#------------------------------------------------------------------------------ #$Date: 2023-11-28 20:30:13 +0200 (Tue, 28 Nov 2023) $ #$Revision: 287836 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/35/08/4350822.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_4350822 loop_ _publ_author_name 'Mohamed Essalhi' 'Midhun Mohan' 'Nour Dissem' 'Najmedinne Ferhi' 'Adela Abidi' 'Thierry Maris' 'Adam Duong' _publ_section_title ; Two different pore architectures of cyamelurate-based metal-organic frameworks for highly selective CO2 capture under ambient conditions ; _journal_name_full 'Inorganic Chemistry Frontiers' _journal_page_first 1037 _journal_page_last 1048 _journal_paper_doi 10.1039/d2qi02208g _journal_volume 10 _journal_year 2023 _chemical_formula_moiety 'C6 H4 N7 Nd O5' _chemical_formula_sum 'C6 H4 N7 Nd O5' _chemical_formula_weight 398.40 _chemical_name_systematic ; catena-[(\m-1,3,4,6,7,9,9b-heptaazaphenalene-2,5,8-triolato) -diaqua-neodymium(iii) N,N-dimethylformamide solvate] ; _space_group_crystal_system tetragonal _space_group_IT_number 91 _space_group_name_Hall 'P 4w 2c' _space_group_name_H-M_alt 'P 41 2 2' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary dual _audit_creation_date 2020-02-07 _audit_creation_method ; Olex2 1.3 (compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.6409(2) _cell_length_b 8.6409(2) _cell_length_c 20.1002(6) _cell_measurement_reflns_used 9022 _cell_measurement_temperature 100 _cell_measurement_theta_max 69.877 _cell_measurement_theta_min 5.119 _cell_volume 1500.78(7) _computing_cell_refinement ; SAINT (2013) V8.40A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173. ; _computing_data_collection ; APEX 2 (2013) Bruker AXS Inc., Madison, WI 53719-1173. ; _computing_data_reduction ; SAINT (2013) V8.40A; Integration Software for Single Crystal Data. Bruker AXS Inc., Madison, WI 53719-1173. ; _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XT (Sheldrick, 2015)' _diffrn_ambient_temperature 100 _diffrn_detector 'CCD area detector' _diffrn_detector_area_resol_mean 8.3 _diffrn_detector_type 'Bruker APEX2 CCD' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker Smart APEX' _diffrn_measurement_method '\w scans' _diffrn_radiation_collimation 'Focusing mirrors' _diffrn_radiation_monochromator 'Quazar MX Mirror Optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_unetI/netI 0.0082 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 41941 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 69.985 _diffrn_reflns_theta_min 5.118 _diffrn_source 'Microfocus Source' _diffrn_source_current 0.65 _diffrn_source_power 0.02912 _diffrn_source_target Cu _diffrn_source_type 'Incoatec I\mS High Brilliance Microsource' _diffrn_source_voltage 44.8 _exptl_absorpt_coefficient_mu 26.672 _exptl_absorpt_correction_T_max 0.1348 _exptl_absorpt_correction_T_min 0.0357 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0780 before and 0.0460 after correction. The Ratio of minimum to maximum transmission is 0.2648. