Chiral ring-in-ring complexes with torsion-induced circularly polarized luminescence
Liu, Jia; Han, Xiujie; Wen, Xin; Yu, Hao; Li, Bao; Wang, Ming; Liu, Minghua; Wu, Guanglu; Chemical Science 16 (2025) 7858–7863; doi:10.1039/D5SC00624D

data_1574280
_publ_section_title
;
 Chiral ring-in-ring complexes with torsion-induced circularly polarized
 luminescence
;
_journal_issue                   18
_journal_name_full               'Chemical Science'
_journal_page_first              7858
_journal_page_last               7863
_journal_paper_doi               10.1039/D5SC00624D
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety
'C48 H48 N32 O16, C49 H38 N6 O2, 2(Cl), 28(H2 O)'
_chemical_formula_sum            'C97 H86 Cl2 N38 O46'
_chemical_formula_weight         2590.93
_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     dual
_audit_creation_date             2024-06-21
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-11-22 deposited with the CCDC.	2025-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.666(3)
_cell_length_b                   21.729(4)
_cell_length_c                   34.167(7)
_cell_measurement_reflns_used    26084
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.65
_cell_measurement_theta_min      2.21
_cell_volume                     12373(4)
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            48553
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.683
_diffrn_reflns_theta_min         1.192
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.154
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_description       block
_exptl_crystal_F_000             5344
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.549
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Flack x determined using 9240 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.47(3)
_refine_ls_extinction_coef       0.0058(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1669
_refine_ls_number_reflns         26084
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0820
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.001
_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          0.2512
_refine_ls_wR_factor_ref         0.2593
_reflns_Friedel_coverage         0.854
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                23776
_reflns_number_total             26084
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc00624d2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 1574280.cif.'
_cod_database_code               1574280
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.991
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Others
 Sof(O46)=1-FVAR(1)
 Sof(O45)=FVAR(1)
 Sof(O48)=1-FVAR(2)
 Sof(O47)=FVAR(2)
3.a Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C8(H8), C9(H9), C14(H14), C15(H15), C20(H20), C21(H21),
 C26(H26), C27(H27), C32(H32), C33(H33), C38(H38), C39(H39), C44(H44), C45(H45)
3.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C11(H11A,H11B), C12(H12A,H12B), C17(H17A,H17B),
 C18(H18A,H18B), C23(H23A,H23B), C24(H24A,H24B), C29(H29A,H29B), C30(H30A,H30B),
  C35(H35A,H35B), C36(H36A,H36B), C41(H41A,H41B), C42(H42A,H42B), C47(H47A,
 H47B), C48(H48A,H48B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B)
3.c Aromatic/amide H refined with riding coordinates:
 C49(H49), C50(H50), C52(H52), C53(H53), C54(H54), C55(H55), C60(H60),
 C62(H62), C63(H63), C65(H65), C66(H66), C68(H68), C69(H69), C70(H70), C71(H71),
  C75(H75), C76(H76), C78(H78), C79(H79), C81(H81), C82(H82), C84(H84),
 C85(H85), C86(H86), C91(H91), C92(H92), C93(H93), C94(H94), C96(H96), C97(H97),
  N33(H33A), N38(H38A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              92333
_shelx_fab_checksum              9784
_olex2_submission_special_instructions 'No special instructions were received'