Hierarchical chiral MOFs with the induced chirality of AIE ligands exhibiting non-reciprocal CPL.
Fu, Hong-Ru; Ren, Dan-Dan; Zhang, Kun; Wang, Shuang; Yang, Xu-Jing; Ding, Qing-Rong; Wu, Ya-Pan; Chemical communications (Cambridge, England) 60 (2024) 6182–6185; doi:10.1039/d4cc00925h

data_7133059
_publ_section_title
;
 Hierarchical chiral MOFs with the induced chirality of AIE ligands
 exhibiting non-reciprocal CPL.
;
_journal_issue                   48
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              6182
_journal_page_last               6185
_journal_paper_doi               10.1039/d4cc00925h
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         '0.04(C180 H156 N16 O52 Zn16)'
_chemical_formula_sum            'C45 H39 N4 O13 Zn4'
_chemical_formula_weight         1105.36
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-03-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-05-24 deposited with the CCDC.	2024-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6565(3)
_cell_length_b                   29.6834(9)
_cell_length_c                   14.1762(4)
_cell_measurement_reflns_used    7916
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.3920
_cell_measurement_theta_min      3.9960
_cell_volume                     5746.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1169
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.863
_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    -30.00  10.00   1.00   45.00    --  -15.61  57.00-180.00   40
  2  \w    -45.00  63.00   1.00   45.00    --   16.78   0.00  90.00  108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0237491000
_diffrn_orient_matrix_UB_12      0.0187030000
_diffrn_orient_matrix_UB_13      0.0209881000
_diffrn_orient_matrix_UB_21      0.0413057000
_diffrn_orient_matrix_UB_22      0.0137006000
_diffrn_orient_matrix_UB_23      -0.0100944000
_diffrn_orient_matrix_UB_31      -0.0205759000
_diffrn_orient_matrix_UB_32      0.0058512000
_diffrn_orient_matrix_UB_33      -0.0442912000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.863
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19296
_diffrn_reflns_point_group_measured_fraction_full 0.941
_diffrn_reflns_point_group_measured_fraction_max 0.774
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.249
_diffrn_reflns_theta_min         3.310
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.704
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
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    1.263
_exptl_crystal_description       block
_exptl_crystal_F_000             2305
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.439
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details
;
 Flack x determined using 3676 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.017(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         12101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0532
_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^)+(0.0982P)^2^+1.9486P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.1565
_reflns_Friedel_coverage         0.639
_reflns_Friedel_fraction_full    0.873
_reflns_Friedel_fraction_max     0.666
_reflns_number_gt                10496
_reflns_number_total             15639
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00925h2.cif
_cod_data_source_block           DCF-16_auto_sq
_cod_depositor_comments
'Adding full bibliography for 7133057--7133060.cif.'
_cod_database_code               7133059
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.970
_reflns_odcompleteness_completeness 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C45(0.5) C43(0.5) C46(0.5) C47(0.5)
3.a Ternary CH refined with riding coordinates:
 C26(H26)
3.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C19(H19A,H19B), C28(H28A,H28B), C39(H39A,H39B), C18(H18A,H18B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1), C11(H11), C5(H5), C15(H15), C12(H12), C4(H4), C14(H14),
 C7(H7), C6(H6), N3(H3), C10(H10), C9(H9)
3.d Fitted hexagon refined as free rotating group:
 C8(C7,C6,N3,C10,C9)
3.e Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C34(H34A,H34B,H34C), C37(H37A,H37B,H37C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              6674
_shelx_fab_checksum              8922
_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 1.177
_oxdiff_exptl_absorpt_empirical_full_min 0.868