A V-shaped small molecule-based crystalline nonporous supramolecular organic framework for capturing benzene-based contaminants
Chen, Jin-Fa; Wang, Yuxuan; Shi, Bingbing; Yao, Hong; Wei, Tai-Bao; Lin, Qi; Chemical Communications 61 (2025) 9912–9915; doi:10.1039/D5CC01950H

data_7134625
_publ_section_title
;
 A V-shaped small molecule-based crystalline nonporous supramolecular
 organic framework for capturing benzene-based contaminants
;
_journal_issue                   54
_journal_name_full               'Chemical Communications'
_journal_page_first              9912
_journal_page_last               9915
_journal_paper_doi               10.1039/D5CC01950H
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C48 H30 N4, 3(C6 H6)'
_chemical_formula_sum            'C66 H48 N4'
_chemical_formula_weight         897.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-05-27
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-05-27 deposited with the CCDC.	2025-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.111(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.0124(7)
_cell_length_b                   9.1087(2)
_cell_length_c                   19.0026(4)
_cell_measurement_reflns_used    10692
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      75.4840
_cell_measurement_theta_min      1.6040
_cell_volume                     4799.45(19)
_computing_cell_refinement       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.918
_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   -107.00 -74.00   0.50    0.32    -- -100.00  77.00-180.00   66
  2  \w    -65.00 -26.00   0.50    0.32    -- -100.00  77.00-180.00   78
  3  \w    -73.00 -26.00   0.50    0.32    -- -100.00  61.00-180.00   94
  4  \w    -60.00 -27.00   0.50    0.32    -- -100.00  61.00-120.00   66
  5  \w    -53.00 -27.00   0.50    0.32    -- -100.00  45.00   0.00   52
  6  \w    -54.00 -25.00   0.50    0.32    -- -100.00  45.00  60.00   58
  7  \w    -74.00 -48.00   0.50    0.32    -- -100.00  61.00 120.00   52
  8  \w    -52.00 -25.00   0.50    0.32    -- -100.00  45.00 150.00   54
  9  \w    -69.00 -37.00   0.50    0.32    -- -100.00 125.00  60.00   64
 10  \w    -55.00 -29.00   0.50    0.32    -- -100.00 125.00  30.00   52
 11  \w   -111.00 -68.00   0.50    0.32    -- -100.00 125.00  30.00   86
 12  \w   -104.00 -78.00   0.50    0.32    -- -100.00 125.00  60.00   52
 13  \w   -119.00 -32.00   0.50    0.61    --  -44.63 -12.00-133.00  174
 14  \w   -159.00 -54.00   0.50    0.32    -- -100.00 -12.00-133.00  210
 15  \w   -120.00 -67.00   0.50    0.61    --  -44.63-179.00 120.00  106
 16  \w     39.00  68.00   0.50    0.32    --  111.16 -61.00  60.00   58
 17  \w     42.00  67.00   0.50    0.32    --  111.16 -61.00  30.00   50
 18  \w    -11.00  20.00   0.50    0.61    --   44.63 -19.00  60.00   62
 19  \w     39.00  64.00   0.50    0.32    --  111.16 -61.00 -90.00   50
 20  \w    -30.00  -5.00   0.50    0.61    --   44.63 -12.00-133.00   50
 21  \w     64.00 102.00   0.50    0.32    --  111.16-125.00-180.00   76
 22  \w     49.00  79.00   0.50    0.32    --  111.16 -94.00  30.00   60
 23  \w     65.00 145.00   0.50    0.32    --  111.16  12.00  38.00  160
 24  \w    105.00 150.00   0.50    0.32    --  111.16  30.00 150.00   90
 25  \w     16.00 121.00   0.50    0.61    --   44.63  12.00  38.00  210
 26  \w    -21.00   4.00   0.50    0.61    --  -44.63  12.00  38.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0518004000
_diffrn_orient_matrix_UB_12      0.0179237000
_diffrn_orient_matrix_UB_13      0.0513410000
_diffrn_orient_matrix_UB_21      -0.0185292000
_diffrn_orient_matrix_UB_22      -0.0204931000
_diffrn_orient_matrix_UB_23      0.0674784000
_diffrn_orient_matrix_UB_31      0.0078473000
_diffrn_orient_matrix_UB_32      -0.1668818000
_diffrn_orient_matrix_UB_33      -0.0027726000
_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  0.0619
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9510
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.716
_diffrn_reflns_theta_min         1.593
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.555
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         9510
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.1168
_refine_ls_R_factor_gt           0.0962
_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^)+(0.0749P)^2^+12.7288P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2730
_refine_ls_wR_factor_ref         0.2824
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6997
_reflns_number_total             9510
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01950h2.cif
_cod_data_source_block           yxw-kz-bz_1021_auto_tw
_cod_depositor_comments
'Adding full bibliography for 7134621--7134626.cif.'
_cod_database_code               7134625
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.921
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.66403
 0.33597
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C9(H9), C11(H11), C12(H12), C14(H14), C19(H19),
 C21(H21), C23(H23), C24(H24), C26(H26), C28(H28), C30(H30), C33(H33), C37(H37),
  C38(H38), C39(H39), C42(H42), C45(H45), C48(H48), C51(H51), C52(H52),
 C55(H55), C58(H58), C59(H59), C60(H60), C63(H63), C65(H65), C66(H66), C2(H2),
 C5(H5), C31(H31), C35(H35), C47(H47), C53(H53), C13(H13), C15(H15), C27(H27),
 C29(H29), C49(H49), C57(H57), C17(H17), C25(H25), C41(H41), C43(H43), C61(H61),
  C64(H64)
;
_shelx_res_checksum              26657
_shelx_hkl_checksum              95179
_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 2.053
_oxdiff_exptl_absorpt_empirical_full_min 0.633