Circularly Polarized Thermally Activated Delayed Fluorescence Emitters in Through-Space Charge Transfer on Asymmetric Spiro Skeletons.
Yang, Sheng-Yi; Wang, Ya-Kun; Peng, Chen-Chen; Wu, Zheng-Guang; Yuan, Shuai; Yu, You-Jun; Li, Hao; Wang, Tong-Tong; Li, Hong-Cheng; Zheng, You-Xuan; Jiang, Zuo-Quan; Liao, Liang-Sheng; Journal of the American Chemical Society 142 (2020) 17756–17765; doi:10.1021/jacs.0c08980

data_4135279
_publ_section_title
;
 Circularly Polarized Thermally Activated Delayed Fluorescence Emitters in
 Through-Space Charge Transfer on Asymmetric Spiro Skeletons.
;
_journal_issue                   41
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17756
_journal_page_last               17765
_journal_paper_doi               10.1021/jacs.0c08980
_journal_volume                  142
_journal_year                    2020
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C52 H32 N4 O'
_chemical_formula_sum            'C52 H32 N4 O'
_chemical_formula_weight         728.81
_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             2020-07-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.527(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.8332(4)
_cell_length_b                   15.6637(6)
_cell_length_c                   43.2298(16)
_cell_measurement_reflns_used    9134
_cell_measurement_temperature    170
_cell_measurement_theta_max      74.796
_cell_measurement_theta_min      3.001
_cell_volume                     7328.4(5)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            88708
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         75.032
_diffrn_reflns_theta_min         2.046
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.621
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.6387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1662 before and 0.0843 after correction. The Ratio of minimum to maximum transmission is 0.8473. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       block
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Flack x determined using 10365 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.10(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2053
_refine_ls_number_reflns         28627
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0982
_refine_ls_R_factor_gt           0.0945
_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^)+(0.1132P)^2^+15.3404P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2557
_refine_ls_wR_factor_ref         0.2579
_reflns_Friedel_coverage         0.852
_reflns_Friedel_fraction_full    0.929
_reflns_Friedel_fraction_max     0.905
_reflns_number_gt                26931
_reflns_number_total             28627
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c08980_si_007.cif
_cod_data_source_block           cu_22020405_0m
_cod_depositor_comments
'Adding full bibliography for 4135274--4135279.cif.'
_cod_database_code               4135279
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.952
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C181(H181), C157(H157), C126(H126), C54(H54), C34(H34), C91(H91), C38(H38),
 C98(H98), C52(H52), C17(H17), C172(H172), C166(H166), C123(H123), C18(H18),
 C151(H151), C180(H180), C90(H90), C125(H125), C171(H171), C47(H47), C168(H168),
  C207(H207), C195(H195), C175(H175), C102(H102), C4(H4), C5(H5), C46(H46),
 C39(H39), C50(H50), C89(H89), C205(H205), C23(H23), C108(H108), C193(H193),
 C148(H148), C145(H145), C43(H43), C12(H12), C20(H20), C69(H69), C97(H97),
 C187(H187), C51(H51), C21(H21), C3(H3), C161(H161), C116(H116), C206(H206),
 C31(H31), C182(H182), C128(H128), C158(H158), C92(H92), C160(H160), C57(H57),
 C194(H194), C33(H33), C40(H40), C25(H25), C150(H150), C174(H174), C119(H119),
 C118(H118), C1(H1), C122(H122), C24(H24), C45(H45), C103(H103), C99(H99),
 C61(H61), C44(H44), C55(H55), C63(H63), C83(H83), C167(H167), C16(H16),
 C120(H120), C70(H70), C186(H186), C183(H183), C192(H192), C32(H32), C117(H117),
  C143(H143), C107(H107), C111(H111), C201(H201), C62(H62), C198(H198),
 C10(H10), C129(H129), C106(H106), C130(H130), C188(H188), C189(H189),
 C200(H200), C149(H149), C87(H87), C11(H11), C139(H139), C144(H144), C71(H71),
 C199(H199), C80(H80), C84(H84), C110(H110), C86(H86), C76(H76), C85(H85),
 C137(H137), C56(H56), C136(H136), C156(H156), C184(H184), C159(H159), C14(H14),
  C79(H79), C155(H155), C2(H2), C105(H105), C154(H154), C77(H77), C13(H13),
 C104(H104), C190(H190), C138(H138), C78(H78)
;
_olex2_submission_special_instructions 'No special instructions were received'