#------------------------------------------------------------------------------ #$Date: 2026-07-10 18:09:31 +0100 (Fri, 10 Jul 2026) $ #$Revision: 306697 $ #$URL: svn://www.crystallography.net/cod/cif/3/00/06/3000619.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_3000619 loop_ _publ_author_name 'Soshi Hirota' 'Haruki Sugiyama' 'Nao Hirata' 'Sachiko Nakano' 'Junichi Usuba' 'Yuh Hijikata' 'Ryotaro Matsuda' 'Takanori Nakane' 'Akihiro Kawamoto' 'Genji Kurisu' 'Yasutomo Segawa' _publ_section_title ; Crystalline 3D covalent organic frameworks with nbo topology ; _journal_name_full 'Science Advances' _journal_page_first aeg6230 _journal_paper_doi 10.1126/sciadv.aeg6230 _journal_year 2026 _chemical_formula_moiety 'C22 H20 B O4, 1[C8NH16]' _chemical_formula_sum 'C30 H36 B N O4' _chemical_formula_weight 485.432 _space_group_crystal_system cubic _space_group_IT_number 229 _space_group_name_Hall '-I 4 2 3' _space_group_name_H-M_alt 'I m -3 m' _symmetry_Int_Tables_number 229 _atom_sites_solution_primary dual _audit_creation_date 2025-09-26 _audit_creation_method ; Olex2 1.5-alpha (compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7317) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 12 _cell_length_a 25.2887(3) _cell_length_b 25.2887(3) _cell_length_c 25.2887(3) _cell_measurement_reflns_used 93157 _cell_measurement_temperature 79 _cell_measurement_theta_max 0.9090983812130389 _cell_measurement_theta_min 0.11986258219100374 _cell_volume 16172.6(3) _computing_molecular_graphics 'Olex2 1.5-alpha (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5-alpha (Dolomanov et al., 2009)' _computing_structure_refinement 'olex2.refine 1.5-alpha (Bourhis et al., 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 79 _diffrn_detector 'Falcon 3 direct electron camera (integration mode)' _diffrn_detector_type CMOS _diffrn_measured_fraction_theta_full 0.9952 _diffrn_measured_fraction_theta_max 0.9960 _diffrn_measurement_device_type 'Talos Arctica electron microscope' _diffrn_measurement_method 'continuous rotation electron diffraction (MicroED)' _diffrn_radiation_probe electron _diffrn_radiation_type electron _diffrn_radiation_wavelength 0.02508 _diffrn_reflns_av_R_equivalents 0.4013 _diffrn_reflns_av_unetI/netI 0.0258 _diffrn_reflns_Laue_measured_fraction_full 0.9952 _diffrn_reflns_Laue_measured_fraction_max 0.9960 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 1607590 _diffrn_reflns_point_group_measured_fraction_full 0.9952 _diffrn_reflns_point_group_measured_fraction_max 0.9960 _diffrn_reflns_theta_full 0.8622 _diffrn_reflns_theta_max 0.92 _diffrn_reflns_theta_min 0.11 _diffrn_source 'Talos Arctica Field Emission Gun' _exptl_absorpt_coefficient_mu 0.000 _exptl_crystal_colour black _exptl_crystal_colour_primary black _exptl_crystal_density_diffrn 0.598 _exptl_crystal_description block _exptl_crystal_F_000 1286.616 _refine_diff_density_max 0.6202 _refine_diff_density_min -0.6546 _refine_diff_density_rms 0.0820 _refine_ls_d_res_high 