1999 _chemical_formula_moiety 'C28 H16 N2 O4 ' _chemical_formula_sum 'C28 H16 N2 O4' _chemical_formula_weight 444.45 _chemical_melting_point 664. _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' _audit_creation_method 'from TEXRAY.INF file' _cell_angle_alpha 90 _cell_angle_beta 90.868(11) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.3987(15) _cell_length_b 6.890(4) _cell_length_c 17.8585(15) _cell_measurement_reflns_used 25 _cell_measurement_temperature 296.2 _cell_measurement_theta_max 24.8 _cell_measurement_theta_min 21.9 _cell_volume 1033.3(6) _computing_cell_refinement 'MSC/AFC Diffractometer Control Software' _computing_data_collection 'MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1988)' _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1995)' _computing_publication_material TEXSAN _computing_structure_refinement TEXSAN _computing_structure_solution 'SHELXS86 (Sheldrick, 1985)' _diffrn_ambient_temperature 296.2 _diffrn_measurement_device 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.016 _diffrn_reflns_av_sigmaI/netI 0.000 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 3608 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_reflns_theta_max 30.0 _diffrn_reflns_theta_min 1.3 _diffrn_standards_decay_% 0.14 _diffrn_standards_interval_count 100 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.097 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_meas 1.425 _exptl_crystal_density_method 'flotation in aqueous KI' _exptl_crystal_description prismatic _exptl_crystal_F_000 460.00 _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.300 _refine_diff_density_max 0.22 _refine_diff_density_min -0.28 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 1.145 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 154 _refine_ls_number_reflns 1833 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.0487 _refine_ls_shift/esd_max 0.0020 _refine_ls_shift/esd_mean 0.0000 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00090|Fo|^2^]' _refine_ls_wR_factor_obs 0.0668 _reflns_number_observed 1833 _reflns_number_total 3273 _reflns_observed_criterion >2.0sigma(I) _[local]_cod_data_source_file oa1075.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/c ' _[local]_cod_chemical_formula_sum_orig 'C28 H16 N2 O4 ' _cod_original_cell_volume 1033.3(7) _cod_database_code 2008282 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z 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 0.0461(9) 0.0473(9) 0.0950(10) -0.0027(7) -0.0014(9) 0.0315(9) O2 0.0276(6) 0.0578(10) 0.0800(10) -0.0015(6) -0.0017(7) 0.0238(8) N1 0.0288(7) 0.0361(8) 0.0475(9) 0.0033(7) -0.0032(6) 0.0062(7) C1 0.0430(10) 0.0640(10) 0.0470(10) 