Design Strategy for Ag(I)-Based Thermally Activated Delayed Fluorescence Reaching an Efficiency Breakthrough
Shafikov, Marsel Z.; Suleymanova, Alfiya F.; Czerwieniec, Rafał; Yersin, Hartmut; Chemistry of Materials 29 (2017) 1708–; doi:10.1021/acs.chemmater.6b05175

data_4002708
_publ_section_title
;
 Design Strategy for Ag(I)-Based Thermally Activated Delayed Fluorescence
 Reaching an Efficiency Breakthrough
;
_journal_issue                   4
_journal_name_full               'Chemistry of Materials'
_journal_page_first              1708
_journal_paper_doi               10.1021/acs.chemmater.6b05175
_journal_volume                  29
_journal_year                    2017
_chemical_formula_moiety         'C46 H54 Ag B9 N2 P2, 0.5(C4 H10 O)'
_chemical_formula_sum            'C48 H59 Ag B9 N2 O0.5 P2'
_chemical_formula_weight         939.07
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-05-10
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.02.24 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.6853(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.24578(12)
_cell_length_b                   23.5847(2)
_cell_length_c                   23.60800(17)
_cell_measurement_reflns_used    35923
_cell_measurement_temperature    293.53(10)
_cell_measurement_theta_max      73.4400
_cell_measurement_theta_min      3.7910
_cell_volume                     10014.22(13)
_computing_cell_refinement       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.53(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.966
_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   -115.00 -11.00   0.50   10.00    --  -40.71 -57.00-120.00  208
  2  \w    -98.00  -2.00   0.50   10.00    --  -40.71 125.00  90.00  192
  3  \w     29.00  69.00   0.50   30.00    --  106.98 -30.00 120.00   80
  4  \w     73.00 158.00   0.50   30.00    --  106.98  77.00  60.00  170
  5  \w     23.00 109.00   0.50   30.00    --  106.98 -94.00 -60.00  172
  6  \w     29.00  69.00   0.50   30.00    --  106.98 -30.00 -60.00   80
  7  \w     29.00  69.00   0.50   30.00    --  106.98 -30.00 -30.00   80
  8  \w     32.00  77.00   0.50   30.00    --  106.98 -45.00-150.00   90
  9  \w     28.00 141.00   0.50   30.00    --  106.98 -77.00 -30.00  226
 10  \w     77.00 158.00   0.50   30.00    --  106.98  61.00 120.00  162
 11  \w   -115.00 -11.00   0.50   10.00    --  -40.71 -57.00   0.00  208
 12  \w   -115.00 -11.00   0.50   10.00    --  -40.71 -57.00 120.00  208
 13  \w    -20.00  83.00   0.50   10.00    --   40.71 -99.00 -90.00  206
 14  \w     79.00 119.00   0.50   30.00    --  106.98  45.00 -60.00   80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0195472000
_diffrn_orient_matrix_UB_12      0.0635926000
_diffrn_orient_matrix_UB_13      -0.0032624000
_diffrn_orient_matrix_UB_21      0.0539770000
_diffrn_orient_matrix_UB_22      0.0091191000
_diffrn_orient_matrix_UB_23      -0.0427661000
_diffrn_orient_matrix_UB_31      -0.0636139000
_diffrn_orient_matrix_UB_32      -0.0118844000
_diffrn_orient_matrix_UB_33      -0.0503952000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            59570
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         73.484
_diffrn_reflns_theta_min         3.404
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.089
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.928
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       plate
_exptl_crystal_F_000             3896
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.862
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1180
_refine_ls_number_reflns         19465
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+5.8400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0854
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17850
_reflns_number_total             19465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm6b05175_si_004.cif
_cod_data_source_block           p055_sq
_cod_depositor_comments
;
        Adding full bibliography for 4002708.cif.

2020-05-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C96 H118 Ag2 B18 N4 O P4'
_cod_original_formula_weight         1878.14
_cod_original_formula_moiety         '2(C46 H54 Ag B9 N2 P2), C4 H10 O'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        10014.25(13)
_cod_database_code               4002708
_chemical_oxdiff_formula         'C46 H54 B9 N2 P2 Ag'
_chemical_oxdiff_usercomment     Suleymanova_Yersin_AS22
_reflns_odcompleteness_completeness 99.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H6B-B6 = B6-H6A
 1.1 with sigma of 0.02
 H6B-B5 \\sim H6B-B1
 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C17(H17A,H17B), C50(H50A,H50B), C48(H48A,H48B), C19(H19A,
 H19B), C18(H18A,H18B), C63(H63A,H63B), C4(H4A,H4B), C61(H61A,H61B), C62(H62A,
 H62B), C4AA(H4AA,H4AB), C3AA(H3AA,H3AB), C95(H95A,H95B), C94(H94A,H94B)
3.b Aromatic/amide H refined with riding coordinates:
 C28(H28), C68(H68), C40(H40), C29(H29), C44(H44), C34(H34), C15(H15A),
 C35(H35), C52(H52), C30(H30), C72(H72), C74(H74), C6(H6), C86(H86), C80(H80),
 C59(H59), C32(H32), C76(H76), C13(H13A), C38(H38), C7(H7), C36(H36), C75(H75),
 C78(H78), C12(H12A), C31(H31), C77(H77), C0AA(H0AA), C58(H58), C70(H70),
 C22(H22), C69(H69), C26(H26), C37(H37), C66(H66), C71(H71), C43(H43), C65(H65),
  C53(H53), C81(H81), C41(H41), C24(H24), C42(H42), C90(H90), C23(H23),
 C87(H87), C84(H84), C25(H25), C82(H82), C83(H83), C88(H88), C89(H89)
3.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C47(H47A,H47B,H47C), C64(H64A,H64B,H64C), C2AA(H2AA,H2AB,
 H2AC), C93(H93A,H93B,H93C), C96(H96A,H96B,H96C)
3.d Boron cage BH refined with riding coordinates:
 B7(H7A), B9(H9), B13(H13), B10(H10), B11(H11), B12(H12), B15(H15), B17(H17)
;
_shelx_res_checksum              96020
_shelx_hkl_checksum              6532
_shelx_fab_checksum              33130
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-04-28
_olex2_date_sample_submission    2016-04-22
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems CryoStream 700'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder with inert oil'
_olex2_submission_original_sample_id AS-22
_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 1.833
_oxdiff_exptl_absorpt_empirical_full_min 0.696