Efficient circularly polarized multiple resonance thermally activated delayed fluorescence from B,N-embedded hetero[8]helicene enantiomers.
Huang, Tingting; Yuan, Li; Lu, Xueying; Qu, Yupei; Qu, Cheng; Xu, Yincai; Zheng, You-Xuan; Wang, Yue; Chemical science 15 (2024) 15170–15177; doi:10.1039/d4sc03854a

data_1572409
_publ_section_title
;
 Efficient circularly polarized multiple resonance thermally activated
 delayed fluorescence from B,N-embedded hetero[8]helicene enantiomers.
;
_journal_issue                   37
_journal_name_full               'Chemical science'
_journal_page_first              15170
_journal_page_last               15177
_journal_paper_doi               10.1039/d4sc03854a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C70 H60 B N3'
_chemical_formula_sum            'C70 H60 B N3'
_chemical_formula_weight         954.02
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-03-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-06-07 deposited with the CCDC.	2024-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                104.893(2)
_cell_angle_beta                 90.229(2)
_cell_angle_gamma                96.128(2)
_cell_formula_units_Z            2
_cell_length_a                   11.1226(7)
_cell_length_b                   15.8329(9)
_cell_length_c                   15.9866(9)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    295.0
_cell_measurement_theta_max      27.189
_cell_measurement_theta_min      2.631
_cell_volume                     2703.7(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      295.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0709
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            113254
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.53
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  0.9933
_exptl_absorpt_correction_T_min  0.9913
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.600
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         12428
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1271
_refine_ls_R_factor_gt           0.0762
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1070P)^2^+1.4090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1967
_refine_ls_wR_factor_ref         0.2410
_reflns_number_gt                7397
_reflns_number_total             12428
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d4sc03854a2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 1572409.cif.'
_cod_database_code               1572409
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C60-C55 \\sim C60A-C55 \\sim C61-C55 \\sim C61A-C55 \\sim C59-C55 \\sim
C59A-C55
 with sigma of 0.02
 C17-C16 \\sim C17-C22 \\sim C17-C18
 with sigma of 0.02
 C68-C58 \\sim C66A-C58 \\sim C69-C58 \\sim C67A-C58 \\sim C58-C70 \\sim
C58-C65A
 with sigma of 0.02
 C16-C22 \\sim C22-C18
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C70) = Uanis(C67A) = Uanis(C69) = Uanis(C66A) = Uanis(C68) = Uanis(C65A)
Uanis(C60A) = Uanis(C60) = Uanis(C59A) = Uanis(C59) = Uanis(C61A) = Uanis(C61)
Uanis(C62A) = Uanis(C63) = Uanis(C63A) = Uanis(C64) = Uanis(C64A) = Uanis(C62)
4. Others
 Sof(C59)=Sof(H59D)=Sof(H59E)=Sof(H59F)=Sof(C60)=Sof(H60D)=Sof(H60E)=Sof(H60F)=
 Sof(C61)=Sof(H61D)=Sof(H61E)=Sof(H61F)=1-FVAR(1)
 Sof(C59A)=Sof(H59A)=Sof(H59B)=Sof(H59C)=Sof(C60A)=Sof(H60A)=Sof(H60B)=
 Sof(H60C)=Sof(C61A)=Sof(H61A)=Sof(H61B)=Sof(H61C)=FVAR(1)
 Sof(C62)=Sof(H62D)=Sof(H62E)=Sof(H62F)=Sof(C63)=Sof(H63D)=Sof(H63E)=Sof(H63F)=
 Sof(C64)=Sof(H64D)=Sof(H64E)=Sof(H64F)=1-FVAR(2)
 Sof(C62A)=Sof(H62A)=Sof(H62B)=Sof(H62C)=Sof(C63A)=Sof(H63A)=Sof(H63B)=
 Sof(H63C)=Sof(C64A)=Sof(H64A)=Sof(H64B)=Sof(H64C)=FVAR(2)
 Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=
 Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=1-FVAR(3)
 Sof(C65A)=Sof(H65D)=Sof(H65E)=Sof(H65F)=Sof(C66A)=Sof(H66D)=Sof(H66E)=
 Sof(H66F)=Sof(C67A)=Sof(H67D)=Sof(H67E)=Sof(H67F)=FVAR(3)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C8(H8), C10(H10), C11(H11), C18(H18), C19(H19), C20(H20),
 C21(H21), C24(H24), C25(H25), C26(H26), C27(H27), C31(H31), C34(H34), C35(H35),
  C36(H36), C37(H37), C40(H40), C44(H44), C45(H45), C47(H47), C50(H50), C52(H52)
5.b Idealised Me refined as rotating group:
 C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C59A(H59A,H59B,
 H59C), C60A(H60A,H60B,H60C), C61A(H61A,H61B,H61C), C62A(H62A,H62B,H62C),
 C63A(H63A,H63B,H63C), C64A(H64A,H64B,H64C), C65A(H65D,H65E,H65F), C66A(H66D,
 H66E,H66F), C67A(H67D,H67E,H67F), C59(H59D,H59E,H59F), C60(H60D,H60E,H60F),
 C61(H61D,H61E,H61F), C62(H62D,H62E,H62F), C63(H63D,H63E,H63F), C64(H64D,H64E,
 H64F), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C)
;
_olex2_submission_special_instructions 'No special instructions were received'