0.0160(10) -0.0030(9) 0.0120(10) C2 0.0550(10) 0.0470(10) 0.0540(10) 0.0220(10) 0.0000(10) -0.0010(10) C3 0.0470(10) 0.0460(10) 0.0450(10) 0.0100(9) -0.0062(9) -0.0045(9) C4 0.0296(8) 0.0382(10) 0.0399(9) 0.0060(7) -0.0002(7) 0.0048(8) C5 0.0440(10) 0.0400(10) 0.0470(10) 0.0033(9) -0.0040(9) -0.0016(9) C6 0.0440(10) 0.0590(10) 0.0450(10) 0.0000(10) -0.0109(9) 0.0030(10) C7 0.0334(9) 0.0358(10) 0.0490(10) 0.0013(8) -0.0018(8) 0.0045(9) C8 0.0289(8) 0.0352(9) 0.0396(9) 0.0013(7) -0.0010(7) 0.0036(8) C9 0.0301(9) 0.0380(10) 0.0530(10) -0.0035(8) 0.0024(8) 0.0083(9) C10 0.0260(8) 0.0420(10) 0.0490(10) 0.0022(8) 0.0012(7) 0.0042(9) C11 0.0266(8) 0.0353(9) 0.0353(9) 0.0026(7) 0.0005(6) 0.0014(8) C12 0.0262(8) 0.0393(10) 0.0440(10) 0.0010(7) 0.0007(7) 0.0063(8) C13 0.0253(8) 0.0376(10) 0.0398(9) 0.0019(7) -0.0004(7) 0.0035(8) C14 0.0281(8) 0.0394(10) 0.0440(10) 0.0026(8) -0.0019(7) 0.0073(8) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_occupancy O1 0.2860(2) 0.7108(2) 0.34130(10) 0.0629(5) Uani d 1.00 O2 -0.0448(2) 0.2487(2) 0.43640(10) 0.0552(5) Uani d 1.00 N1 0.0865(2) 0.5036(2) 0.37977(9) 0.0375(4) Uani d 1.00 C1 -0.3015(3) 0.7885(4) 0.28000(10) 0.0511(6) Uani d 1.00 C2 -0.2094(3) 0.8822(3) 0.33250(10) 0.0521(6) Uani d 1.00 C3 -0.0819(3) 0.7890(3) 0.36660(10) 0.0462(6) Uani d 1.00 C4 -0.0473(2) 0.6013(3) 0.34610(10) 0.0359(5) Uani d 1.00 C5 -0.1369(2) 0.5063(3) 0.29180(10) 0.0436(5) Uani d 1.00 C6 -0.2655(3) 0.6012(4) 0.25890(10) 0.0496(6) Uani d 1.00 C7 0.2454(2) 0.5655(3) 0.37220(10) 0.0394(5) Uani d 1.00 C8 0.3438(2) 0.4133(3) 0.40870(10) 0.0346(4) Uani d 1.00 C9 0.5065(2) 0.3957(3) 0.41640(10) 0.0405(5) Uani d 1.00 C10 0.5646(2) 0.2321(3) 0.45250(10) 0.0391(5) Uani d 1.00 C11 0.4657(2) 0.0868(3) 0.48089(10) 0.0324(4) Uani d 1.00 C12 0.3001(2) 0.1092(3) 0.47250(10) 0.0365(5) Uani d 1.00 C13 0.2438(2) 0.2722(3) 0.43680(10) 0.0343(4) Uani d 1.00 C14 0.0767(2) 0.3299(3) 0.41970(10) 0.0373(5) Uani d 1.00 H1 -0.3912 0.8521 0.2576 0.0599 Uiso calc 1.00 H2 -0.2341 1.0134 0.3461 0.0630 Uiso calc 1.00 H3 -0.0174 0.8559 0.4033 0.0551 Uiso calc 1.00 H4 -0.1107 0.3774 0.2762 0.0517 Uiso calc 1.00 H5 -0.3292 0.5373 0.2218 0.0580 Uiso calc 1.00 H6 0.5761 0.4930 0.3975 0.0476 Uiso calc 1.00 H7 0.6770 0.2177 0.4581 0.0462 Uiso calc 1.00 H8 0.2286 0.0128 0.4907 0.0436 Uiso calc 1.00 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 5 0 0 1 3 0 0 2 8 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_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C4 N1 C7 1_555 1_555 1_555 123.7(2) yes C4 N1 C14 1_555 1_555 1_555 124.4(2) yes C7 N1 C14 1_555 1_555 1_555 111.80(10) yes C2 C1 C6 1_555 1_555 1_555 120.3(2) yes C2 C1 H1 1_555 1_555 1_555 120.3(2) no C6 C1 H1 