Coordination-Induced Thermally Activated Delayed Fluorescence: From Non-TADF Donor–Acceptor-Type Ligand to TADF-Active Ag-Based Complexes
Jia, Ji-Hui; Liang, Dong; Yu, Rongmin; Chen, Xu-Lin; Meng, Lingyi; Chang, Jian-Fei; Liao, Jian-Zhen; Yang, Mingxue; Li, Xiao-Ning; Lu, Can-Zhong; Chemistry of Materials  (2019) –; doi:10.1021/acs.chemmater.9b04585

data_4003450
_publ_section_title
;
 Coordination-Induced Thermally Activated Delayed Fluorescence: From
 Non-TADF Donor--Acceptor-Type Ligand to TADF-Active Ag-Based Complexes
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.9b04585
_journal_year                    2019
_chemical_formula_moiety         'C30 H26 N4'
_chemical_formula_sum            'C30 H26 N4'
_chemical_formula_weight         442.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-07-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.657(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0497(8)
_cell_length_b                   19.8573(11)
_cell_length_c                   8.9019(5)
_cell_measurement_reflns_used    4313
_cell_measurement_temperature    100.00(14)
_cell_measurement_theta_max      30.0320
_cell_measurement_theta_min      3.9650
_cell_volume                     2274.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3468
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -36.00  47.00   1.00   17.07    --   11.83 -19.00-150.00   83
  2  \w    -62.00  30.00   1.00   17.07    --   11.83   0.00 120.00   92
  3  \w    -84.00 -59.00   1.00   17.07    --  -12.62 178.00   0.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0524736000
_diffrn_orient_matrix_UB_12      -0.0011496000
_diffrn_orient_matrix_UB_13      -0.0114599000
_diffrn_orient_matrix_UB_21      0.0095402000
_diffrn_orient_matrix_UB_22      -0.0273603000
_diffrn_orient_matrix_UB_23      0.0517356000
_diffrn_orient_matrix_UB_31      -0.0139798000
_diffrn_orient_matrix_UB_32      -0.0229432000
_diffrn_orient_matrix_UB_33      -0.0610036000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.857
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12826
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.857
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.127
_diffrn_reflns_theta_min         3.461
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         5760
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0450P)^2^+1.1095P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1144
_refine_ls_wR_factor_ref         0.1267
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4546
_reflns_number_total             5760
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            DMAC-MPyPz.cif
_cod_data_source_block           DMAC-MPyPz
_cod_database_code               4003450
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C H N O'
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.985
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_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.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C27(H27), C19(H19), C11(H11), C17(H17), C5(H5), C30(H30), C28(H28),
 C16(H16), C1(H1), C3(H3), C9(H9), C18(H18), C29(H29), C4(H4), C8(H8), C2(H2)
2.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C)
;
_olex2_date_sample_data_collection 2019-05-07
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.116
_oxdiff_exptl_absorpt_empirical_full_min 0.832