Chiral emissive porous organic cages.
Sun, Yu-Ling; Wang, Zhen; Ma, Hui; Zhang, Qing-Pu; Yang, Bin-Bin; Meng, Xianggao; Zhang, Yaohua; Zhang, Chun; Chemical communications (Cambridge, England) 59 (2023) 302–305; doi:10.1039/d2cc05283k

data_7131074
_publ_section_title
;
 Chiral emissive porous organic cages.
;
_journal_issue                   3
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              302
_journal_page_last               305
_journal_paper_doi               10.1039/d2cc05283k
_journal_volume                  59
_journal_year                    2023
_chemical_absolute_configuration syn
_chemical_formula_moiety         '0.5(C2 H4 Cl4), 0.667(C126 H120 N12)'
_chemical_formula_sum            'C85 H82 Cl2 N8'
_chemical_formula_weight         1286.48
_space_group_crystal_system      cubic
_space_group_IT_number           195
_space_group_name_Hall           'P 2 2 3'
_space_group_name_H-M_alt        'P 2 3'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-04-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-04-13 deposited with the CCDC.	2022-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   24.8853(2)
_cell_length_b                   24.8853(2)
_cell_length_c                   24.8853(2)
_cell_measurement_reflns_used    14235
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      57.0650
_cell_measurement_theta_min      3.0940
_cell_volume                     15410.9(2)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      99.99(10)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            83118
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.226
_diffrn_reflns_theta_min         2.511
_exptl_absorpt_coefficient_mu    0.839
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70436
_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_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.832
_exptl_crystal_description       block
_exptl_crystal_F_000             4092
_exptl_crystal_size_max          0.512
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 2888 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.142(12)
_refine_ls_extinction_coef       0.00016(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         10373
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0617
_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^)+(0.1409P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1790
_refine_ls_wR_factor_ref         0.1997
_reflns_Friedel_coverage         0.858
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.982
_reflns_number_gt                7649
_reflns_number_total             10373
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05283k2.cif
_cod_data_source_block           tpe_r
_cod_depositor_comments
'Adding full bibliography for 7131074--7131075.cif.'
_cod_original_cell_volume        15410.9(4)
_cod_database_code               7131074
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.673
_olex2_refinement_description
;
1. Restrained distances
 Cl1-C45 = Cl2-C45
 1.8 with sigma of 0.02
 Cl1-Cl2
 3 with sigma of 0.04
 Cl1-C45 \\sim Cl2-C45
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl2 \\sim C45: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 1.7A
Uanis(C45) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: Cl1(0.5) C45(0.5) H45A(0.5) H45B(0.5)
4.a Ternary CH refined with riding coordinates:
 C31(H31), C35(H35), C42(H42), C43(H43)
4.b Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C36(H36A,
 H36B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C44(H44A,H44B)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13), C14(H14),
 C16(H16), C17(H17), C19(H19), C20(H20), C22(H22), C23(H23), C25(H25), C26(H26),
  C27(H27), C28(H28), C30(H30), C41(H41)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              22249
_shelx_hkl_checksum              87641
_shelx_fab_checksum              23097
_olex2_submission_special_instructions 'No special instructions were received'