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_4135275
_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_formula_moiety         'C H2 Cl2, C52 H32 N4 O'
_chemical_formula_sum            'C53 H34 Cl2 N4 O'
_chemical_formula_weight         813.74
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-09-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                88.5140(10)
_cell_angle_beta                 81.0940(10)
_cell_angle_gamma                73.9990(10)
_cell_formula_units_Z            4
_cell_length_a                   10.7802(4)
_cell_length_b                   16.7891(6)
_cell_length_c                   23.3522(9)
_cell_measurement_reflns_used    8190
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.335
_cell_measurement_theta_min      2.632
_cell_volume                     4013.2(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 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      173.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            41406
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.297
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.209
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1230 before and 0.0566 after correction. The Ratio of minimum to maximum transmission is 0.8849. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.647
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.019(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1083
_refine_ls_number_reflns         14093
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1550
_refine_ls_R_factor_gt           0.1076
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1633P)^2^+8.1544P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2889
_refine_ls_wR_factor_ref         0.3298
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8841
_reflns_number_total             14093
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c08980_si_003.cif
_cod_data_source_block           22019938hcz_0m
_cod_depositor_comments
'Adding full bibliography for 4135274--4135279.cif.'
_cod_database_code               4135275
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.990
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1(10)
 0(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C54(H54A,H54B), C55(H55A,H55B)
3.b Aromatic/amide H refined with riding coordinates:
 C34(H34), C70(H70), C79(H79), C10(H10), C80(H80), C71(H71), C35(H35),
 C88(H88), C78(H78), C58(H58), C28(H28), C38(H38), C21(H21), C72(H72), C89(H89),
  C68(H68), C17(H17), C92(H92), C11(H11), C73(H73), C37(H37), C12(H12),
 C91(H91), C16(H16), C22(H22), C56(H56), C65(H65), C15(H15), C29(H29), C57(H57),
  C24(H24), C14(H14), C23(H23), C30(H30), C67(H67), C100(H100), C66(H66),
 C97(H97), C98(H98), C96(H96), C99(H99), C53(H53), C45(H45), C103(H103),
 C44(H44), C1(H1), C51(H51), C46(H46), C83(H83), C47(H47), C52(H52), C104(H104),
  C50(H50), C105(H105), C43(H43), C49(H49), C106(H106), C2(H2), C84(H84),
 C107(H107), C4(H4), C86(H86), C85(H85), C3(H3)
;
_olex2_submission_special_instructions 'No special instructions were received'