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_1554122
_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         'C39 H32 N2 O2 S'
_chemical_formula_sum            'C39 H32 N2 O2 S'
_chemical_formula_weight         592.72
_chemical_name_systematic
'3,6-Bis(diphenylamino)-9,9-dimethyl-9H-thioxanthene 10,10-dioxide'
_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     direct
_audit_creation_date             2017-10-25
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                76.4901(19)
_cell_angle_beta                 75.1590(18)
_cell_angle_gamma                83.1146(19)
_cell_formula_units_Z            4
_cell_length_a                   12.4874(6)
_cell_length_b                   13.7988(7)
_cell_length_c                   18.8029(9)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.05
_cell_measurement_theta_min      2.20
_cell_volume                     3039.0(3)
_computing_cell_refinement       'SAINT v8.38A (Bruker, 2017)'
_computing_data_collection       'APEX3 v.2016.1-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2016/6 multi-CPU (Sheldrick, 2015a)'
_computing_structure_solution    'ShelXS 2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'Bruker PHOTON 100 CMOS'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '3-circle area detector diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            54215
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        28.699
_diffrn_reflns_theta_max         28.699
_diffrn_reflns_theta_min         2.293
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_standards_number         0
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_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9526
_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 0.0560 before and 0.0452 after correction. The Ratio of 
minimum to maximum transmission is 0.9526. The \l/2 correction factor 
is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_recrystallization_method 'from acetone/hexane'
_exptl_crystal_size_max          0.217
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.0025(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick, 2015a)'
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     802
_refine_ls_number_reflns         15690
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0540P)^2^+0.6090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1087
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11430
_reflns_number_total             15690
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            azepines.cif
_cod_data_source_block           m-DDPA-TXO2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               1554122
_ccdc_comments                   'locally archived as 17srv288'
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.969
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Uiso(H14A)=Uiso(H14B)=Uiso(H14C)=FVAR(1)
 Uiso(H15A)=Uiso(H15B)=Uiso(H15C)=FVAR(2)
 Uiso(H15D)=Uiso(H15E)=Uiso(H15F)=FVAR(3)
 Uiso(H14D)=Uiso(H14E)=Uiso(H14F)=FVAR(4)
3.a Aromatic/amide H refined with riding coordinates:
 C2'(H2'), C4'(H4'), C5'(H5'), C9'(H9'), C10'(H10'), C12'(H12'), C17'(H17'),
 C18'(H18'), C19'(H19'), C20'(H20'), C21'(H21'), C23'(H23'), C24'(H24'),
 C25'(H25'), C26'(H26'), C27'(H27'), C29'(H29'), C30'(H30'), C31'(H31'),
 C32'(H32'), C33'(H33'), C35'(H35'), C36'(H36'), C37'(H37'), C38'(H38'),
 C39'(H39'), C2(H2), C4(H4), C5(H5), C9(H9), C10(H10), C12(H12), C17(H17),
 C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26),
  C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C35(H35),
 C36(H36), C37(H37), C38(H38), C39(H39)
3.b Idealised Me refined as rotating group:
 C14'(H14A,H14B,H14C), C15'(H15A,H15B,H15C), C14(H14D,H14E,H14F), C15(H15D,
 H15E,H15F)
;
_shelx_res_checksum              71110
_shelx_hkl_checksum              19201
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'