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.763 _exptl_crystal_description octahedron _exptl_crystal_F_000 756 _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.055 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.985 _refine_diff_density_min -1.490 _refine_diff_density_rms 0.158 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.20(2) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 90 _refine_ls_number_reflns 1434 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.062 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0465 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0948P)^2^+6.0132P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1321 _refine_ls_wR_factor_ref 0.1321 _reflns_Friedel_coverage 0.588 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 1.000 _reflns_number_gt 1424 _reflns_number_total 1434 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ada2452.cif _cod_data_source_block ada2452 _cod_original_cell_volume 1500.78(8) _cod_database_code 4350822 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, z+1/2' 3 '-y, x, z+1/4' 4 'y, -x, z+3/4' 5 '-x, y, -z' 6 'x, -y, -z+1/2' 7 'y, x, -z+3/4' 8 '-y, -x, -z+1/4' loop_ _atom_site_label _atom_site_type_symbol _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.45942(6) 0.45942(6) 0.375000 0.0343(3) Uani 1 2 d S T P . . O1 O 0.4096(12) 0.500000 0.250000 0.0329(19) Uani 1 2 d S T P . . O2 O -0.2671(10) 0.5469(14) 0.0837(3) 0.055(2) Uani 1 1 d . . . . . N1 N 0.1942(11) 0.4768(14) 0.3092(4) 0.039(2) Uani 1 1 d . . . . . N2 N -0.0336(10) 0.4646(13) 0.3671(4) 0.047(2) Uani 1 1 d . . . . . N3 N -0.0384(15) 0.500000 0.250000 0.045(3) Uani 1 2 d S T P . . N4 N -0.2737(12) 0.5140(17) 0.1930(5) 0.049(3) Uani 1 1 d . . . . . C1 C 0.2660(18) 0.500000 0.250000 0.032(3) Uani 1 2 d S T P . . C2 C 0.0432(12) 0.4795(15) 0.3096(5) 0.039(2) Uani 1 1 d . . . . . C3 C -0.2009(19) 0.500000 0.250000 0.048(4) Uani 1 2 d S T P . . C4 C -0.1898(13) 0.5311(17) 0.1363(5) 0.047(3) Uani 1 1 d . . . . . O3 O 0.2239(10) 0.466(2) 0.4464(4) 0.076(4) Uani 1 1 d . . . . . H3A H 0.147796 0.516700 0.435475 0.114 Uiso 1 1 d R U . . . H3B H 0.239276 0.452820 0.486665 0.114 Uiso 1 1 d R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.0426(4) 0.0426(4) 0.0178(4) 0.0009(2) -0.0009(2) 0.0010(3) O1 0.040(5) 0.036(5) 0.022(5) 0.002(4) 0.000 0.000 O2 0.045(4) 