CPL on/off switching by enantiomer encapsulation in TPE heterochiral molecular cages.
Yu, Wei; Hu, Ming; Wen, Xin; Xu, Zhi-Rong; Liu, Minghua; Zheng, Yan-Song; Chemical science 16 (2025) 20924–20930; doi:10.1039/d5sc05405b

data_1575911
_publ_section_title
;
 CPL on/off switching by enantiomer encapsulation in TPE heterochiral
 molecular cages.
;
_journal_issue                   44
_journal_name_full               'Chemical science'
_journal_page_first              20924
_journal_page_last               20930
_journal_paper_doi               10.1039/d5sc05405b
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety
'0.376(F6 P), 0.047(C156 H160 N8), 0.376(C2 H3 N)'
_chemical_formula_sum            'C11 H10 F6 N O P'
_chemical_formula_weight         317.17
_space_group_crystal_system      orthorhombic
_space_group_IT_number           68
_space_group_name_Hall           '-C 2a 2ac'
_space_group_name_H-M_alt        'C c c a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-06
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-05-23 deposited with the CCDC.	2025-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            85
_cell_length_a                   43.8342(9)
_cell_length_b                   23.9492(4)
_cell_length_c                   18.8318(2)
_cell_measurement_reflns_used    28562
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      73.8140
_cell_measurement_theta_min      3.1480
_cell_volume                     19769.5(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_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    -45.00 -19.00   0.50    1.00    --    0.00 -77.00 -30.00   52
  2  \w    -22.00  29.00   0.50    1.00    --    0.00 -82.00-150.00  102
  3  \w     -7.00  18.00   0.50    1.00    --    0.00 -82.00 -60.00   50
  4  \w     -6.00  30.00   0.50    1.00    --    0.00 -82.00   0.00   72
  5  \w    -33.00   7.00   0.50    1.00    --    0.00 -82.00-180.00   80
  6  \w     19.00  69.00   0.50    4.00    --   95.20 -82.00-120.00  100
  7  \w      7.00  77.00   0.50    4.00    --   95.20 -30.00   0.00  140
  8  \w      7.00  51.00   0.50    4.00    --   95.20 -45.00   0.00   88
  9  \w     13.00 125.00   0.50    4.00    --   95.20 -82.00 -30.00  224
 10  \w     65.00  91.00   0.50    4.00    --   95.20 -45.00   0.00   52
 11  \w     49.00  87.00   0.50    4.00    --   95.20 -61.00 -60.00   76
 12  \w     35.00  73.00   0.50    4.00    --   95.20 -77.00 -60.00   76
 13  \w      6.00 127.00   0.50    4.00    --   95.20 -82.00 -90.00  242
 14  \w     81.00 180.00   0.50    4.00    --   95.20  15.00 150.00  198
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0342128000
_diffrn_orient_matrix_UB_12      -0.0143059000
_diffrn_orient_matrix_UB_13      -0.0039236000
_diffrn_orient_matrix_UB_21      -0.0073379000
_diffrn_orient_matrix_UB_22      -0.0615457000
_diffrn_orient_matrix_UB_23      0.0165599000
_diffrn_orient_matrix_UB_31      -0.0032345000
_diffrn_orient_matrix_UB_32      -0.0120442000
_diffrn_orient_matrix_UB_33      -0.0800114000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            56697
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.309
_diffrn_reflns_theta_min         3.151
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.586
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.264
_exptl_crystal_F_000             13600
_refine_diff_density_max         2.189
_refine_diff_density_min         -0.916
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         9936
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.941
_refine_ls_R_factor_all          0.1370
_refine_ls_R_factor_gt           0.1272
_refine_ls_shift/su_max          4.804
_refine_ls_shift/su_mean         0.097
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4142
_refine_ls_wR_factor_ref         0.4252
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8351
_reflns_number_total             9936
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc05405b2.cif
_cod_data_source_block           20231206_2
_cod_depositor_comments
'Adding full bibliography for 1575910--1575911.cif.'
_cod_original_sg_symbol_Hall     '-C 2b 2bc'
_cod_original_sg_symbol_H-M      'C c c e'
_cod_database_code               1575911
_shelx_shelxl_version_number     2018/3
_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.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C30(H30), C40(H40), C11(H11), C23(H23), C27(H27), C7(H7), C15(H15), C31(H31),
 C2(H2), C33(H33), C17(H17), C35(H35)
2.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C36(H36A,H36B,H36C), C43(H43A,H43B,H43C), C25(H25A,H25B,
 H25C), C13(H13A,H13B,H13C), C29(H29A,H29B,H29C), C19(H19A,H19B,H19C), C39(H39A,
 H39B,H39C), C5(H5A,H5B,H5C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              307
_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 1.886
_oxdiff_exptl_absorpt_empirical_full_min 0.600