#------------------------------------------------------------------------------ #$Date: 2022-09-17 19:03:29 +0100 (Sat, 17 Sep 2022) $ #$Revision: 277941 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/01/4000110.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4000110 loop_ _publ_author_name 'Chan, Suk Hang' 'Wong, Wing Tak' 'Chan, Wai Kin' _publ_section_title ; Synthesis and Properties of Polyimide with Diazacrown Ether Moiety and the Corresponding Polymer Barium Complexes ; _journal_coden_ASTM CMATEX _journal_issue 12 _journal_name_full 'Chemistry of Materials' _journal_page_first 4635 _journal_page_last 4641 _journal_paper_doi 10.1021/cm0103500 _journal_volume 13 _journal_year 2001 _chemical_formula_sum 'C28 H42 Ba N6 O5 S2' _chemical_formula_weight 744.13 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _audit_creation_date 'Fri Aug 8 16:44:03 1997' _audit_creation_method 'from TEXRAY.INF file' _cell_angle_alpha 90 _cell_angle_beta 110.88(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 17.727(7) _cell_length_b 9.722(7) _cell_length_c 20.761(6) _cell_measurement_reflns_used 25 _cell_measurement_temperature 301.2 _cell_measurement_theta_max 16.7 _cell_measurement_theta_min 13.5 _cell_volume 3343(2) _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_data_reduction teXsan _computing_publication_material teXsan _computing_structure_refinement teXsan _computing_structure_solution SHELXS86 _diffrn_ambient_temperature 301.2 _diffrn_measurement_device AFC7R _diffrn_measurement_method 'omega/2-theta scans' _diffrn_orient_matrix_UB_11 0.02734 _diffrn_orient_matrix_UB_12 0.08853 _diffrn_orient_matrix_UB_13 -0.00289 _diffrn_orient_matrix_UB_21 0.00702 _diffrn_orient_matrix_UB_22 -0.03248 _diffrn_orient_matrix_UB_23 -0.04322 _diffrn_orient_matrix_UB_31 -0.05337 _diffrn_orient_matrix_UB_32 0.04108 _diffrn_orient_matrix_UB_33 -0.02795 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type MoKalpha _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.03 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 3243 _diffrn_reflns_theta_max 25.00 _diffrn_standards_decay_% -5.97 _diffrn_standards_interval_count 250 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.356 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.973 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_crystal_colour colourlessXDIM _exptl_crystal_density_diffrn 1.478 _exptl_crystal_description XDIM _exptl_crystal_F_000 1520.00 _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.220 _exptl_crystal_size_min 0.210 _refine_diff_density_max 0.20 _refine_diff_density_min -0.30 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 1.255 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 