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_1572302
_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           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-11
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-12-14 deposited with the CCDC.	2024-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.150(7)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   16.6654(17)
_cell_length_b                   38.187(4)
_cell_length_c                   29.129(3)
_cell_measurement_reflns_used    9877
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      56.33
_cell_measurement_theta_min      2.52
_cell_volume                     18510(3)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'APEX4 V2021.10-0 (Bruker, 2021)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Metaljet PHOTON II'
_diffrn_measurement_method       '\w and \f shutterless scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_monochromator  'Helios Multi-layer Optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.1273
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            298664
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.907
_diffrn_reflns_theta_min         2.013
_diffrn_source                   MetalJet
_diffrn_source_current           2.86
_diffrn_source_power             0.19937059999999998
_diffrn_source_type              'Liquid Metal source'
_diffrn_source_voltage           69.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.346
_exptl_absorpt_correction_T_max  0.7439
_exptl_absorpt_correction_T_min  0.6197
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1655 before and 0.1112 after correction.
The Ratio of minimum to maximum transmission is 0.8330.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.078
_exptl_crystal_description       block
_exptl_crystal_F_000             6216
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DMF/Acetone'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1054
_refine_ls_number_reflns         16920
_refine_ls_number_restraints     272
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.2026
_refine_ls_R_factor_gt           0.1469
_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^)+(0.0600P)^2^+100.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3193
_refine_ls_wR_factor_ref         0.3485
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9031
_reflns_number_total             16920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02751e2.cif
_cod_data_source_block           a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1572302--1572305.cif.
;
_cod_database_code               1572302
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.956
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 O1-C1
 1.25 with sigma of 0.005
 C46-C102
 1.53 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
N4 \\sim C67 \\sim O3 \\sim C66 \\sim C65 \\sim C64 \\sim C63 \\sim C62 \\sim
C61 \\sim C60 \\sim C59 \\sim C58 \\sim C57: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C50 \\sim C51 \\sim C55 \\sim C56 \\sim C49 \\sim N3 \\sim C48 \\sim C47 \\sim
C46 \\sim C52 \\sim C53 \\sim C54 \\sim O4: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C2 \\sim C3
\\sim C4 \\sim C1 \\sim N1 \\sim O1: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
4.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), C21(H21), C25(H25), C26(H26), C20(H20), C30(H30), C23(H23),
 C31(H31), N1(H1), C32(H32), C17(H17), C52(H52), C53(H53), C8(H8), C47(H47),
 C44(H44), C36(H36), C42(H42), C9(H9), C39(H39), N3(H3), C48(H48), C5(H5),
 C14(H14), C13(H13), C54(H54), C37(H37), C43(H43), C63(H63), C58(H58), C59(H59),
  C64(H64), C65(H65), C3(H3A), C4(H4A), N8(H8A), C81(H81), C84(H84), C80(H80),
 N7(H7), C87(H87), C90(H90), C93(H93), C72(H72), C77(H77), C92(H92), C76(H76),
 C97(H97), C99(H99), C71(H71), C88(H88), C70(H70), C98(H98)
;
_shelx_res_checksum              88852
_shelx_fab_checksum              14075
_olex2_submission_special_instructions 'No special instructions were received'