0.105(8) 0.016(3) 0.008(5) -0.003(3) 0.018(5) N1 0.043(5) 0.052(6) 0.021(5) 0.003(4) 0.000(3) -0.006(4) N2 0.043(5) 0.079(7) 0.019(4) 0.004(5) 0.003(4) -0.013(4) N3 0.048(7) 0.069(9) 0.017(6) 0.003(6) 0.000 0.000 N4 0.046(5) 0.078(8) 0.025(5) 0.005(5) -0.002(4) 0.006(5) C1 0.050(8) 0.025(7) 0.021(7) 0.004(5) 0.000 0.000 C2 0.042(5) 0.056(6) 0.020(5) 0.008(4) -0.001(4) -0.002(5) C3 0.045(8) 0.077(14) 0.021(8) 0.005(7) 0.000 0.000 C4 0.045(5) 0.078(8) 0.017(5) 0.008(5) 0.003(4) 0.011(5) O3 0.040(4) 0.170(13) 0.018(4) 0.008(6) -0.002(3) 0.025(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -3.1807 10.9079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 O1 Nd1 O1 177.5(3) 3_655 . O1 Nd1 N1 127.92(18) . 7 O1 Nd1 N1 50.2(3) . . O1 Nd1 N1 50.2(3) 3_655 7 O1 Nd1 N1 127.92(19) 3_655 . O1 Nd1 N4 68.7(3) 3_655 3_665 O1 Nd1 N4 68.7(3) . 6_665 O1 Nd1 N4 113.2(2) 3_655 6_665 O1 Nd1 N4 113.2(2) . 3_665 O1 Nd1 C1 23.7(3) 3_655 3_655 O1 Nd1 C1 23.7(3) . . O1 Nd1 C1 154.4(2) 3_655 . O1 Nd1 C1 154.4(2) . 3_655 O2 Nd1 O1 62.88(17) 6_665 3_655 O2 Nd1 O1 62.88(17) 3_665 . O2 Nd1 O1 119.0(3) 3_665 3_655 O2 Nd1 O1 119.0(3) 6_665 . O2 Nd1 O2 98.7(5) 6_665 3_665 O2 Nd1 N1 76.3(3) 3_665 . O2 Nd1 N1 169.2(2) 6_665 . O2 Nd1 N1 169.2(2) 3_665 7 O2 Nd1 N1 76.3(3) 6_665 7 O2 Nd1 N4 76.7(4) 3_665 6_665 O2 Nd1 N4 50.3(3) 6_665 6_665 O2 Nd1 N4 76.7(4) 6_665 3_665 O2 Nd1 N4 50.3(3) 3_665 3_665 O2 Nd1 C1 66.7(2) 3_665 . O2 Nd1 C1 66.7(2) 6_665 3_655 O2 Nd1 C1 142.7(3) 3_665 3_655 O2 Nd1 C1 142.7(3) 6_665 . N1 Nd1 N1 110.3(5) 7 . N1 Nd1 N4 118.9(3) . 6_665 N1 Nd1 N4 106.2(4) . 3_665 N1 Nd1 N4 106.2(4) 7 6_665 N1 Nd1 N4 118.9(3) 7 3_665 N1 Nd1 C1 122.9(2) 7 . N1 Nd1 C1 122.9(2) . 3_655 N1 Nd1 C1 26.5(3) 7 3_655 N1 Nd1 C1 26.5(3) . . N4 Nd1 N4 96.4(6) 3_665 6_665 N4 Nd1 C1 92.4(3) 3_665 3_655 N4 Nd1 C1 111.6(3) 6_665 3_655 N4 Nd1 C1 92.4(3) 6_665 . N4 Nd1 C1 111.6(3) 3_665 . C1 Nd1 C1 144.2(3) . 3_655 O3 Nd1 O1 115.0(3) . . O3 Nd1 O1 63.42(19) 7 . O3 Nd1 O1 115.0(3) 7 3_655 O3 Nd1 O1 63.42(19) . 3_655 O3 Nd1 O2 125.5(2) . 6_665 O3 Nd1 O2 98.7(5) 7 6_665 O3 Nd1 O2 125.5(2) 7 3_665 O3 Nd1 O2 98.7(5) . 3_665 O3 Nd1 N1 65.2(3) . . O3 Nd1 N1 77.2(4) 7 . O3 Nd1 N1 77.2(4) . 7 O3 Nd1 N1 65.1(3) 7 7 O3 Nd1 N4 76.0(4) 7 6_665 O3 Nd1 N4 172.3(5) 7 3_665 O3 Nd1 N4 76.0(4) . 3_665 O3 Nd1 N4 172.3(5) . 6_665 O3 Nd1 C1 68.3(3) 7 . O3 Nd1 C1 91.4(3) . . O3 Nd1 C1 68.3(3) . 3_655 O3 Nd1 C1 91.4(3) 7 3_655 O3 Nd1 O3 111.7(8) 7 . Nd1 O1 Nd1 160.7(4) . 4_564 C1 O1 Nd1 99.6(2) . 4_564 C1 O1 Nd1 99.6(2) . . C4 O2 Nd1 102.7(6) . 4_464 C1 N1 Nd1 92.9(7) . . C2 N1 Nd1 149.6(7) . . C2 N1 C1 117.4(10) . . C2 N2 C4 116.7(9) . 6_565 C2 N3 C2 119.6(13) . 6_565 C2 N3 C3 120.2(6) 6_565 . C2 N3 C3 120.2(6) . . C3 N4 Nd1 149.5(9) . 