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_7134622
_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           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             2025-04-29
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-04-29 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                   29.6967(6)
_cell_length_b                   15.1954(3)
_cell_length_c                   8.9495(2)
_cell_measurement_reflns_used    4816
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      76.1860
_cell_measurement_theta_min      2.9570
_cell_volume                     4038.49(15)
_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 0.996
_diffrn_measured_fraction_theta_max 0.946
_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    -26.00  44.00   0.50    0.05    --   46.68 -37.00  90.00  140
  2  \w     82.00 111.00   0.50    0.05    --  104.75-125.00-120.00   58
  3  \w     12.00  62.00   0.50    0.05    --   46.68 -57.00-150.00  100
  4  \w     45.00  72.00   0.50    0.05    --  104.75 -61.00 -90.00   54
  5  \w     93.00 121.00   0.50    0.05    --  104.75  30.00-180.00   56
  6  \w     86.00 112.00   0.50    0.05    --   46.68 136.00 104.00   52
  7  \w     85.00 151.00   0.50    0.05    --  104.75 144.00   9.00  132
  8  \w    -25.00   0.00   0.50    0.05    --  -46.68  19.00 150.00   50
  9  \w   -114.00 -70.00   0.50    0.05    -- -102.00 133.00 -73.00   88
 10  \w    -65.00 -31.00   0.50    0.05    -- -102.00 133.00 -73.00   68
 11  \w    -69.00 -31.00   0.50    0.05    -- -102.00  61.00-120.00   76
 12  \w   -157.00 -77.00   0.50    0.05    -- -102.00  -5.00 -96.00  160
;
_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      -0.0160257000
_diffrn_orient_matrix_UB_12      0.0961912000
_diffrn_orient_matrix_UB_13      -0.0111953000
_diffrn_orient_matrix_UB_21      -0.0493316000
_diffrn_orient_matrix_UB_22      -0.0313577000
_diffrn_orient_matrix_UB_23      0.0018988000
_diffrn_orient_matrix_UB_31      -0.0004255000
_diffrn_orient_matrix_UB_32      0.0065903000
_diffrn_orient_matrix_UB_33      0.1717736000
_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  0.0315
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            7121
_diffrn_reflns_point_group_measured_fraction_full 0.735
_diffrn_reflns_point_group_measured_fraction_max 0.687
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.328
_diffrn_reflns_theta_min         3.267
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94856
_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    1.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.130
_refine_diff_density_min         -0.122
_refine_diff_density_rms         0.030
_refine_ls_abs_structure_details
;
 Flack x determined using 661 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.6(6)
_refine_ls_extinction_coef       0.00079(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         2963
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0383
_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^)+(0.0417P)^2^+0.7300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0885
_reflns_Friedel_coverage         0.360
_reflns_Friedel_fraction_full    0.434
_reflns_Friedel_fraction_max     0.390
_reflns_number_gt                2707
_reflns_number_total             2963
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc01950h2.cif
_cod_data_source_block           yxw-k2-p_0831_auto
_cod_depositor_comments
'Adding full bibliography for 7134621--7134626.cif.'
_cod_database_code               7134622
_shelx_shelxl_version_number     2019/3
_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
 C31-C13 = C31-C30 = C30-C27 = C3-C27 = C3-C25 = C25-C13
 1.395 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C13 \\sim C3 \\sim C25 \\sim C27 \\sim C29 \\sim C30 \\sim C7 \\sim C31: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Others
 Fixed Sof: C3(0.5) H3(0.5) C7(0.5) H7A(0.5) H7B(0.5) H7C(0.5) C13(0.5)
 C25(0.5) H25(0.5) C27(0.5) C29(0.5) H29A(0.5) H29B(0.5) H29C(0.5) C30(0.5)
 H30(0.5) C31(0.5) H31(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C14(H14), C15(H15),
 C16(H16), C17(H17), C19(H19), C21(H21), C23(H23), C26(H26), C28(H28), C3(H3),
 C25(H25), C30(H30), C31(H31)
5.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              55753
_shelx_hkl_checksum              52986
_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 1.405
_oxdiff_exptl_absorpt_empirical_full_min 0.739