Steric hindrance regulation in hydrogen-bonded organic frameworks: from nonporous to microporous.
Wang, Xiaokang; Liu, Hongyan; Sun, Meng; Gao, Fei; Feng, Xueying; Xu, Mingming; Fan, Weidong; Sun, Daofeng; Chemical communications (Cambridge, England) 61 (2025) 10538–10541; doi:10.1039/d5cc02617b

data_7134720
_publ_section_title
;
 Steric hindrance regulation in hydrogen-bonded organic frameworks: from
 nonporous to microporous.
;
_journal_issue                   57
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10538
_journal_page_last               10541
_journal_paper_doi               10.1039/d5cc02617b
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C22 H16 O6, C3 H7 N O, 0.625[C3H7NO]'
_chemical_formula_sum            'C26.88 H27.38 N1.62 O7.62'
_chemical_formula_weight         495.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2yc'
_space_group_name_H-M_alt        'I 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-06-03
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-06-03 deposited with the CCDC.	2025-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.418(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.5252(19)
_cell_length_b                   7.1491(5)
_cell_length_c                   30.553(2)
_cell_measurement_reflns_used    3014
_cell_measurement_temperature    294.8(6)
_cell_measurement_theta_max      69.8190
_cell_measurement_theta_min      3.7490
_cell_volume                     5138.5(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip  (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      294.8(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -22.00  69.00   1.00    7.50    --    0.00  57.00 120.00   91
  2  \w    -69.00  22.00   1.00    7.50    --    0.00 -57.00   0.00   91
  3  \w     92.00 122.00   1.00   25.00    --   53.63  57.00 -30.00   30
  4  \w    -15.00  26.00   1.00   25.00    --   53.63 -57.00-180.00   41
  5  \w    -15.00  73.00   1.00   25.00    --   53.63 -57.00-150.00   88
  6  \w     20.00  66.00   1.00   25.00    --   53.63 -57.00 -90.00   46
  7  \w    -15.00  56.00   1.00   25.00    --   53.63 -57.00  90.00   71
  8  \w     79.00 116.00   1.00   25.00    --  107.26 -63.00  90.00   37
  9  \w     52.00 147.00   1.00   25.00    --  107.26 -25.00-120.00   95
 10  \w     85.00 115.00   1.00   25.00    --  107.26  38.00 -90.00   30
 11  \w     97.00 123.00   1.00   25.00    --  107.26 -63.00-120.00   26
 12  \w    101.00 172.00   1.00   25.00    --  107.26 111.00-150.00   71
 13  \w    127.00 178.00   1.00   25.00    --  107.26 111.00-120.00   51
 14  \w     40.00  85.00   1.00   25.00    --  107.26 -63.00-120.00   45
 15  \w     39.00 134.00   1.00   25.00    --  107.26 -38.00  90.00   95
 16  \w    124.00 175.00   1.00   25.00    --  107.26  38.00 -90.00   51
 17  \w     46.00  72.00   1.00   25.00    --  107.26 -50.00 -30.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0459283000
_diffrn_orient_matrix_UB_12      -0.0433376000
_diffrn_orient_matrix_UB_13      -0.0240488000
_diffrn_orient_matrix_UB_21      -0.0353250000
_diffrn_orient_matrix_UB_22      0.1027160000
_diffrn_orient_matrix_UB_23      -0.0430100000
_diffrn_orient_matrix_UB_31      0.0305020000
_diffrn_orient_matrix_UB_32      0.1844307000
_diffrn_orient_matrix_UB_33      0.0183068000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            9639
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        66.598
_diffrn_reflns_theta_max         66.598
_diffrn_reflns_theta_min         3.758
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.783
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68267
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       block
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.678
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.293
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.816
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         4613
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.816
_refine_ls_R_factor_all          0.1436
_refine_ls_R_factor_gt           0.1324
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4163
_refine_ls_wR_factor_ref         0.4338
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3664
_reflns_number_total             4613
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc02617b2.cif
_cod_data_source_block           UPC-HOF-15
_cod_depositor_comments
'Adding full bibliography for 7134720--7134721.cif.'
_cod_database_code               7134720
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O'
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.926
_reflns_odcompleteness_completeness 99.42
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9660(19)
 0.0340(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
3. Others
 Fixed Sof: O2(0.5) O1(0.5) H1(0.5) H25(0.5) H25A(0.5) O1A(0.5) H1A(0.5)
 O2A(0.5) O7(0.5) O7A(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C22(H22), C21(H21), C3(H3A), C12(H12), C19(H19), C18(H18), C15(H15), C14(H14),
  C11(H11), C7(H7), C25(H25), C25(H25A)
4.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C8(H8A,H8B,H8C)
4.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O3(H3), O5(H5), O1A(H1A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              90432
_shelx_hkl_checksum              33002
_shelx_fab_checksum              83163
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.607
_oxdiff_exptl_absorpt_empirical_full_min 0.754