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_1573009
_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_formula_moiety         'C74 H46 N4, C H2 Cl2'
_chemical_formula_sum            'C75 H48 Cl2 N4'
_chemical_formula_weight         1076.07
_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             2024-01-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-07-23 deposited with the CCDC.	2024-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.082(2)
_cell_length_b                   16.518(2)
_cell_length_c                   26.742(4)
_cell_measurement_reflns_used    3776
_cell_measurement_temperature    294.3
_cell_measurement_theta_max      30.63
_cell_measurement_theta_min      2.58
_cell_volume                     6220.4(15)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      294.3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2081
_diffrn_reflns_av_unetI/netI     0.1680
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            72869
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.436
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.150
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6457
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0893 before and 0.0758 after correction.
The Ratio of minimum to maximum transmission is 0.8653.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_description       block
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.202
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 1091 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     730
_refine_ls_number_reflns         10932
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.936
_refine_ls_R_factor_all          0.2236
_refine_ls_R_factor_gt           0.0809
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1059P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1751
_refine_ls_wR_factor_ref         0.2455
_reflns_Friedel_coverage         0.814
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4067
_reflns_number_total             10932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05056h2.cif
_cod_data_source_block           1
_cod_database_code               1573009
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.987
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
C08Y \\sim Cl \\sim Cl1: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
3.a Secondary CH2 refined with riding coordinates:
 C021(H02A,H02B), C029(H02C,H02D), C02U(H02E,H02F), C05D(H05A,H05B), C08Y(H08A,
 H08B)
3.b Aromatic/amide H refined with riding coordinates:
 C00P(H00P), C01F(H01F), C020(H020), C03I(H03I), C03K(H03K), C03U(H03U),
 C04B(H04B), C04S(H04S), C04W(H04W), C050(H050), C05C(H05C), C05J(H05J),
 C05S(H05S), C05V(H05V), C066(H066), C068(H068), C069(H069), C06D(H06D),
 C06F(H06F), C06K(H06K), C06S(H06S), C06U(H06U), C06W(H06W), C076(H076),
 C07B(H07B), C07C(H07C), C07E(H07E), C07G(H07G), C07J(H07J), C07M(H07M),
 C07R(H07R), C081(H081), C08C(H08C), C08E(H08E), C08H(H08H), C08I(H08I),
 C08J(H08J), C08R(H08R)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 150 electrons were 
found in a volume of 1340\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[CH2Cl2] per Asymmetric Unit 
which account for 168 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              29294
_shelx_hkl_checksum              26721
_shelx_fab_checksum              60926
_olex2_submission_special_instructions 'No special instructions were received'