4_464 C3 N4 C4 119.1(11) . . C4 N4 Nd1 91.3(6) . 4_464 Nd1 C1 Nd1 113.3(5) 4_564 . O1 C1 Nd1 56.6(2) . . O1 C1 Nd1 56.6(2) . 4_564 O1 C1 N1 117.2(7) . 6_565 O1 C1 N1 117.2(7) . . N1 C1 Nd1 60.6(5) . . N1 C1 Nd1 60.6(5) 6_565 4_564 N1 C1 Nd1 173.7(9) . 4_564 N1 C1 Nd1 173.7(9) 6_565 . N1 C1 N1 125.5(14) . 6_565 N1 C2 N2 119.9(10) . . N1 C2 N3 120.0(10) . . N2 C2 N3 120.1(10) . . N4 C3 N3 118.6(8) 6_565 . N4 C3 N3 118.6(8) . . N4 C3 N4 122.7(16) . 6_565 O2 C4 Nd1 53.5(6) . 4_464 O2 C4 N2 119.0(10) . 6_565 O2 C4 N4 115.7(10) . . N2 C4 Nd1 172.2(8) 6_565 4_464 N2 C4 N4 125.3(10) 6_565 . N4 C4 Nd1 62.2(6) . 4_464 Nd1 O3 H3A 120.8 . . Nd1 O3 H3B 115.4 . . H3A O3 H3B 117.7 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Nd1 O1 2.5732(17) 3_655 Nd1 O1 2.5732(17) . Nd1 O2 2.505(8) 6_665 Nd1 O2 2.505(8) 3_665 Nd1 N1 2.650(9) . Nd1 N1 2.650(9) 7 Nd1 N4 2.690(10) 6_665 Nd1 N4 2.690(10) 3_665 Nd1 C1 3.038(8) 3_655 Nd1 C1 3.038(8) . Nd1 O3 2.491(9) 7 Nd1 O3 2.491(9) . O1 C1 1.240(19) . O2 C4 1.257(13) . N1 C1 1.357(11) . N1 C2 1.305(15) . N2 C2 1.340(13) . N2 C4 1.352(15) 6_565 N3 C2 1.401(12) 6_565 N3 C2 1.401(12) . N3 C3 1.40(2) . N4 C3 1.314(12) . N4 C4 1.359(14) . O3 H3A 0.8199 . O3 H3B 0.8276 . 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 _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O3 H3A N2 0.82 2.13 2.737(13) 130.5 . yes O3 H3B O2 0.83 1.96 2.786(11) 171.7 2_565 yes 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Nd1 O1 C1 Nd1 180.000(2) 4_564 . . . Nd1 O1 C1 Nd1 180.000(1) . . . 4_564 Nd1 O1 C1 N1 178.4(6) . . . 6_565 Nd1 O1 C1 N1 178.4(6) 4_564 . . . Nd1 O1 C1 N1 -1.6(6) 4_564 . . 6_565 Nd1 O1 C1 N1 -1.6(6) . . . . Nd1 O2 C4 N2 -177.4(11) 4_464 . . 6_565 Nd1 O2 C4 N4 1.2(14) 4_464 . . . Nd1 N1 C1 O1 1.6(5) . . . . Nd1 N1 C1 N1 -178.4(5) . . . 6_565 Nd1 N1 C2 N2 -2(3) . . . . Nd1 N1 C2 N3 176.8(11) . . . . Nd1 N4 C3 N3 -176.4(13) 4_464 . . . Nd1 N4 C3 N4 3.6(13) 4_464 . . 6_565 Nd1 N4 C4 O2 -1.1(13) 4_464 . . . Nd1 N4 C4 N2 177.4(14) 4_464 . . 6_565 C1 N1 C2 N2 -176.9(10) . . . . C1 N1 C2 N3 2.4(18) . . . . C2 N1 C1 Nd1 177.2(14) . . . . C2 N1 C1 O1 178.8(9) . . . . C2 N1 C1 N1 -1.2(9) . . . 6_565 C2 N3 C2 N1 -1.3(10) 6_565 . . . C2 N3 C2 N2 178.0(14) 6_565 . . . C2 N3 C3 N4 2.4(9) . . . 6_565 C2 N3 C3 N4 -177.6(9) . . . . C2 N3 C3 N4 2.4(9) 6_565 . . . C2 N3 C3 N4 -177.6(9) 6_565 . . 6_565 C3 N3 C2 N1 178.7(10) . . . . C3 N3 C2 N2 -2.0(14) . . . . C3 N4 C4 Nd1 -177.5(14) . . . 4_464 C3 N4 C4 O2 -178.7(13) . . . . C3 N4 C4 N2 0(2) . . . 6_565 C4 N2 C2 N1 179.8(13) 6_565 . . . C4 N2 C2 N3 0.6(18) 6_565 . . . C4 N4 C3 N3 -1.3(15) . . . . C4 N4 C3 N4 178.7(15) . . . 6_565 _cod_database_fobs_code 4350822