Enhanced chiroptical activity for narrow deep-blue emission in axial chiral frameworks <i>via</i> three-dimensional interlocking.
Mo, Xuechao; Chen, Guohao; Li, Yulan; Xiao, Biao; Chen, Xuefeng; Yin, Xiaojun; Yang, Chuluo; Chemical science 15 (2024) 17663–17670; doi:10.1039/d4sc05056h

data_1573008
_publ_section_title
;
 Enhanced chiroptical activity for narrow deep-blue emission in axial
 chiral frameworks <i>via</i> three-dimensional interlocking.
;
_journal_issue                   42
_journal_name_full               'Chemical science'
_journal_page_first              17663
_journal_page_last               17670
_journal_paper_doi               10.1039/d4sc05056h
_journal_volume                  15
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         '2(C54 H34 N2), C H2 Cl2'
_chemical_formula_sum            'C109 H70 Cl2 N4'
_chemical_formula_weight         1506.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-10
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-07-23 deposited with the CCDC.	2024-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 123.416(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   25.6752(14)
_cell_length_b                   7.7929(4)
_cell_length_c                   22.2195(18)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      57.026
_cell_measurement_theta_min      2.997
_cell_volume                     3710.9(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      170.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0926
_diffrn_reflns_av_unetI/netI     0.0643
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            41935
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         57.331
_diffrn_reflns_theta_min         2.996
_diffrn_source_current           3.57
_diffrn_source_power             0.24954300000000001
_diffrn_source_voltage           69.9
_exptl_absorpt_coefficient_mu    0.810
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.6523
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1808 before and 0.1137 after correction.
The Ratio of minimum to maximum transmission is 0.8683.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_description       needle
_exptl_crystal_F_000             1572
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.198
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.05(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         7631
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0571P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1066
_reflns_Friedel_coverage         0.852
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                6083
_reflns_number_total             7631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05056h2.cif
_cod_data_source_block           230607_rr_bcz_bn_0602
_cod_database_code               1573008
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.868
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.95(4)
 0.05(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
3. Restrained distances
 C55-Cl1A
 1.75 with sigma of 0.02
 C55-Cl1
 1.75 with sigma of 0.02
 Cl1-C55 \\sim Cl1A-C55
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C55 \\sim Cl1 \\sim Cl1A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
5. Others
 Sof(Cl1A)=1-FVAR(1)
 Sof(H55C)=Sof(H55D)=0.5*(1-FVAR(2))
 Sof(H55A)=Sof(H55B)=0.5*FVAR(2)
 Sof(Cl1)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C38(H38A,H38B), C55(H55A,H55B), C55(H55C,H55D)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C13(H13), C14(H14), C15(H15),
 C16(H16), C19(H19), C20(H20), C24(H24), C25(H25), C26(H26), C27(H27), C30(H30),
  C31(H31), C34(H34), C35(H35), C36(H36), C37(H37), C40(H40), C41(H41),
 C42(H42), C43(H43), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54)
;
_shelx_res_checksum              47613
_shelx_hkl_checksum              77866
_olex2_submission_special_instructions 'No special instructions were received'