191 _refine_ls_number_reflns 2065 _refine_ls_number_restraints 0 _refine_ls_R_factor_obs 0.0406 _refine_ls_shift/esd_max 0.0020 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_obs 0.0358 _reflns_number_observed 2065 _reflns_number_total 3130 _reflns_observed_criterion 1.50 _cod_original_sg_symbol_H-M 'C 2/c' _cod_original_formula_sum 'C28 H42 Ba N6 O5 S2 ' _cod_database_code 4000110 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,y,-z+1/2 3 -x,-y,-z 4 x,-y,z+1/2 5 x+1/2,y+1/2,z 6 -x+1/2,y+1/2,-z+1/2 7 -x+1/2,-y+1/2,-z 8 x+1/2,-y+1/2,z+1/2 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 Ba(1) 0.0414(2) 0.0539(3) 0.0425(2) 0.0000 0.0041(2) 0.0000 S(1) 0.084(1) 0.136(2) 0.101(2) 0.012(1) 0.028(1) 0.028(1) O(1) 0.084(3) 0.081(3) 0.061(3) 0.011(3) 0.023(2) -0.005(2) O(2) 0.048(2) 0.081(3) 0.074(3) 0.003(2) 0.013(2) -0.002(2) O(3) 0.066(3) 0.047(4) 0.088(4) 0.0000 0.008(3) 0.0000 N(1) 0.069(3) 0.054(3) 0.051(2) 0.003(3) 0.003(2) 0.004(3) N(2) 0.087(3) 0.069(3) 0.065(3) 0.001(3) -0.021(3) -0.013(3) N(3) 0.111(5) 0.102(6) 0.097(5) -0.026(4) 0.033(4) 0.005(4) C(1) 0.095(5) 0.107(6) 0.048(3) 0.019(5) 0.018(3) -0.006(4) C(2) 0.113(6) 0.095(5) 0.068(4) 0.025(5) 0.033(4) -0.014(4) C(3) 0.075(4) 0.094(5) 0.091(5) 0.016(4) 0.040(4) -0.005(4) C(4) 0.061(4) 0.112(6) 0.104(6) 0.008(4) 0.035(4) -0.005(5) C(5) 0.050(3) 0.075(5) 0.091(5) 0.009(3) -0.010(3) -0.005(4) C(6) 0.083(5) 0.059(4) 0.062(4) 0.007(4) -0.020(3) 0.000(3) C(7) 0.070(4) 0.051(3) 0.053(3) 0.008(3) 0.000(3) 0.006(3) C(8) 0.065(4) 0.045(3) 0.055(3) 0.005(3) 0.003(3) 0.004(3) C(9) 0.081(4) 0.050(3) 0.058(4) -0.014(3) 0.012(3) 0.003(3) C(10) 0.071(4) 0.056(4) 0.079(4) -0.010(3) 0.002(3) 0.001(3) C(11) 0.081(4) 0.036(4) 0.064(4) 0.007(3) -0.003(3) -0.003(3) C(12) 0.092(5) 0.073(5) 0.054(4) 0.023(4) 0.008(3) -0.012(3) C(13) 0.069(4) 0.073(4) 0.066(4) 0.013(3) 0.010(3) -0.009(4) C(14) 0.059(4) 0.077(5) 0.072(4) -0.018(3) 0.021(3) -0.024(4) 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 Ba(1) 0.0000 0.12772(6) 0.7500 0.0489(1) Uij S(1) -0.0717(1) -0.2808(3) 0.8755(1) 0.1086(8) Uij O(1) -0.0691(3) 0.2187(4) 0.8466(2) 0.076(1) Uij O(2) -0.1530(2) 0.2486(4) 0.7048(2) 0.070(1) Uij O(3) 0.0000 0.4060(5) 0.7500 0.073(2) Uij N(1) -0.0971(3) 0.1163(5) 0.6004(2) 0.063(1) Uij N(2) -0.3953(3) -0.1247(6) 0.3325(2) 0.087(2) Uij N(3) -0.0930(4) -0.0963(7) 0.7697(3) 0.105(3) Uij C(1) 0.0472(4) 0.1512(8) 0.9403(3) 0.086(2) Uij C(2) -0.0132(5) 0.2631(8) 0.9097(3) 0.092(3) Uij C(3) -0.1355(4) 0.3134(7) 0.8190(4) 0.083(2) Uij C(4) -0.1917(4) 0.2557(8) 0.7524(4) 0.091(3) Uij C(5) -0.2060(3) 0.2076(7) 0.6373(4) 0.081(2) Uij C(6) -0.1605(4) 0.2195(6) 0.5896(3) 0.080(2) Uij C(7) -0.1302(3) -0.0257(6) 