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_7134623
_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_absolute_configuration unk
_chemical_formula_moiety         'C48 H30 N4, C8 H10'
_chemical_formula_sum            'C56 H40 N4'
_chemical_formula_weight         768.92
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-09-01
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2025-04-25 deposited with the CCDC.	2025-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9030(2)
_cell_length_b                   28.7810(4)
_cell_length_c                   8.88980(10)
_cell_measurement_reflns_used    17241
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      76.2990
_cell_measurement_theta_min      3.1490
_cell_volume                     4068.90(9)
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.973
_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     59.00  97.00   0.50    0.17    --   46.68 155.00 128.00   76
  2  \w     83.00 153.00   0.50    0.32    --  104.75 119.00 -27.00  140
  3  \w     72.00 102.00   0.50    0.32    --  104.75 -94.00-120.00   60
  4  \w     39.00  64.00   0.50    0.32    --  104.75 -61.00-120.00   50
  5  \w    -25.00  56.00   0.50    0.17    --   46.68 -55.00 120.00  162
  6  \w    -25.00   0.00   0.50    0.17    --  -46.68  19.00  90.00   50
  7  \w    -77.00 -32.00   0.50    0.32    -- -102.00  66.00  93.00   90
  8  \w    -69.00 -31.00   0.50    0.32    -- -102.00  61.00  60.00   76
  9  \w    -69.00 -41.00   0.50    0.32    -- -102.00  61.00  30.00   56
 10  \w    -61.00 -30.00   0.50    0.32    -- -102.00  55.00 -96.00   62
 11  \w    -37.00   1.00   0.50    0.17    --  -46.68  37.00   0.00   76
 12  \w   -158.00 -99.00   0.50    0.32    -- -102.00 -15.00  60.00  118
 13  \w   -174.00-146.00   0.50    0.32    -- -102.00 -55.00 120.00   56
 14  \w   -126.00 -88.00   0.50    0.32    -- -102.00 -55.00 120.00   76
 15  \w    -86.00 -37.00   0.50    0.32    -- -102.00 155.00 128.00   98
 16  \w    -39.00 -10.00   0.50    0.17    --  -46.68  37.00  30.00   58
 17  \w     -6.00  22.00   0.50    0.17    --  -46.68  37.00  30.00   56
 18  \w    -59.00 -33.00   0.50    0.32    -- -102.00  61.00 -60.00   52
 19  \w     52.00 105.00   0.50    0.32    --  104.75 -94.00  90.00  106
 20  \w    142.00 176.00   0.50    0.32    --  104.75  30.00-150.00   68
 21  \w     94.00 120.00   0.50    0.32    --  104.75  30.00  30.00   52
 22  \w     36.00  63.00   0.50    0.32    --  104.75 -61.00 -30.00   54
 23  \w    136.00 162.00   0.50    0.32    --  104.75  30.00  30.00   52
 24  \w     39.00  67.00   0.50    0.32    --  104.75 -61.00  60.00   56
 25  \w     35.00  69.00   0.50    0.32    --  104.75 -61.00 -90.00   68
 26  \w     51.00  76.00   0.50    0.17    --   46.68  55.00 -96.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0321864000
_diffrn_orient_matrix_UB_12      -0.1120423000
_diffrn_orient_matrix_UB_13      -0.0367647000
_diffrn_orient_matrix_UB_21      0.0905672000
_diffrn_orient_matrix_UB_22      -0.0223745000
_diffrn_orient_matrix_UB_23      -0.0177132000
_diffrn_orient_matrix_UB_31      0.0121568000
_diffrn_orient_matrix_UB_32      -0.1302445000
_diffrn_orient_matrix_UB_33      0.0346472000
_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  0.0331
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            26555
_diffrn_reflns_point_group_measured_fraction_full 0.905
_diffrn_reflns_point_group_measured_fraction_max 0.860
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.333
_diffrn_reflns_theta_min         3.071
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.566
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83769
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.212
_refine_diff_density_min         -0.185
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details
;
 Flack x determined using 2580 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.24(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         7318
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0541P)^2^+0.2969P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0894
_reflns_Friedel_coverage         0.656
_reflns_Friedel_fraction_full    0.796
_reflns_Friedel_fraction_max     0.730
_reflns_number_gt                6893
_reflns_number_total             7318
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01950h2.cif
_cod_data_source_block           yxw-k2-d_0831_auto
_cod_depositor_comments
'Adding full bibliography for 7134621--7134626.cif.'
_cod_database_code               7134623
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C7(H7), C11(H11), C18(H18), C19(H19), C20(H20), C21(H21),
 C23(H23), C28(H28), C29(H29), C30(H30), C31(H31), C33(H33), C35(H35), C37(H37),
  C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44),
 C45(H45), C47(H47), C48(H48), C50(H50), C52(H52), C54(H54), C56(H56), C13(H13),
  C25(H25), C51(H51), C53(H53)
2.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C55(H55A,H55B,H55C)
;
_shelx_res_checksum              86042
_shelx_hkl_checksum              6089
_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 1.277
_oxdiff_exptl_absorpt_empirical_full_min 0.847