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_7133058
_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_absolute_configuration ad
_chemical_formula_moiety         'C55 H42 Cd2 N6 O10'
_chemical_formula_sum            'C55 H42 Cd2 N6 O10'
_chemical_formula_weight         1171.74
_chemical_name_systematic        DCF-15
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-04-14
_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                   9.6554(2)
_cell_length_b                   17.7129(4)
_cell_length_c                   36.6589(6)
_cell_measurement_reflns_used    7549
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.6110
_cell_measurement_theta_min      3.4860
_cell_volume                     6269.6(2)
_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)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1169
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.859
_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    -51.00 -21.00   0.30    2.65    --   17.09   0.00-150.00  100
  2  \w     31.00  71.20   0.30    2.65    --   17.09   0.00-150.00  134
  3  \w      1.00  85.00   0.30    2.65    --   17.09  38.00-120.00  280
;
_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      0.0247844000
_diffrn_orient_matrix_UB_12      -0.0141527000
_diffrn_orient_matrix_UB_13      -0.0169204000
_diffrn_orient_matrix_UB_21      -0.0103954000
_diffrn_orient_matrix_UB_22      -0.0374392000
_diffrn_orient_matrix_UB_23      0.0062977000
_diffrn_orient_matrix_UB_31      -0.0683666000
_diffrn_orient_matrix_UB_32      0.0005704000
_diffrn_orient_matrix_UB_33      -0.0070759000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0781
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.859
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            22080
_diffrn_reflns_point_group_measured_fraction_full 0.905
_diffrn_reflns_point_group_measured_fraction_max 0.744
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.464
_diffrn_reflns_theta_min         3.334
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.731
_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 white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_description       block
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.393
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.139
_refine_ls_abs_structure_details
;
 Flack x determined using 2740 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         12971
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0728
_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^)+(0.1391P)^2^+0.3555P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2034
_refine_ls_wR_factor_ref         0.2291
_reflns_Friedel_coverage         0.576
_reflns_Friedel_fraction_full    0.792
_reflns_Friedel_fraction_max     0.604
_reflns_number_gt                10114
_reflns_number_total             12971
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00925h2.cif
_cod_data_source_block           DCF-15_auto_sq
_cod_depositor_comments
'Adding full bibliography for 7133057--7133060.cif.'
_cod_database_code               7133058
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.930
_shelx_estimated_absorpt_t_min   0.810
_reflns_odcompleteness_completeness 99.38
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C54) \\sim Ueq, Uanis(C50) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.001
Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Secondary CH2 refined with riding coordinates:
 C50(H50A,H50B), C51(H51A,H51B)
3.b Aromatic/amide H refined with riding coordinates:
 C44(H44), C38(H38), C45(H45), C43(H43), C40(H40), C37(H37), C26(H26),
 C30(H30), C29(H29), C46(H46), C7(H7), C41(H41), C18(H18), C27(H27), C10(H10),
 C8(H8), C17(H17), C11(H11), C22(H22), C15(H15), C32(H32), C4(H4), C33(H33),
 C1(H1), C20(H20), C23(H23), C34(H34), C14(H14), C35(H35), C5(H5), C2(H2),
 C21(H21)
3.c Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C), C49(H49A,H49B,H49C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              69266
_shelx_fab_checksum              10554
_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 1.582
_oxdiff_exptl_absorpt_empirical_full_min 0.780