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_1572305
_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         '2(C68 H36 N6 O4), 3.5(C2 H4)'
_chemical_formula_sum            'C143 H86 N12 O8'
_chemical_formula_weight         2100.23
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-14
_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                 109.751(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.729(3)
_cell_length_b                   30.677(9)
_cell_length_c                   16.645(4)
_cell_measurement_reflns_used    9795
_cell_measurement_temperature    275.00
_cell_measurement_theta_max      54.31
_cell_measurement_theta_min      2.51
_cell_volume                     5637(3)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'APEX4 V2022.1-1 (Bruker, 2022)'
_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      275.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_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  0.0531
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            114357
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         57.652
_diffrn_reflns_theta_min         2.506
_diffrn_source                   MetalJet
_diffrn_source_current           2.23
_diffrn_source_power             0.1554533
_diffrn_source_type              'Liquid Metal source'
_diffrn_source_voltage           69.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.393
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.6631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0938 before and 0.0614 after correction.
The Ratio of minimum to maximum transmission is 0.8827.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_description       block
_exptl_crystal_F_000             2184
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'C2H4 gas diffuse into NCU-HOF1a crystal'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         5844
_refine_ls_number_restraints     113
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1183
_refine_ls_R_factor_gt           0.0942
_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^)+(0.1500P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2587
_refine_ls_wR_factor_ref         0.2843
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3867
_reflns_number_total             5844
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02751e2.cif
_cod_data_source_block           a_CCDC1
_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               1572305
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.951
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 C37-C38
 1.35 with sigma of 0.005
 C35-C36
 1.35 with sigma of 0.005
 C44-C43
 1.35 with sigma of 0.005
 C42-C41
 1.35 with sigma of 0.005
 C39-C40
 1.35 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C37 \\sim C38 \\sim C35 \\sim C36: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01 within 2A
C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
C29 \\sim C28: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
C8 \\sim N1: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
within 2A
4. Others
 Fixed Sof: C36(0.25) H36A(0.25) H36B(0.25) C35(0.25) H35A(0.25) H35B(0.25)
 C38(0.25) H38A(0.25) H38B(0.25) C37(0.25) H37A(0.25) H37B(0.25) C40(0.125)
 H40A(0.125) H40B(0.125) C41(0.125) H41A(0.125) H41B(0.125) C42(0.125)
 H42A(0.125) H42B(0.125) C39(0.125) H39A(0.125) H39B(0.125) C43(0.125)
 H43A(0.125) H43B(0.125) C44(0.125) H44A(0.125) H44B(0.125)
5.a Riding coordinates:
 C36(H36A,H36B), C35(H35A,H35B), C38(H38A,H38B), C37(H37A,H37B), C40(H40A,
 H40B), C41(H41A,H41B), C42(H42A,H42B), C39(H39A,H39B), C43(H43A,H43B),
 C44(H44A,H44B)
5.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C17(H17), N3(H3), C25(H25), C26(H26), C23(H23), C5(H5), C14(H14),
 C20(H20), C13(H13), C10(H10), C9(H9), C21(H21), C33(H33), C31(H31), C3(H3A),
 C32(H32), C4(H4)
;
_shelx_res_checksum              40574
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU