Employing racemization strategies to simultaneously enhance the quantum yield, lifetime, and water stability of room-temperature phosphorescent materials.
Lin, Zenggang; Zhang, Peng; Song, Fuqiang; Yang, Yuzhu; Miao, Xuan; Liu, Weisheng; Chemical science 15 (2024) 8052–8061; doi:10.1039/d4sc01719f

data_1571525
_publ_section_title
;
 Employing racemization strategies to simultaneously enhance the quantum
 yield, lifetime, and water stability of room-temperature phosphorescent
 materials.
;
_journal_issue                   21
_journal_name_full               'Chemical science'
_journal_page_first              8052
_journal_page_last               8061
_journal_paper_doi               10.1039/d4sc01719f
_journal_volume                  15
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C48 H34 Br2 N2 O4, 3(C H4 O)'
_chemical_formula_sum            'C51 H42 Br2 N2 O7'
_chemical_formula_weight         954.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-25
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-02-29 deposited with the CCDC.	2024-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.414(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   36.1548(8)
_cell_length_b                   10.7003(2)
_cell_length_c                   12.0413(2)
_cell_measurement_reflns_used    15837
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      75.6220
_cell_measurement_theta_min      2.4730
_cell_volume                     4619.44(16)
_computing_cell_refinement       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.935
_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   -101.00 -75.00   0.50    1.24    --  -45.27 149.00 -48.00   52
  2  \w   -119.00 -66.00   0.50    1.24    --  -45.27-149.00 -94.00  106
  3  \w    -76.00 -50.00   0.50    1.24    --  -45.27 122.00 149.00   52
  4  \w     39.00  93.00   0.50    1.24    --   45.27-122.00  68.00  108
  5  \w     60.00 119.00   0.50    1.24    --   45.27 149.00 -48.00  118
  6  \w   -152.00-127.00   0.50    4.50    -- -100.00-122.00  68.00   50
  7  \w   -122.00 -70.00   0.50    4.50    -- -100.00-149.00 -94.00  104
  8  \w   -164.00-139.00   0.50    4.50    -- -100.00-149.00 -94.00   50
  9  \w   -110.00 -29.00   0.50    4.50    -- -100.00 122.00 149.00  162
 10  \w   -106.00 -81.00   0.50    4.50    -- -100.00 149.00 -48.00   50
 11  \w    134.00 161.00   0.50    4.50    --  109.64 149.00 -48.00   54
 12  \w     82.00 114.00   0.50    4.50    --  109.64 149.00 -48.00   64
 13  \w     78.00 172.00   0.50    4.50    --  109.64 122.00 149.00  188
 14  \w     77.00 110.00   0.50    4.50    --  109.64-122.00  68.00   66
 15  \w    -29.00  21.00   0.50    1.24    --  -45.27  19.00  60.00  100
 16  \w    -29.00  22.00   0.50    1.24    --  -45.27  19.00 120.00  102
 17  \w    -27.00  34.00   0.50    1.24    --  -45.27  19.00 -30.00  122
 18  \w     70.00 110.00   0.50    1.24    --   45.27-149.00 -94.00   80
 19  \w    -33.00  22.00   0.50    1.24    --   45.27 -19.00 120.00  110
 20  \w    -26.00  -1.00   0.50    1.24    --   45.27 -37.00 -60.00   50
 21  \w    -32.00  24.00   0.50    1.24    --   45.27 -19.00  60.00  112
 22  \w    -19.00  23.00   0.50    1.24    --   45.27 -19.00 150.00   84
 23  \w    -53.00 -25.00   0.50    4.50    -- -100.00  45.00-150.00   56
 24  \w    -85.00 -26.00   0.50    4.50    -- -100.00  77.00 -30.00  118
 25  \w   -175.00-139.00   0.50    4.50    -- -100.00 -30.00 120.00   72
 26  \w   -175.00 -72.00   0.50    4.50    -- -100.00 -15.00 -90.00  206
 27  \w   -106.00 -77.00   0.50    4.50    -- -100.00 107.00  92.15   58
 28  \w    -54.00 -25.00   0.50    4.50    -- -100.00  45.00 120.00   58
 29  \w   -176.00-139.00   0.50    4.50    -- -100.00 -30.00 -30.00   74
