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_7134624
_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, C7 H8'
_chemical_formula_sum            'C55 H38 N4'
_chemical_formula_weight         754.89
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-01-14
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_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                   30.1235(7)
_cell_length_b                   14.8515(4)
_cell_length_c                   8.8086(2)
_cell_measurement_reflns_used    4272
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.7840
_cell_measurement_theta_min      2.9340
_cell_volume                     3940.78(17)
_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 0.992
_diffrn_measured_fraction_theta_max 0.972
_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    -15.00  16.00   0.50    0.05    --   44.63 -19.00  60.00   62
  2  \w    -24.00   9.00   0.50    0.05    --   44.63 -36.00  28.00   66
  3  \w     12.00  38.00   0.50    0.05    --   44.63 -36.00  28.00   52
  4  \w    -31.00  19.00   0.50    0.05    --   44.63 -19.00 -30.00  100
  5  \w    -33.00  22.00   0.50    0.05    --   44.63 -19.00 -90.00  110
  6  \w     42.00  67.00   0.50    0.05    --  108.93 -61.00 -60.00   50
  7  \w     40.00  67.00   0.50    0.05    --  108.93 -61.00-150.00   54
  8  \w     45.00 108.00   0.50    0.05    --  108.93-125.00-180.00  126
  9  \w     41.00  67.00   0.50    0.05    --  108.93 -61.00  30.00   52
 10  \w     36.00  68.00   0.50    0.05    --  108.93-135.00 163.00   64
 11  \w    -53.00 -27.00   0.50    0.05    -- -100.00  45.00-150.00   52
 12  \w    -54.00 -28.00   0.50    0.05    -- -100.00  45.00   0.00   52
 13  \w   -123.00 -97.00   0.50    0.05    -- -100.00 -36.00  28.00   52
 14  \w   -170.00-127.00   0.50    0.05    -- -100.00-135.00 163.00   86
 15  \w   -122.00 -84.00   0.50    0.05    -- -100.00-135.00 163.00   76
 16  \w   -168.00-103.00   0.50    0.05    -- -100.00 -85.00-134.00  130
 17  \w   -147.00-121.00   0.50    0.05    -- -100.00 -36.00  28.00   52
 18  \w    -31.00   5.00   0.50    0.05    --   44.63 -19.00   0.00   72
 19  \w     -9.00  18.00   0.50    0.05    --   44.63 -19.00-150.00   54
 20  \w    -27.00   1.00   0.50    0.05    --   44.63 -19.00-180.00   56
 21  \w    -54.00 -29.00   0.50    0.05    -- -100.00  45.00 150.00   50
 22  \w   -173.00-129.00   0.50    0.05    -- -100.00 -45.00 150.00   88
 23  \w   -155.00-124.00   0.50    0.05    -- -100.00-125.00 150.00   62
 24  \w   -112.00 -86.00   0.50    0.05    -- -100.00-125.00 150.00   52
 25  \w    -59.00 -29.00   0.50    0.05    -- -100.00  61.00  90.00   60
 26  \w   -104.00 -79.00   0.50    0.05    -- -100.00 -45.00 150.00   50
 27  \w     59.00  88.00   0.50    0.05    --  108.93 -77.00-150.00   58
 28  \w     35.00  68.00   0.50    0.05    --  108.93 -61.00 120.00   66
 29  \w     46.00  72.00   0.50    0.05    --  108.93 -77.00 -60.00   52
 30  \w     35.00  68.00   0.50    0.05    --  108.93 -61.00-180.00   66
 31  \w     41.00  99.00   0.50    0.05    --  108.93 -94.00  30.00  116
 32  \w    -89.00 -64.00   0.50    0.05    --  -44.63 135.00-131.00   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      0.0123013000
_diffrn_orient_matrix_UB_12      0.0997362000
_diffrn_orient_matrix_UB_13      0.0235425000
_diffrn_orient_matrix_UB_21      -0.0435966000
_diffrn_orient_matrix_UB_22      0.0285006000
_diffrn_orient_matrix_UB_23      -0.0779218000
_diffrn_orient_matrix_UB_31      -0.0238004000
_diffrn_orient_matrix_UB_32      -0.0007819000
_diffrn_orient_matrix_UB_33      0.1546800000
_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  0.0628
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            13292
_diffrn_reflns_point_group_measured_fraction_full 0.738
_diffrn_reflns_point_group_measured_fraction_max 0.709
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.312
_diffrn_reflns_theta_min         5.959
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89116
_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    1.272
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack x determined using 557 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         2981
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0601
_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^)+(0.1101P)^2^+0.2140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1536
_refine_ls_wR_factor_ref         0.1685
_reflns_Friedel_coverage         0.365
_reflns_Friedel_fraction_full    0.443
_reflns_Friedel_fraction_max     0.407
_reflns_number_gt                2403
_reflns_number_total             2981
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01950h2.cif
_cod_data_source_block           yxw-kz-tol_0113_auto
_cod_depositor_comments
'Adding full bibliography for 7134621--7134626.cif.'
_cod_database_code               7134624
_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. Restrained distances
 C3-C25
 1.395 with sigma of 0.005
 C25-C13
 1.395 with sigma of 0.005
 C13-C27
 1.395 with sigma of 0.005
3. Rigid bond restraints
 C10, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
5. Others
 Fixed Sof: H7A(0.5) H7B(0.5) H7C(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C17(H17), C18(H18),
 C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C26(H26), C28(H28), C3(H3),
 C13(H13), C25(H25)
6.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_shelx_res_checksum              81957
_shelx_hkl_checksum              97978
_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 1.165
_oxdiff_exptl_absorpt_empirical_full_min 0.785