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_1572304
_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, C2 H4'
_chemical_formula_sum            'C70 H40 N6 O4'
_chemical_formula_weight         1029.08
_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             2022-11-29
_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                 108.819(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6021(19)
_cell_length_b                   30.046(4)
_cell_length_c                   16.575(2)
_cell_measurement_reflns_used    4930
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      53.24
_cell_measurement_theta_min      3.54
_cell_volume                     5469.1(14)
_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      193.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.925
_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  0.0564
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16530
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.111
_diffrn_reflns_theta_min         2.559
_diffrn_source                   MetalJet
_diffrn_source_current           2.86
_diffrn_source_power             0.19931339999999997
_diffrn_source_type              'Liquid Metal source'
_diffrn_source_voltage           69.69
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.399
_exptl_absorpt_correction_T_max  0.7518
_exptl_absorpt_correction_T_min  0.4943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1116 before and 0.0671 after correction.
The Ratio of minimum to maximum transmission is 0.6575.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       block
_exptl_crystal_F_000             2136
_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         0.531
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5721
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1740
_refine_ls_R_factor_gt           0.1105
_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^)+(0.1200P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2831
_refine_ls_wR_factor_ref         0.3232
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2839
_reflns_number_total             5721
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02751e2.cif
_cod_data_source_block           221128li_lidz217170_0m
_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_original_cell_volume        5469.2(14)
_cod_database_code               1572304
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.950
_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
 C38-C37
 1.35 with sigma of 0.005
 C35-C36
 1.35 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C36 \\sim C35: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C38 \\sim C37: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C2 \\sim C11: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
C3 \\sim C4: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
within 2A
C10 \\sim N1: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
Uanis(C36) \\sim Ueq, Uanis(C35) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: C37(0.25) H37A(0.25) H37B(0.25) C38(0.25) H38A(0.25) H38B(0.25)
 C35(0.25) H35A(0.25) H35B(0.25) C36(0.25) H36A(0.25) H36B(0.25)
5.a Riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B), C35(H35A,H35B), C36(H36A,H36B)
5.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C30(H30), C25(H25), N1(H1), C26(H26), C9(H9), C23(H23), C21(H21),
 C20(H20), C8(H8), C17(H17), C32(H32), C14(H14), C31(H31), C13(H13), C4(H4),
 C5(H5), C3(H3)
;
_shelx_res_checksum              31082
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU