Regulating the Excited State Chirality to Fabricate High-Performance-Solid-State Circularly Polarized Luminescence Materials
Han, Jianlei; Shi, Yonghong; Jin, Xue; Yang, Xuefeng; Duan, Pengfei; Chemical Science  (2022) –; doi:10.1039/D2SC01846B

data_1566880
_publ_section_title
;
 Regulating the Excited State Chirality to Fabricate
 High-Performance-Solid-State Circularly Polarized Luminescence Materials
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC01846B
_journal_year                    2022
_chemical_formula_moiety         'C50 H32 O4'
_chemical_formula_sum            'C50 H32 O4'
_chemical_formula_weight         696.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-20 deposited with the CCDC.	2022-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.9510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.95280(10)
_cell_length_b                   13.30690(10)
_cell_length_c                   37.0562(4)
_cell_measurement_reflns_used    26424
_cell_measurement_temperature    169.97(11)
_cell_measurement_theta_max      75.0330
_cell_measurement_theta_min      2.3780
_cell_volume                     3426.46(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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      169.97(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.972
_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  25.00   0.50    0.10    --  -47.57  35.00-168.00  122
  2  \w   -112.00 -71.00   0.50    0.10    --  -47.57 -35.00  34.00   82
  3  \w     44.00  79.00   0.50    0.10    --   47.57  35.00-168.00   70
  4  \w    -24.00  11.00   0.50    0.10    --   47.57 -35.00  34.00   70
  5  \w   -151.00-126.00   0.50    0.30    --  -99.00 -35.00  34.00   50
  6  \w     91.00 152.00   0.50    0.30    --  103.25  35.00-168.00  122
  7  \w    -22.00  28.00   0.50    0.10    --  -47.57  19.00 -30.00  100
  8  \w   -118.00 -74.00   0.50    0.10    --  -47.57-125.00-180.00   88
  9  \w   -118.00 -92.00   0.50    0.10    --  -47.57-125.00   0.00   52
 10  \w    -68.00 -33.00   0.50    0.10    --  -47.57 -57.00 -90.00   70
 11  \w    -76.00 -36.00   0.50    0.10    --  -47.57 -19.00 -90.00   80
 12  \w     35.00 108.00   0.50    0.10    --   47.57  77.00-120.00  146
 13  \w     34.00 119.00   0.50    0.10    --   47.57  57.00 -30.00  170
 14  \w   -117.00 -79.00   0.50    0.30    --  -99.00 -71.00 -16.72   76
 15  \w   -156.00-130.00   0.50    0.30    --  -99.00 -78.00 -26.30   52
 16  \w   -106.00 -79.00   0.50    0.30    --  -99.00 -70.00   3.01   54
 17  \w   -142.00 -80.00   0.50    0.30    --  -99.00 -68.00 -92.64  124
 18  \w   -166.00-129.00   0.50    0.30    --  -99.00 -77.00   0.00   74
 19  \w   -167.00 -76.00   0.50    0.30    --  -99.00 -77.00 -60.00  182
 20  \w   -107.00 -62.00   0.50    0.30    --  -99.00 125.00-120.00   90
 21  \w   -106.00 -79.00   0.50    0.30    --  -99.00 -72.00 -80.24   54
 22  \w    -61.00 -26.00   0.50    0.30    --  -99.00  61.00  60.00   70
 23  \w   -101.00 -75.00   0.50    0.30    --  -99.00 -79.00 -42.98   52
 24  \w   -100.00 -75.00   0.50    0.30    --  -99.00 -80.00  -8.53   50
 25  \w   -103.00 -77.00   0.50    0.30    --  -99.00 -74.00 -90.55   52
 26  \w   -102.00 -75.00   0.50    0.30    --  -99.00 -80.00 -73.44   54
 27  \w    -68.00 -27.00   0.50    0.30    --  -99.00  61.00 -90.00   82
 28  \w   -160.00-115.00   0.50    0.30    --  -99.00 -50.00 -58.32   90
 29  \w   -167.00-125.00   0.50    0.30    --  -99.00 -55.00-111.92   84
 30  \w   -101.00 -76.00   0.50    0.30    --  -99.00 -78.00 -26.30   50
 31  \w    -68.00 -43.00   0.50    0.30    --  -99.00  61.00 -60.00   50
 32  \w   -121.00 -76.00   0.50    0.30    --  -99.00 -77.00   0.00   90
 33  \w    -66.00 -30.00   0.50    0.30    --  -99.00  61.00 -30.00   72
 34  \w   -147.00 -79.00   0.50    0.30    --  -99.00 -70.00-101.94  136
 35  \w   -109.00 -26.00   0.50    0.30    --  -99.00 125.00-150.00  166
 36  \w   -111.00 -84.00   0.50    0.30    --  -99.00 -55.00 -61.55   54
 37  \w    -59.00 -26.00   0.50    0.30    --  -99.00 125.00-120.00   66
 38  \w    -67.00 -27.00   0.50    0.30    --  -99.00  61.00  30.00   80
 39  \w   -104.00 -75.00   0.50    0.30    --  -99.00 -80.00 -51.27   58
 40  \w   -103.00 -77.00   0.50    0.30    --  -99.00 -74.00 -72.41   52
 41  \w   -158.00-126.00   0.50    0.30    --  -99.00 -80.00  -8.53   64
 42  \w   -109.00 -83.00   0.50    0.30    --  -99.00 -60.00 -38.95   52
 43  \w   -108.00 -82.00   0.50    0.30    --  -99.00 -61.00 -60.00   52
 44  \w    -60.00 -34.00   0.50    0.30    --  -99.00  61.00   0.00   52
 45  \w   -110.00 -85.00   0.50    0.30    --  -99.00 -50.00 -58.32   50
 46  \w   -102.00 -76.00   0.50    0.30    --  -99.00 -77.00 -30.00   52
 47  \w   -113.00 -86.00   0.50    0.30    --  -99.00 -46.00 -42.04   54
 48  \w   -143.00 -82.00   0.50    0.30    --  -99.00 -61.00   0.00  122
 49  \w     32.00  74.00   0.50    0.30    --  103.25 -61.00  30.00   84
 50  \w     36.00  75.00   0.50    0.30    --  103.25 -61.00 150.00   78
 51  \w     39.00  66.00   0.50    0.30    --  103.25 -61.00  60.00   54
 52  \w     74.00 168.00   0.50    0.30    --  103.25   0.00-180.00  188
 53  \w     37.00  63.00   0.50    0.30    --  103.25   0.00-180.00   52
 54  \w     31.00  74.00   0.50    0.30    --  103.25 -61.00  90.00   86
 55  \w     32.00  75.00   0.50    0.30    --  103.25 -61.00 120.00   86
 56  \w     82.00 108.00   0.50    0.30    --  103.25-125.00-120.00   52
 57  \w     32.00  57.00   0.50    0.30    --  103.25-125.00-120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1164585000
_diffrn_orient_matrix_UB_12      0.0197650000
_diffrn_orient_matrix_UB_13      -0.0338863000
_diffrn_orient_matrix_UB_21      -0.1623760000
_diffrn_orient_matrix_UB_22      -0.0473602000
_diffrn_orient_matrix_UB_23      -0.0237096000
_diffrn_orient_matrix_UB_31      -0.0961419000
_diffrn_orient_matrix_UB_32      0.1037888000
_diffrn_orient_matrix_UB_33      -0.0043599000
_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  0.0370
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            53442
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.215
_diffrn_reflns_theta_min         2.386
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       plate
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.184
_refine_diff_density_min         -0.185
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details
;
 Flack x determined using 5493 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         13331
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0341
_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^)+(0.0506P)^2^+0.4710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0894
_reflns_Friedel_coverage         0.854
_reflns_Friedel_fraction_full    0.971
_reflns_Friedel_fraction_max     0.907
_reflns_number_gt                12664
_reflns_number_total             13331
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01846b5.cif
_cod_data_source_block           tx5443
_cod_database_code               1566880
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHO
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C25(H25A,H25B), C32(H32A,H32B), C33(H33A,H33B), C24A(H24C,
 H24D), C25A(H25C,H25D), C32A(H32C,H32D), C33A(H33C,H33D)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13),
 C20(H20), C21(H21), C23(H23), C27(H27), C28(H28), C31(H31), C36(H36), C37(H37),
  C39(H39), C40(H40), C42(H42), C43(H43), C44(H44), C46(H46), C47(H47),
 C2A(H2A), C3A(H3A), C5A(H5A), C6A(H6A), C8A(H8A), C9A(H9A), C10A(H10A),
 C12A(H12A), C13A(H13A), C20A(H20A), C21A(H21A), C23A(H23A), C27A(H27A),
 C28A(H28A), C31A(H31A), C36A(H36A), C37A(H37A), C39A(H39A), C40A(H40A),
 C42A(H42A), C43A(H43A), C44A(H44A), C46A(H46A), C47A(H47A)
;
_shelx_res_checksum              37657
_shelx_hkl_checksum              54011
_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 1.567
_oxdiff_exptl_absorpt_empirical_full_min 0.585