1_555 1_555 1_555 119.4(2) no C1 C2 C3 1_555 1_555 1_555 120.6(2) yes C1 C2 H2 1_555 1_555 1_555 119.7(2) no C3 C2 H2 1_555 1_555 1_555 119.7(2) no C2 C3 C4 1_555 1_555 1_555 119.0(2) yes C2 C3 H3 1_555 1_555 1_555 120.1(2) no C4 C3 H3 1_555 1_555 1_555 120.8(2) no N1 C4 C3 1_555 1_555 1_555 119.8(2) yes N1 C4 C5 1_555 1_555 1_555 119.1(2) yes C3 C4 C5 1_555 1_555 1_555 121.1(2) yes C4 C5 C6 1_555 1_555 1_555 119.1(2) yes C4 C5 H4 1_555 1_555 1_555 121.1(2) no C6 C5 H4 1_555 1_555 1_555 119.8(2) no C1 C6 C5 1_555 1_555 1_555 119.9(2) yes C1 C6 H5 1_555 1_555 1_555 119.9(2) no C5 C6 H5 1_555 1_555 1_555 120.1(2) no O1 C7 N1 1_555 1_555 1_555 125.0(2) yes O1 C7 C8 1_555 1_555 1_555 129.5(2) yes N1 C7 C8 1_555 1_555 1_555 105.5(2) yes C7 C8 C9 1_555 1_555 1_555 130.8(2) yes C7 C8 C13 1_555 1_555 1_555 108.7(2) yes C9 C8 C13 1_555 1_555 1_555 120.6(2) yes C8 C9 C10 1_555 1_555 1_555 117.4(2) yes C8 C9 H6 1_555 1_555 1_555 121.0(2) no C10 C9 H6 1_555 1_555 1_555 121.6(2) no C9 C10 C11 1_555 1_555 1_555 123.0(2) yes C9 C10 H7 1_555 1_555 1_555 118.4(2) no C11 C10 H7 1_555 1_555 1_555 118.6(2) no C10 C11 C11 1_555 1_555 3_656 120.9(2) yes C10 C11 C12 1_555 1_555 1_555 118.3(2) yes C11 C11 C12 3_656 1_555 1_555 120.9(2) yes C11 C12 C13 1_555 1_555 1_555 118.3(2) yes C11 C12 H8 1_555 1_555 1_555 120.9(2) no C13 C12 H8 1_555 1_555 1_555 120.9(2) no C8 C13 C12 1_555 1_555 1_555 122.5(2) yes C8 C13 C14 1_555 1_555 1_555 108.3(2) yes C12 C13 C14 1_555 1_555 1_555 129.2(2) yes O2 C14 N1 1_555 1_555 1_555 125.5(2) yes O2 C14 C13 1_555 1_555 1_555 128.7(2) yes N1 C14 C13 1_555 1_555 1_555 105.8(2) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 C7 1_555 1_555 1.196(2) yes O2 C14 1_555 1_555 1.205(2) yes N1 C4 1_555 1_555 1.434(2) yes N1 C7 1_555 1_555 1.409(2) yes N1 C14 1_555 1_555 1.396(3) yes C1 C2 1_555 1_555 1.369(3) yes C1 C6 1_555 1_555 1.378(3) yes C2 C3 1_555 1_555 1.382(3) yes C3 C4 1_555 1_555 1.376(3) yes C4 C5 1_555 1_555 1.383(3) yes C5 C6 1_555 1_555 1.385(3) yes C7 C8 1_555 1_555 1.480(3) yes C8 C9 1_555 1_555 1.377(2) yes C8 C13 1_555 1_555 1.384(3) yes C9 C10 1_555 1_555 1.384(3) yes C10 C11 1_555 1_555 1.401(3) yes C11 C11 1_555 3_656 1.488(3) yes C11 C12 1_555 1_555 1.405(2) yes C12 C13 1_555 1_555 1.371(3) yes C13 C14 1_555 1_555 1.486(2) yes loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O1 C6 3.234(3) 1_555 2_555 O1 C5 3.357(3) 1_555 2_555 O2 C10 3.299(2) 1_555 1_455 O2 C2 3.413(3) 1_555 1_545 O2 C3 3.416(3) 1_555 1_545 C1 C7 3.360(3) 1_555 2_555 C1 C8 3.491(3) 1_555 2_555 C2 C12 3.577(3) 1_555 3_566 C3 C12 3.503(3) 1_555 3_566 C8 C10 3.556(3) 1_555 3_666 C8 C9 3.598(3) 1_555 3_666 C9 C9 3.316(4) 1_555 3_666 C9 C10 3.529(3) 1_555 3_666