0.7804 _refine_ls_d_res_low 6.3222 _refine_ls_extinction_coef 287(41) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method olex.refine _refine_ls_goodness_of_fit_ref 1.3807 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_constraints 7 _refine_ls_number_parameters 44 _refine_ls_number_reflns 1746 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.3807 _refine_ls_R_factor_all 0.1250 _refine_ls_R_factor_gt 0.1215 _refine_ls_shift/su_max 0.0005 _refine_ls_shift/su_mean 0.0002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3356 _refine_ls_wR_factor_ref 0.3386 _reflns_Friedel_coverage 0.0 _reflns_limit_h_max 18 _reflns_limit_h_min 0 _reflns_limit_k_max 32 _reflns_limit_k_min 3 _reflns_limit_l_max 22 _reflns_limit_l_min 0 _reflns_number_gt 1401 _reflns_number_total 1746 _reflns_threshold_expression I>=2u(I) _cod_data_source_file COFa.cif _cod_data_source_block COFa _cod_depositor_comments ;Extending hold period by 1 months (from 2026-06-04 to 2026-07-04) Extending hold period by 1 months (from 2026-07-04 to 2026-08-04) Releasing structure 3000619 into public domain as published material. ; _cod_original_formula_sum 'C30 H36 B1 N1 O4' _cod_database_code 3000619 _cod_database_fobs_code 3000619 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Others Fixed Sof: H5a(0.5) H5b(0.5) H6b(0.5) H6c(0.5) 3.a Secondary CH2 refined with riding coordinates: C5(H5a,H5b) 3.b Me refined with riding coordinates: C6(H6a,H6b,H6c) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 x,-z,y 3 x,z,-y 4 z,y,-x 5 -z,y,x 6 -y,x,z 7 y,-x,z 8 z,x,y 9 y,z,x 10 -y,-z,x 11 z,-x,-y 12 -y,z,-x 13 -z,-x,y 14 -z,x,-y 15 y,-z,-x 16 x,-y,-z 17 -x,y,-z 18 -x,-y,z 19 y,x,-z 20 -y,-x,-z 21 z,-y,x 22 -z,-y,-x 23 -x,z,y 24 -x,-z,-y 25 -x,-y,-z 26 -x,z,-y 27 -x,-z,y 28 -z,-y,x 29 z,-y,-x 30 y,-x,-z 31 -y,x,-z 32 -z,-x,-y 33 -y,-z,-x 34 y,z,-x 35 -z,x,y 36 y,-z,x 37 z,x,-y 38 z,-x,y 39 -y,z,x 40 -x,y,z 41 x,-y,z 42 x,y,-z 43 -y,-x,z 44 y,x,z 45 -z,y,-x 46 z,y,x 47 x,-z,-y 48 x,z,y 49 x+1/2,y+1/2,z+1/2 50 x+1/2,-z+1/2,y+1/2 51 x+1/2,z+1/2,-y+1/2 52 z+1/2,y+1/2,-x+1/2 53 -z+1/2,y+1/2,x+1/2 54 -y+1/2,x+1/2,z+1/2 55 y+1/2,-x+1/2,z+1/2 56 z+1/2,x+1/2,y+1/2 57 y+1/2,z+1/2,x+1/2 58 -y+1/2,-z+1/2,x+1/2 59 z+1/2,-x+1/2,-y+1/2 60 -y+1/2,z+1/2,-x+1/2 61 -z+1/2,-x+1/2,y+1/2 62 -z+1/2,x+1/2,-y+1/2 63 y+1/2,-z+1/2,-x+1/2 64 x+1/2,-y+1/2,-z+1/2 65 -x+1/2,y+1/2,-z+1/2 66 -x+1/2,-y+1/2,z+1/2 67 y+1/2,x+1/2,-z+1/2 68 -y+1/2,-x+1/2,-z+1/2 69 z+1/2,-y+1/2,x+1/2 70 -z+1/2,-y+1/2,-x+1/2 71 -x+1/2,z+1/2,y+1/2 72 -x+1/2,-z+1/2,-y+1/2 73 -x+1/2,-y+1/2,-z+1/2 74 -x+1/2,z+1/2,-y+1/2 75 -x+1/2,-z+1/2,y+1/2 76 -z+1/2,-y+1/2,x+1/2 77 z+1/2,-y+1/2,-x+1/2 78 y+1/2,-x+1/2,-z+1/2 79 -y+1/2,x+1/2,-z+1/2 80 -z+1/2,-x+1/2,-y+1/2 81 -y+1/2,-z+1/2,-x+1/2 82 y+1/2,z+1/2,-x+1/2 83 -z+1/2,x+1/2,y+1/2 84 y+1/2,-z+1/2,x+1/2 85 z+1/2,x+1/2,-y+1/2 86 z+1/2,-x+1/2,y+1/2 87 -y+1/2,z+1/2,x+1/2 88 -x+1/2,y+1/2,z+1/2 89 x+1/2,-y+1/2,z+1/2 90 x+1/2,y+1/2,-z+1/2 91 -y+1/2,-x+1/2,z+1/2 92 y+1/2,x+1/2,z+1/2 93 -z+1/2,y+1/2,-x+1/2 94 z+1/2,y+1/2,x+1/2 95 x+1/2,-z+1/2,-y+1/2 96 x+1/2,z+1/2,y+1/2 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_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_group C3 C 1.0 0.52797(9) 0.43136(9) 0.0317(7) Uani 1.000000 2 S T P . C1 C 1.0 0.52757(10) 0.33485(10) 0.0403(8) Uani 1.000000 2 S T P . O1 O 1.0 0.54616(10) 0.28546(9) 0.0507(8) Uani 1.000000 2 S T P . C2 C 1.0 0.55500(10) 0.38090(9) 0.0395(8) Uani 1.000000 2 S T P . B1 B 1.0 0.5 0.25 0.0330(13) Uani 1.000000 8 S T P . C4 C 1.0 0.61373(10) 0.38627(10) 0.0427(11) Uani 1.000000 4 S T P . C5 C 0.95038(14) 0.63904(9) 0.36096(9) 0.0555(10) Uani 1.000000 2 S T P . H5a H 0.95139(14) 0.67770(9) 0.36701(9) 0.0666(12) Uiso 0.500000 1 R . P . H5b H 0.95139(14) 0.63299(9) 0.32230(9) 0.0666(12) Uiso 0.500000 1 R . P . C6 C 0.90008(19) 0.61782(13) 0.38218(13) 0.0858(14) Uani 1.000000 2 S T P . H6a H 0.87027(19) 0.63532(13) 0.36468(13) 0.129(2) Uiso 0.5 1 RS T P -1 H6b H 0.89835(19) 0.57967(13) 0.37558(13) 0.129(2) Uiso 0.500000 1 R . P -1 H6c H 0.89835(19) 0.62442(13) 0.42033(13) 0.129(2) Uiso 0.500000 1 R . P -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 C3 0.0421(14) 0.0305(13) 0.0224(12) -0.000000 -0.000000 0.0042(10) C1 0.0649(18) 0.0267(13) 0.0294(14) -0.000000 -0.000000 0.0072(10) O1 0.0685(17) 0.0574(15) 0.0261(11) -0.000000 -0.000000 -0.0016(9) C2 0.0699(19) 0.0301(14) 0.0184(12) -0.000000 -0.000000 0.0007(9) B1 0.037(2) 0.037(2) 0.024(3) -0.000000 -0.000000 0.000000 C4 0.070(3) 0.0291(12) 0.0291(12) -0.000000 -0.000000 -0.0011(13) C5 0.083(3) 0.0415(11) 0.0415(11) 0.0131(11) -0.0131(11) -0.0000(13) C6 0.082(3) 0.088(2) 0.088(2) 0.0237(17) -0.0237(17) 0.008(2) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source _atom_type_scat_dispersion_source B 0.00000 0.00000 0.13000 0.52000 1.37700 0.76700 0.41800 3.92100 16.66300 51.75100 0.00000 'Custom 4-Gaussian' custom C 0.00000 0.00000 0.13600 0.54800 1.22700 0.59700 0.37300 3.28100 13.04600 41.02000 0.00000 'Custom 4-Gaussian' custom H 0.00000 0.00000 0.03700 0.12700 0.23600 0.12900 0.56100 3.79100 13.55600 37.72300 0.00000 'Custom 4-Gaussian' custom O 0.00000 0.00000 0.14300 0.51000 0.93700 0.39200 0.30500 2.26800 8.26200 25.66500 0.00000 'Custom 4-Gaussian' custom 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 C2 C1 O1 128.6(2) . . B1 O1 C1 106.9(2) 18_765 . C1 C2 C3 121.0(2) . . C4 C2 C3 113.0(2) . . C4 C2 C1 126.0(2) . . O1 B1 O1 104.95(19) . 18_765 O1 B1 O1 111.78(10) 68_665 . O1 B1 O1 111.78(10) 68_665 18_765 O1 B1 O1 111.78(10) 67_545 18_765 O1 B1 O1 111.78(10) 67_545 . O1 B1 O1 104.95(19) 68_665 67_545 C2 C4 C2 100.4(3) 24_766 . C5 C4 C2 111.98(8) . 24_766 C5 C4 C2 111.98(8) 24_766 . C5 C4 C2 111.98(8) . . C5 C4 C2 111.98(8) 24_766 24_766 C5 C4 C5 108.4(3) 24_766 . H5a C5 C4 108.90(9) 47_566 . H5a C5 C4 108.90(9) . . H5a C5 H5a 107.7 . 47_566 H5b C5 C4 108.90(9) . . H5b C5 C4 108.90(9) 47_566 . H5b C5 H5a 107.7 . . H5b C5 H5a 0.0 47_566 . H5b C5 H5a 0.0 . 