Importance of Chromophore Rigidity on the Efficiency of Blue Thermally Activated Delayed Fluorescence Emitters
Kukhta, Nadzeya A.; Batsanov, Andrei S.; Bryce, Martin R.; Monkman, Andrew P.; The Journal of Physical Chemistry C 122 (2018) 28564–; doi:10.1021/acs.jpcc.8b10867

data_1554124
_publ_section_title
;
 Importance of Chromophore Rigidity on the Efficiency of Blue Thermally
 Activated Delayed Fluorescence Emitters
;
_journal_issue                   50
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_page_first              28564
_journal_paper_doi               10.1021/acs.jpcc.8b10867
_journal_volume                  122
_journal_year                    2018
_chemical_formula_moiety         'C43 H36 N2 O2 S, C H2 Cl2'
_chemical_formula_sum            'C44 H38 Cl2 N2 O2 S'
_chemical_formula_weight         729.72
_chemical_name_systematic
;
 3,6-Bis(10,11-dihydro-5H-dibenzo[b,f]azepin-5-yl)-9,9-dimethyl-9H-thioxanthene 
 10,10-dioxide, dichloromethane solvate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-07-02
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.8912(6)
_cell_length_b                   11.3960(4)
_cell_length_c                   37.1194(14)
_cell_measurement_reflns_used    9861
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.53
_cell_measurement_theta_min      2.34
_cell_volume                     7145.2(4)
_computing_cell_refinement       'APEX3 v2017.3-0 (Bruker AXS, 2005-2017)'
_computing_data_collection
'Diamond I19 EH1 GDA (Allan et al., 2017), DIALS (Winter et al., 2018)'
_computing_data_reduction
'cbf_to_sfrm.py (Johnson & Probert, 2016), SAINT V8.38A (Bruker AXS, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015a)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Dectris Pilatus 2M'
_diffrn_detector_area_resol_mean 0.0350
_diffrn_detector_type            'pixel-array photon-counting detector'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device       'I19 EH1'
_diffrn_measurement_device_type  'dual air-bearing fixed-\c diffractometer'
_diffrn_measurement_method       'thin-slice \f and \w scans'
_diffrn_radiation_collimation    '0.3 x 1.5 Double Pinhole'
_diffrn_radiation_monochromator  'double crystal silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.1014
_diffrn_reflns_av_unetI/netI     0.1404
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            49066
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         26.572
_diffrn_reflns_theta_min         1.063
_diffrn_source                   'Beamline I19, Diamond Light Source, RAL'
_diffrn_source_type              undulator
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.261
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS-2016/2 (Krause et al., 2015) was used for absorption correction. 
 wR2(int) was 0.1377 before and 0.1034 after correction. The Ratio of 
 minimum to maximum transmission is 0.5689. The \l/2 correction factor 
 is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       spearhead
_exptl_crystal_F_000             3056
_exptl_crystal_recrystallization_method 'from DCM/ethanol'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.624
_refine_diff_density_min         -1.151
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       0.0019(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick, 2015a)'
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         8004
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0846
_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^)+(0.1284P)^2^+7.2811P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2421
_refine_ls_wR_factor_ref         0.2726
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5620
_reflns_number_total             8004
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            azepines.cif
_cod_data_source_block           p-DAz-TXO2-100K
_cod_database_code               1554124
_ccdc_comments                   'full data archived locally as 17srv286'
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Uiso(H14A)=Uiso(H14B)=Uiso(H14C)=FVAR(1)
 Uiso(H15A)=Uiso(H15B)=Uiso(H15C)=FVAR(2)
3.a Rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
3.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C23(H23A,H23B), C36(H36A,H36B), C37(H37A,H37B), C44(H44A,H44B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C9(H9), C11(H11), C12(H12), C17(H17), C18(H18),
 C19(H19), C20(H20), C25(H25), C26(H26), C27(H27), C28(H28), C31(H31), C32(H32),
  C33(H33), C34(H34), C39(H39), C40(H40), C41(H41), C42(H42)
;
_shelx_res_checksum              54269
_shelx_hkl_checksum              97383