Construction of Isostructural Hydrogen-bonded Organic Frameworks: Limitations and Possibilities of Pore Expansion
Suzuki, Yuto; GUTIÉRREZ, MARIO; Tanaka, Senri; Gomez Garcia, Eduardo; Tohnai, Norimitsu; Yasuda, Nobuhiro; Matubayasi, Nobuyuki; Douhal, Abderrazzak; Hisaki, Ichiro; Chemical Science  (2021) –; doi:10.1039/D1SC02690A

data_1563670
_publ_section_title
;
 Construction of Isostructural Hydrogen-bonded Organic Frameworks:
 Limitations and Possibilities of Pore Expansion
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC02690A
_journal_year                    2021
_chemical_formula_moiety         'C102 H60 N6 O12'
_chemical_formula_sum            'C102 H60 N6 O12'
_chemical_formula_weight         1561.56
_chemical_name_common            TolHAT
_chemical_name_systematic
'4,4',4'',4''',4'''',4'''''-((dipyrazino[2,3-f:2',3'-h]quinoxaline-2,3,6,7,10,11-hexaylhexakis(benzene-4,1-diyl))hexakis(ethyne-2,1-diyl))hexabenzoic acid'
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2021-04-30 deposited with the CCDC.	2021-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                120.0000
_cell_formula_units_Z            6
_cell_length_a                   59.5294(11)
_cell_length_b                   59.5294(11)
_cell_length_c                   6.96369(19)
_cell_measurement_reflns_used    5371
_cell_measurement_temperature    90
_cell_measurement_theta_max      25.07
_cell_measurement_theta_min      1.56
_cell_volume                     21371.4(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_structure_refinement  'SHELXL Version 2018/1 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'SPring-8 BL40XU, Pilatus100K, DECTRIS'
_diffrn_measurement_method       \w
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.81106
_diffrn_reflns_av_R_equivalents  0.1398
_diffrn_reflns_av_unetI/netI     0.1082
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       80
_diffrn_reflns_limit_h_min       -79
_diffrn_reflns_limit_k_max       78
_diffrn_reflns_limit_k_min       -76
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            66289
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        29.120
_diffrn_reflns_theta_max         33.379
_diffrn_reflns_theta_min         1.561
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.194
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellowishgreen
_exptl_crystal_density_diffrn    0.728
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4824.00
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: N,N-dimethylacetamide, 1,2,4-trichlorobenzene'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.61
_refine_diff_density_min         -0.49
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.265
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     181
_refine_ls_number_reflns         5840
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.1994
_refine_ls_R_factor_gt           0.1267
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3874
_refine_ls_wR_factor_ref         0.4200
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2556
_reflns_number_total             5840
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d1sc02690a2.cif
_cod_data_source_block           TolHAT-1
_cod_original_sg_symbol_H-M      'R -3 c:H'
_cod_database_code               1563670
_shelx_res_checksum              19666
_shelx_hkl_checksum              53382
_shelx_fab_checksum              5422