47_566 H5b C5 H5a 107.7 47_566 47_566 H5b C5 H5b 107.7 47_566 . C6 C5 C4 113.4(3) . . C6 C5 H5a 108.90(10) . 47_566 C6 C5 H5a 108.90(10) . . C6 C5 H5b 108.90(10) . 47_566 C6 C5 H5b 108.90(10) . . H6a C6 C5 109.5 . . H6b C6 C5 109.5 47_566 . H6b C6 C5 109.5 . . H6b C6 H6a 109.5 47_566 . H6b C6 H6a 109.5 . . H6b C6 H6b 109.5 47_566 . H6c C6 C5 109.5 . . H6c C6 C5 109.5 47_566 . H6c C6 H6a 109.5 47_566 . H6c C6 H6a 109.5 . . H6c C6 H6b 109.5 47_566 47_566 H6c C6 H6b 0.0 47_566 . H6c C6 H6b 109.5 . . H6c C6 H6b 0.0 . 47_566 H6c C6 H6c 109.5 47_566 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 C3 C3 1.415(5) 18_765 C3 C3 1.454(5) 24_766 C3 C2 1.447(3) . C1 C1 1.394(5) 18_765 C1 O1 1.335(3) . C1 C2 1.355(4) . O1 B1 1.472(2) 18_765 C2 C4 1.491(3) . C4 C5 1.547(4) . C4 C5 1.547(4) 24_766 C5 H5a 0.9900 47_566 C5 H5a 0.9900 . C5 H5b 0.9900 . C5 H5b 0.9900 47_566 C5 C6 1.481(6) . C6 H6a 0.9800 . C6 H6b 0.9800 . C6 H6b 0.9800 47_566 C6 H6c 0.9800 47_566 C6 H6c 0.9800 . 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 C3 C3 C3 C3 0.0 . 18_765 3_556 23_755 C3 C3 C3 C3 0.0 . 24_766 2_565 17_756 C3 C3 C3 C2 180.0 2_565 24_766 . . C3 C3 C3 C2 180.0 3_556 18_765 . . C3 C3 C2 C1 0.0 18_765 . . . C3 C3 C2 C1 180.0 24_766 . . . C3 C3 C2 C4 180.0 18_765 . . . C3 C3 C2 C4 0.0 24_766 . . . C3 C2 C1 C1 0.0 . . . 18_765 C3 C2 C1 O1 180.0 . . . . C3 C2 C4 C2 0.0 . . . 24_766 C3 C2 C4 C5 -119.00(14) . . . . C3 C2 C4 C5 119.00(14) . . . 24_766 C1 C1 O1 B1 0.0 . 18_765 18_765 . C1 C1 C2 C4 180.0 18_765 . . . C1 O1 B1 O1 0.0 . . . 18_765 C1 O1 B1 O1 -121.35(12) . . . 67_545 C1 O1 B1 O1 121.35(12) . . . 68_665 C1 C2 C4 C2 180.0 . . . 24_766 C1 C2 C4 C5 -61.00(14) . . . 24_766 C1 C2 C4 C5 61.00(14) . . . . O1 C1 C1 O1 0.0 . . 18_765 18_765 O1 C1 C1 C2 180.0 . . 18_765 18_765 O1 C1 C2 C4 0.0 . . . . C2 C3 C3 C2 0.0 . . 18_765 18_765 C2 C3 C3 C2 0.0 . . 24_766 24_766 C2 C1 C1 O1 180.0 . . 18_765 18_765 C2 C1 C1 C2 0.0 . . 18_765 18_765 C2 C1 O1 B1 180.0 . . . . C2 C4 C2 C3 0.0 . . 24_766 24_766 C2 C4 C2 C1 180.0 . . 24_766 24_766 C2 C4 C2 C4 180.000(15) . . 24_766 24_766 C2 C4 C5 C4 0(210000000000000) . . 24_766 24_766 C2 C4 C5 C6 -55.97(17) . . 24_766 24_766 C2 C4 C5 C6 55.97(17) . . . . B1 O1 C1 C1 0.0 . . . 18_765 C4 C2 C3 C3 0.0 . 24_766 24_766 . C4 C2 C3 C3 180.0 24_766 . . 18_765 C4 C2 C1 C1 180.0 24_766 . . 18_765 C4 C2 C1 O1 0.0 24_766 . . . C4 C2 C4 C2 0.0 . 24_766 24_766 . C4 C2 C4 C5 -118.98(14) 24_766 . . . C4 C2 C4 C5 118.98(14) . 24_766 24_766 . C4 C5 C4 C2 0(40000000000000) 24_766 . . . C4 C5 C4 C2 0(40000000000000) . 24_766 24_766 . C4 C5 C4 C5 0(40000000000000) . 24_766 24_766 . C5 C4 C2 C3 119.00(19) . . 24_766 24_766 C5 C4 C2 C1 -61.00(19) . . 24_766 24_766 C5 C4 C2 C4 0(600000) . . 24_766 24_766 C5 C4 C5 C4 0(210000000000000) . . 24_766 24_766 C5 C4 C5 C6 -180.0 . . 24_766 24_766 C6 C5 C4 C2 -55.97(11) . . . 24_766 C6 C5 C4 C5 -180.0 . . . 24_766 loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.177 -0.197 -0.083 12300.0 343.1 '12 C8NH16'