0.5857(3) 0.064(2) Uij C(8) -0.2000(3) -0.0496(6) 0.5176(3) 0.060(2) Uij C(9) -0.2772(4) -0.0694(6) 0.5171(3) 0.067(2) Uij C(10) -0.3419(4) -0.0951(6) 0.4558(3) 0.076(2) Uij C(11) -0.3297(4) -0.1011(5) 0.3945(3) 0.068(2) Uij C(12) -0.2532(4) -0.0790(7) 0.3941(3) 0.078(2) Uij C(13) -0.1886(4) -0.0549(6) 0.4553(3) 0.073(2) Uij C(14) -0.0829(4) -0.1699(7) 0.8145(3) 0.070(2) Uij H(1) 0.0814 0.1756 0.9867 0.1016 Uij H(2) 0.0174 0.0698 0.9444 0.1016 Uij H(3) 0.0157 0.3444 0.9028 0.1103 Uij H(4) -0.0394 0.2911 0.9411 0.1103 Uij H(5) -0.1620 0.3319 0.8518 0.0988 Uij H(6) -0.1159 0.4034 0.8100 0.0988 Uij H(7) -0.2418 0.3085 0.7348 0.1068 Uij H(8) -0.2090 0.1634 0.7615 0.1068 Uij H(9) -0.2236 0.1130 0.6379 0.0973 Uij H(10) -0.2546 0.2630 0.6220 0.0973 Uij H(11) -0.1357 0.3105 0.5958 0.0924 Uij H(12) -0.1970 0.2155 0.5423 0.0924 Uij H(13) -0.0861 -0.0881 0.5870 0.0753 Uij H(14) -0.1472 -0.0555 0.6230 0.0753 Uij H(15) -0.2870 -0.0641 0.5605 0.0830 Uij H(16) -0.3962 -0.1111 0.4564 0.0921 Uij H(17) -0.2433 -0.0782 0.3498 0.0936 Uij H(18) -0.1338 -0.0411 0.4541 0.0887 Uij H(19) -0.3893 -0.1668 0.2869 0.0890 Uij H(20) -0.4505 -0.1701 0.3338 0.0890 Uij H(21) -0.0237 0.4952 0.7378 0.0890 Uij loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ba 0 4 -0.324 2.282 'International Tables' N 0 24 0.006 0.003 'International Tables' S 0 8 0.125 0.123 'International Tables' O 0 20 0.011 0.006 'International Tables' C 0 112 0.003 0.002 'International Tables' H 0 168 0.000 0.000 'International Tables' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -3 1 -4 -3 1 -5 -3 3 -1 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) Ba(1) O(1) 143.7(2) ? ? ? yes O(1) Ba(1) O(2) 59.6(1) ? ? ? yes O(1) Ba(1) O(2) 104.1(1) ? ? ? yes O(1) Ba(1) O(3) 71.84(9) ? ? ? yes O(1) Ba(1) N(1) 121.0(1) ? ? ? yes O(1) Ba(1) N(1) 60.5(1) ? ? ? yes O(1) Ba(1) N(3) 73.7(2) ? ? ? yes O(1) Ba(1) N(3) 139.3(2) ? ? ? yes O(1) Ba(1) O(2) 104.1(1) ? ? ? yes O(1) Ba(1) O(2) 59.6(1) ? ? ? yes O(1) Ba(1) O(3) 71.84(9) ? ? ? yes O(1) Ba(1) N(1) 60.5(1) ? ? ? yes O(1) Ba(1) N(1) 121.0(1) ? ? ? yes O(1) Ba(1) N(3) 139.3(2) ? ? ? yes O(1) Ba(1) N(3) 73.7(2) ? ? ? yes O(2) Ba(1) O(2) 130.2(2) ? ? ? yes O(2) Ba(1) O(3) 65.12(8) ? ? ? yes O(2) Ba(1) N(1) 62.1(1) ? ? ? yes O(2) Ba(1) N(1) 119.9(1) ? ? ? yes O(2) Ba(1) N(3) 80.1(2) ? ? ? yes O(2) Ba(1) N(3) 144.7(2) ? ? ? yes O(2) Ba(1) O(3) 65.12(8) ? ? ? yes O(2) Ba(1) N(1) 119.9(1) ? ? ? yes O(2) Ba(1) N(1) 62.1(1) ? ? ? yes O(2) Ba(1) N(3) 144.7(2) ? ? ? yes O(2) Ba(1) N(3) 80.1(2) ? ? ? yes O(3) Ba(1) N(1) 92.15(10) ? ? ? yes O(3) Ba(1) N(1) 92.15(10) ? ? ? yes O(3) Ba(1) N(3) 139.9(1) ? ? ? yes O(3) Ba(1) N(3) 139.9(1) ? ? ? yes N(1) Ba(1) N(1) 175.7(2) ? ? ? yes N(1) Ba(1) N(3) 