Single-crystal chiral two-dimensional supramolecular organic frameworks for tunable circularly polarized luminescence
Cui, Jialin; Wang, Hui; Liu, Hui; Yu, Hailong; Wang, Wei; Wang, Yu; Zhao, Yingjie; Chemical Science 16 (2025) 7513–7522; doi:10.1039/D4SC08811E

data_1574191
_publ_section_title
;
 Single-crystal chiral two-dimensional supramolecular organic frameworks
 for tunable circularly polarized luminescence
;
_journal_issue                   17
_journal_name_full               'Chemical Science'
_journal_page_first              7513
_journal_page_last               7522
_journal_paper_doi               10.1039/D4SC08811E
_journal_volume                  16
_journal_year                    2025
_chemical_absolute_configuration syn
_chemical_formula_moiety         '2(C60 H42 N6 O12), 3(C20 H12)'
_chemical_formula_sum            'C180 H120 N12 O24'
_chemical_formula_weight         2834.87
_space_group_crystal_system      trigonal
_space_group_IT_number           155
_space_group_name_Hall           'R 3 2"'
_space_group_name_H-M_alt        'R 3 2 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-09-21
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-10-15 deposited with the CCDC.	2025-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   24.0472(4)
_cell_length_b                   24.0472(4)
_cell_length_c                   25.9660(5)
_cell_measurement_reflns_used    8493
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      75.4830
_cell_measurement_theta_min      2.7110
_cell_volume                     13003.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 42.84a 64-bit (release 16-02-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (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      99.99(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 0.996
_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     43.00 104.00   0.50    1.81    --  107.17 -94.00 120.00  122
  2  \w     62.00 108.00   0.50    1.81    --  107.17-115.00  84.00   92
  3  \w     35.00 103.00   0.50    1.81    --  107.17 -94.00   0.00  136
  4  \w     53.00  93.00   0.50    1.81    --  107.17 -94.00 -30.00   80
  5  \w     49.00 103.00   0.50    1.81    --  107.17 -94.00-180.00  108
  6  \w    -31.00  18.00   0.50    0.45    --   41.52 -19.00 -90.00   98
  7  \w     43.00  73.00   0.50    1.81    --  107.17 -61.00  30.00   60
  8  \w     40.00  69.00   0.50    1.81    --  107.17 -61.00 120.00   58
  9  \w     33.00  66.00   0.50    1.81    --  107.17 -61.00 150.00   66
 10  \w     54.00 114.00   0.50    0.45    --   41.52 168.00 -40.00  120
 11  \w     83.00 164.00   0.50    1.81    --  107.17  70.00 -66.00  162
 12  \w     36.00  70.00   0.50    1.81    --  107.17 -61.00-180.00   68
 13  \w     61.00  90.00   0.50    0.45    --   41.52-125.00-180.00   58
 14  \w     25.00  53.00   0.50    0.45    --   41.52-125.00-180.00   56
 15  \w     12.00  87.00   0.50    0.45    --   41.52-115.00  84.00  150
 16  \w    -25.00  29.00   0.50    0.45    --  -41.52  37.00-150.00  108
 17  \w    -16.00  23.00   0.50    0.45    --  -41.52  19.00-180.00   78
 18  \w    -85.00 -28.00   0.50    1.81    -- -102.00  70.00 -66.00  114
 19  \w    -68.00 -30.00   0.50    1.81    -- -102.00  61.00 120.00   76
 20  \w    -69.00 -37.00   0.50    1.81    -- -102.00  61.00  60.00   64
 21  \w    -69.00 -30.00   0.50    1.81    -- -102.00 125.00 -30.00   78
 22  \w    -67.00 -28.00   0.50    1.81    -- -102.00 140.00-111.00   78
 23  \w   -121.00 -88.00   0.50    1.81    -- -102.00 140.00-111.00   66
 24  \w   -114.00 -72.00   0.50    1.81    -- -102.00 129.00  75.00   84
 25  \w    -66.00 -35.00   0.50    1.81    -- -102.00 129.00  75.00   62
 26  \w   -171.00 -85.00   0.50    1.81    -- -102.00 -30.00-180.00  172
;
_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      -0.0239112000
_diffrn_orient_matrix_UB_12      0.0332546000
_diffrn_orient_matrix_UB_13      0.0374674000
_diffrn_orient_matrix_UB_21      -0.0332693000
_diffrn_orient_matrix_UB_22      0.0136435000
_diffrn_orient_matrix_UB_23      -0.0449691000
_diffrn_orient_matrix_UB_31      -0.0615497000
_diffrn_orient_matrix_UB_32      -0.0646347000
_diffrn_orient_matrix_UB_33      0.0097428000
_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  0.1261
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            27636
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        65.078
_diffrn_reflns_theta_max         65.078
_diffrn_reflns_theta_min         2.720
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.591
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.086
_exptl_crystal_description       block
_exptl_crystal_F_000             4428
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details
;
 Flack x determined using 1575 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   1.9(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4937
_refine_ls_number_restraints     572
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1251
_refine_ls_R_factor_gt           0.1157
_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^)+(0.1962P)^2^+63.6865P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2923
_refine_ls_wR_factor_ref         0.3040
_reflns_Friedel_coverage         0.855
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                4241
_reflns_number_total             4937
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc08811e2.cif
_cod_data_source_block           bei-s-2
_cod_depositor_comments
'Adding full bibliography for 1574186--1574191.cif.'
_cod_original_cell_volume        13003.6(5)
_cod_original_sg_symbol_H-M      'R 3 2'
_cod_database_code               1574191
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C21-C30 = C27-C28 = C28-C29 = C30-C29 = C27-C26
 1.39 with sigma of 0.01
 C15-C20 \\sim C19-C20 \\sim C17-C18 \\sim C18-C19 \\sim C17-C16 \\sim C15-C16
 with sigma of 0.008
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within -2.5A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within -2.5A
4.a Ternary CH refined with riding coordinates:
 C20(H20), C15(H15)
4.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C18(H18A,H18B), C16(H16A,H16B), C17(H17A,H17B)
4.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C1(H1), C2(H2), C6(H6), C29(H29), C28(H28), C27(H27), C25(H25),
 C24(H24), C23(H23)
4.d Fitted hexagon refined as free rotating group:
 N1(C11,C10,C9,C8,C12), N2(C13,C5,C4,C3,C14), C26(C25,C24,C23,C22,C21)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 2.568
_oxdiff_exptl_absorpt_empirical_full_min 0.432