 30  \w   -120.00 -29.00   0.50    4.50    -- -100.00 136.00  14.58  182
 31  \w    -54.00 -26.00   0.50    4.50    -- -100.00  45.00 -90.00   56
 32  \w   -132.00-107.00   0.50    4.50    -- -100.00 154.00-146.75   50
 33  \w   -154.00 -91.00   0.50    4.50    -- -100.00 -94.00  90.00  126
 34  \w    -59.00 -30.00   0.50    4.50    -- -100.00 125.00  60.00   58
 35  \w   -111.00 -85.00   0.50    4.50    -- -100.00 125.00  60.00   52
 36  \w   -112.00 -30.00   0.50    4.50    -- -100.00 125.00-180.00  164
 37  \w   -160.00 -82.00   0.50    4.50    -- -100.00-125.00-150.00  156
 38  \w   -136.00 -80.00   0.50    4.50    -- -100.00 -30.00 120.00  112
 39  \w    -81.00 -55.00   0.50    4.50    -- -100.00 154.00-146.75   52
 40  \w     51.00  90.00   0.50    4.50    --  109.64 -77.00  90.00   78
 41  \w     96.00 121.00   0.50    4.50    --  109.64  30.00  60.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0137464500
_diffrn_orient_matrix_UB_12      0.0697309500
_diffrn_orient_matrix_UB_13      0.0989098000
_diffrn_orient_matrix_UB_21      0.0405100000
_diffrn_orient_matrix_UB_22      0.0359919000
_diffrn_orient_matrix_UB_23      0.0439671000
_diffrn_orient_matrix_UB_31      -0.0041664500
_diffrn_orient_matrix_UB_32      0.1206581500
_diffrn_orient_matrix_UB_33      -0.0702094000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25307
_diffrn_reflns_point_group_measured_fraction_full 0.809
_diffrn_reflns_point_group_measured_fraction_max 0.750
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.379
_diffrn_reflns_theta_min         2.465
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.657
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50481
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
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    1.373
_exptl_crystal_description       block
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details
;
 Flack x determined using 1918 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.069(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         7289
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0898P)^2^+1.1996P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1336
_refine_ls_wR_factor_ref         0.1403
_reflns_Friedel_coverage         0.520
_reflns_Friedel_fraction_full    0.601
_reflns_Friedel_fraction_max     0.544
_reflns_number_gt                6438
_reflns_number_total             7289
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01719f2.cif
_cod_data_source_block           linzengg_1220_auto
_cod_depositor_comments
'Adding full bibliography for 1571524--1571527.cif.'
_cod_database_code               1571525
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.741
_shelx_estimated_absorpt_t_min   0.707
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H) groups
2. Others
 Fixed Sof: O2(0.8) H2A(0.8) H45A(0.8) H45B(0.8) H45C(0.8) H45D(0.2) H45E(0.2)
 H45F(0.2) O8(0.2) H8(0.2)
3.a Aromatic/amide H refined with riding coordinates:
 N1(H1A), N2(H2), C3(H3), C5(H5), C9(H9), C11(H11), C12(H12), C13(H13),
 C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C25(H25), C27(H27),
  C28(H28), C29(H29), C30(H30), C33(H33), C35(H35), C36(H36), C37(H37),
 C38(H38), C39(H39), C41(H41), C42(H42), C46(H46), C48(H48), C49(H49), C50(H50),
  C51(H51)
3.b Tetrahedral OH refined with riding coordinates:
 O2(H2A), O8(H8)
3.c Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C), C45(H45D,H45E,H45F), C47(H47A,H47B,H47C), C43(H43A,H43B,
 H43C)
3.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O7(H7), O3(H3A), O5(H5A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              88852
_shelx_fab_checksum              83983
_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 2.814
_oxdiff_exptl_absorpt_empirical_full_min 0.247