88.4(2) ? ? ? yes N(1) Ba(1) N(3) 88.3(2) ? ? ? yes N(1) Ba(1) N(3) 88.3(2) ? ? ? yes N(1) Ba(1) N(3) 88.4(2) ? ? ? yes N(3) Ba(1) N(3) 80.3(3) ? ? ? yes Ba(1) O(1) C(2) 114.7(4) ? ? ? yes Ba(1) O(1) C(3) 114.5(3) ? ? ? yes C(2) O(1) C(3) 112.4(5) ? ? ? yes Ba(1) O(2) C(4) 116.6(4) ? ? ? yes Ba(1) O(2) C(5) 115.4(3) ? ? ? yes C(4) O(2) C(5) 113.0(5) ? ? ? yes Ba(1) N(1) C(1) 110.5(3) ? ? ? yes Ba(1) N(1) C(6) 105.2(3) ? ? ? yes Ba(1) N(1) C(7) 106.7(3) ? ? ? yes C(1) N(1) C(6) 109.9(5) ? ? ? yes C(1) N(1) C(7) 111.8(5) ? ? ? yes C(6) N(1) C(7) 112.3(4) ? ? ? yes Ba(1) N(3) C(14) 132.0(5) ? ? ? yes N(1) C(1) C(2) 114.2(5) ? ? ? yes O(1) C(2) C(1) 109.5(5) ? ? ? yes O(1) C(3) C(4) 108.0(5) ? ? ? yes O(2) C(4) C(3) 109.9(5) ? ? ? yes O(2) C(5) C(6) 107.9(5) ? ? ? yes N(1) C(6) C(5) 114.4(5) ? ? ? yes N(1) C(7) C(8) 117.4(4) ? ? ? yes C(7) C(8) C(9) 120.2(5) ? ? ? yes C(7) C(8) C(13) 122.1(6) ? ? ? yes C(9) C(8) C(13) 117.7(5) ? ? ? yes C(8) C(9) C(10) 121.5(6) ? ? ? yes C(9) C(10) C(11) 120.2(6) ? ? ? yes N(2) C(11) C(10) 120.3(6) ? ? ? yes N(2) C(11) C(12) 120.8(6) ? ? ? yes C(10) C(11) C(12) 118.9(6) ? ? ? yes C(11) C(12) C(13) 120.8(6) ? ? ? yes C(8) C(13) C(12) 120.9(6) ? ? ? yes S(1) C(14) N(3) 176.9(6) ? ? ? yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ba(1) O(1) 2.838(4) ? ? yes Ba(1) O(1) 2.838(4) ? ? yes Ba(1) O(2) 2.793(4) ? ? yes Ba(1) O(2) 2.793(4) ? ? yes Ba(1) O(3) 2.706(5) ? ? yes Ba(1) N(1) 2.969(4) ? ? yes Ba(1) N(1) 2.969(4) ? ? yes Ba(1) N(3) 2.849(6) ? ? yes Ba(1) N(3) 2.849(6) ? ? yes S(1) C(14) 1.619(7) ? ? yes O(1) C(2) 1.400(7) ? ? yes O(1) C(3) 1.442(7) ? ? yes O(2) C(4) 1.390(7) ? ? yes O(2) C(5) 1.438(7) ? ? yes N(1) C(1) 1.465(7) ? ? yes N(1) C(6) 1.462(7) ? ? yes N(1) C(7) 1.489(7) ? ? yes N(2) C(11) 1.413(6) ? ? yes N(3) C(14) 1.136(8) ? ? yes C(1) C(2) 1.500(9) ? ? yes C(3) C(4) 1.495(9) ? ? yes C(5) C(6) 1.488(9) ? ? yes C(7) C(8) 1.529(7) ? ? yes C(8) C(9) 1.377(7) ? ? yes C(8) C(13) 1.380(8) ? ? yes C(9) C(10) 1.399(7) ? ? yes C(10) C(11) 1.366(8) ? ? yes C(11) C(12) 1.376(8) ? ? yes C(12) C(13) 1.394(8) ? ? yes loop_ _cod_changelog_entry_id _cod_changelog_entry_author _cod_changelog_entry_date _cod_changelog_entry_text 1 'Vaitkus, Antanas' 2022-09-17T16:45:00+03:00 'Updated bibliographic information.' 2 'Vaitkus, Antanas' 2022-09-17T21:00:00+03:00 ; Changed the values of multiple data items and added additional information after consulting the original CIF file which was provided as supplementary material for the original publication. The previous version of this entry incorrectly contained atomic coordinates and other information from a different crystal structure that is properly described in COD entry 4002652. ;