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_7134621
_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, 2[CH2Cl2]'
_chemical_formula_sum            'C50 H34 Cl4 N4'
_chemical_formula_weight         832.61
_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
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.9340(8)
_cell_length_b                   15.0767(5)
_cell_length_c                   8.7946(2)
_cell_measurement_reflns_used    3924
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      74.2130
_cell_measurement_theta_min      2.9640
_cell_volume                     3969.06(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 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 0.995
_diffrn_measured_fraction_theta_max 0.941
_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   -167.00-112.00   0.50    1.48    -- -100.00-124.00  75.00  110
  2  \w    -76.00 -37.00   0.50    1.48    -- -100.00 125.00 120.00   78
  3  \w   -108.00 -82.00   0.50    1.48    -- -100.00 125.00 120.00   52
  4  \w   -111.00 -82.00   0.50    1.48    -- -100.00 125.00  30.00   58
  5  \w    -72.00 -34.00   0.50    1.48    -- -100.00 125.00  30.00   76
  6  \w    -79.00 -47.00   0.50    0.37    --  -44.30 124.00 154.00   64
  7  \w    -30.00  19.00   0.50    0.37    --  -44.30   6.00   5.00   98
  8  \w    -28.00  23.00   0.50    0.37    --   44.30  -6.00-171.00  102
  9  \w    -20.00  22.00   0.50    0.37    --   44.30 -19.00 150.00   84
 10  \w     37.00  63.00   0.50    1.48    --  109.64 -61.00 120.00   52
 11  \w     95.00 172.00   0.50    1.48    --  109.64   6.00   5.00  154
 12  \w     86.00 170.00   0.50    1.48    --  109.64 131.00  60.00  168
;
_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      0.0465881000
_diffrn_orient_matrix_UB_12      0.0434152000
_diffrn_orient_matrix_UB_13      0.0018931000
_diffrn_orient_matrix_UB_21      0.0218203000
_diffrn_orient_matrix_UB_22      -0.0921719000
_diffrn_orient_matrix_UB_23      -0.0139423000
_diffrn_orient_matrix_UB_31      -0.0012446000
_diffrn_orient_matrix_UB_32      0.0077204000
_diffrn_orient_matrix_UB_33      -0.1746250000
_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  0.0809
_diffrn_reflns_av_unetI/netI     0.0663
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6494
_diffrn_reflns_point_group_measured_fraction_full 0.716
_diffrn_reflns_point_group_measured_fraction_max 0.671
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.558
_diffrn_reflns_theta_min         2.952
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.040
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71319
_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    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Flack x determined using 531 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   6.3(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2850
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0829
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1631P)^2^+3.8987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2293
_refine_ls_wR_factor_ref         0.2368
_reflns_Friedel_coverage         0.333
_reflns_Friedel_fraction_full    0.393
_reflns_Friedel_fraction_max     0.361
_reflns_number_gt                2534
_reflns_number_total             2850
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01950h2.cif
_cod_data_source_block           yxw-kazuoji_0416
_cod_depositor_comments
'Adding full bibliography for 7134621--7134626.cif.'
_cod_original_cell_volume        3969.05(19)
_cod_database_code               7134621
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13),
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 310 electrons were 
found in a volume of 924\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[CH2Cl2] per Asymmetric Unit 
which account for 336 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              45107
_shelx_hkl_checksum              8353
_shelx_fab_checksum              70169
_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 2.796
_oxdiff_exptl_absorpt_empirical_full_min 0.264