Self-correcting mismatches in metastable hydrogen-bonded organic frameworks with an 11-fold interpenetrated array.
Xia, Guomin; Zhou, Chunlei; Xiao, Xingliang; Yang, Yang; Yu, Fuqing; Wang, Hongming; Chemical science 15 (2024) 14336–14343; doi:10.1039/d4sc02751e

data_1572303
_publ_section_title
;
 Self-correcting mismatches in metastable hydrogen-bonded organic
 frameworks with an 11-fold interpenetrated array.
;
_journal_issue                   35
_journal_name_full               'Chemical science'
_journal_page_first              14336
_journal_page_last               14343
_journal_paper_doi               10.1039/d4sc02751e
_journal_volume                  15
_journal_year                    2024
_chemical_compound_source        3,3',6,6'-tetrabromo-9,9'-bicarbazole
_chemical_formula_moiety         'C68 H36 N6 O4'
_chemical_formula_sum            'C68 H36 N6 O4'
_chemical_formula_weight         1001.03
_chemical_name_common            BC-4Np
_chemical_name_systematic
6,6',6'',6'''-([9,9'-bicarbazole]-3,3',6,6'-tetrayl)tetrakis(benzo[cd]indol-2(1H)-one)
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-24
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-12-14 deposited with the CCDC.	2024-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.381(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.685(3)
_cell_length_b                   30.037(8)
_cell_length_c                   16.640(4)
_cell_measurement_reflns_used    6065
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      51.201
_cell_measurement_theta_min      3.543
_cell_volume                     5509(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13692
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        51.468
_diffrn_reflns_theta_max         51.468
_diffrn_reflns_theta_min         3.544
_diffrn_source_current           2.86
_diffrn_source_power             0.1997996
_diffrn_source_voltage           69.86
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.388
_exptl_absorpt_correction_T_max  0.7501
_exptl_absorpt_correction_T_min  0.4910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1246 before and 0.0580 after correction.
The Ratio of minimum to maximum transmission is 0.6546.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_description       block
_exptl_crystal_F_000             2072
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'SCSC from NCU-HOF1'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         4506
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0636
_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^)+(0.1092P)^2^+2.2568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1858
_refine_ls_wR_factor_ref         0.2019
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3107
_reflns_number_total             4506
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02751e2.cif
_cod_data_source_block           11_sq
_cod_depositor_comments
'Adding full bibliography for 1572302--1572305.cif.'
_cod_database_code               1572303
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Rigid bond restraints
 C6, C7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C27, C32
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C13(H13),
 C14(H14), C16(H16), C19(H19), C20(H20), C22(H22), C24(H24), C25(H25), C29(H29),
  C30(H30), C31(H31)
;
_shelx_res_checksum              14995
_shelx_fab_checksum              61404
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'