Multi-resonant thermally activated delayed fluorescence emitters based on tetracoordinate boron-containing PAHs: colour tuning based on the nature of chelates
Meng, Guoyun; Liu, Lijie; He, Zhechang; Hall, David; Wang, Xiang; Peng, Tai; Yin, Xiaodong; Chen, Pangkuan; Beljonne, David; Olivier, Yoann; Zysman-Colman, Eli; Wang, Nan; Wang, Suning; Chemical Science  (2022) –; doi:10.1039/D1SC05692A

data_1566071
_publ_section_title
;
 Multi-resonant thermally activated delayed fluorescence emitters based on
 tetracoordinate boron-containing PAHs: colour tuning based on the nature
 of chelates
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC05692A
_journal_year                    2022
_chemical_formula_moiety         'C51 H54 B N3'
_chemical_formula_sum            'C51 H54 B N3'
_chemical_formula_weight         719.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-11-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-12-04 deposited with the CCDC.	2021-12-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 87.00
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.4761(18)
_cell_length_b                   32.994(3)
_cell_length_c                   18.0610(18)
_cell_measurement_reflns_used    7139
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      23.16
_cell_measurement_theta_min      2.27
_cell_volume                     9209.6(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      180.15
_diffrn_measured_fraction_theta_full 0.865
_diffrn_measured_fraction_theta_max 0.869
_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  0.1133
_diffrn_reflns_av_unetI/netI     0.1504
_diffrn_reflns_Laue_measured_fraction_full 0.865
_diffrn_reflns_Laue_measured_fraction_max 0.869
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            42064
_diffrn_reflns_point_group_measured_fraction_full 0.865
_diffrn_reflns_point_group_measured_fraction_max 0.869
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         2.258
_exptl_absorpt_coefficient_mu    0.060
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.038
_exptl_crystal_description       block
_exptl_crystal_F_000             3088
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.169
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         7463
_refine_ls_number_restraints     98
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.1417
_refine_ls_R_factor_gt           0.0697
_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^)+(0.0889P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1644
_refine_ls_wR_factor_ref         0.1838
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3589
_reflns_number_total             7463
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05692a2.cif
_cod_data_source_block           1
_cod_database_code               1566071
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.982
_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
 C37-C2 \\sim C37A-C2
 with sigma of 0.02
 C1-C37 \\sim C37-C36
 with sigma of 0.02
 C36-C2 \\sim C36A-C2
 with sigma of 0.02
3. Rigid bond restraints
 C2, C36, C2, C37
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.0005
 C2, C3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.0005
 C13, C14
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.0005
4. Uiso/Uaniso restraints and constraints
C2 \\sim C36 \\sim C2 \\sim C37: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 3.8A
C2 \\sim C3: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 3.8A
Uanis(C2) \\sim Ueq, Uanis(C37) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C1A) \\sim Ueq, Uanis(C36A) \\sim Ueq, Uanis(C37A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C36A, C1A, C37A, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C36, C1, C37, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
6. Others
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C36A)=Sof(H36D)=Sof(H36E)=
 Sof(H36F)=Sof(C37A)=Sof(H37D)=Sof(H37E)=Sof(H37F)=1-FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=FVAR(1)
7.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C8(H8), C9(H9), C16(H16), C19(H19), C24(H24), C26(H26),
 C27(H27), C28(H28), C31(H31), C33(H33), C38(H38), C44(H44), C45(H45), C46(H46),
  C47(H47), C48(H48)
7.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,
 H14C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C36(H36A,H36B,H36C), C37(H37A,
 H37B,H37C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C),
 C49(H49A,H49B,H49C), C1A(H1AA,H1AB,H1AC), C36A(H36D,H36E,H36F), C37A(H37D,H37E,
 H37F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              63742
_shelx_fab_checksum              10447
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'