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_1554120
_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_absolute_configuration ad
_chemical_formula_moiety         'C43 H36 N2 O2 S'
_chemical_formula_sum            'C43 H36 N2 O2 S'
_chemical_formula_weight         644.80
_chemical_name_systematic
;
 3,6-Bis(10,11-dihydro-5H-dibenzo[b,f]azepin-5-yl)-9,9-dimethyl-9H-thioxanthene 
 10,10-dioxide 
;
_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             2018-10-09
_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            4
_cell_length_a                   12.9552(4)
_cell_length_b                   12.9939(4)
_cell_length_c                   20.0294(7)
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.74
_cell_measurement_theta_min      2.22
_cell_volume                     3371.72(19)
_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 2018/3 multi-CPU (Sheldrick, 2015a)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_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 0.998
_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  0.0448
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            51913
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         2.220
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.137
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9297
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
  wR2(int) was 0.0624 before and 0.0506 after correction. 
  The Ratio of minimum to maximum transmission is 0.9297. 
  The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_recrystallization_method 'from acetone/DCM/hexane'
_exptl_crystal_size_max          0.152
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.131
_refine_diff_density_max         0.204
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details
;
 Flack x determined using 2511 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
 Flack x = -0.044(62) by classical fit to all intensities. 
 Hooft parameter y = -0.03(2).
;
_refine_ls_abs_structure_Flack   -0.026(19)
_refine_ls_extinction_coef       0.0043(6)
_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   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         6624
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0296
_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^)+(0.0417P)^2^+0.3265P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0712
_reflns_Friedel_coverage         0.789
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                6056
_reflns_number_total             6624
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            azepines.cif
_cod_data_source_block           m-DAz-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               1554120
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.980
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C22B-C21 \\sim C22A-C21
 with sigma of 0.02
 C23B-C22B \\sim C22A-C23A
 with sigma of 0.02
 C23B-C24 \\sim C23A-C24
 with sigma of 0.02
3. Others
 Uiso(H14A)=Uiso(H14B)=Uiso(H14C)=FVAR(1)
 Uiso(H15A)=Uiso(H15B)=Uiso(H15C)=FVAR(2)
 Fixed Sof: C22A(0.92) H22A(0.92) H22B(0.92) C23A(0.92) H23A(0.92) H23B(0.92)
 C22B(0.08) H22C(0.08) H22D(0.08) C23B(0.08) H23C(0.08) H23D(0.08)
4.a Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C37(H37A,H37B), C22A(H22A,H22B), C23A(H23A,H23B), C22B(H22C,
 H22D), C23B(H23C,H23D)
4.b 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), C25(H25), C26(H26), C27(H27), C28(H28), C31(H31), C32(H32),
  C33(H33), C34(H34), C39(H39), C40(H40), C41(H41), C42(H42)
4.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              35532
_shelx_hkl_checksum              90620
_ccdc_comments                   'full data archived locally as 17srv277'
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'