Amplification of luminescence of stable radicals by coordination to NHC–gold(i) complex
Hattori, Yohei; Kitajima, Ryota; Matsuoka, Ryota; Kusamoto, Tetsuro; Nishihara, Hiroshi; Uchida, Kingo; Chemical Communications  (2022) –; doi:10.1039/D1CC06555F

data_7129643
_publ_section_title
;
 Amplification of luminescence of stable radicals by coordination to
 NHC--gold(i) complex
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06555F
_journal_year                    2022
_chemical_formula_moiety
'C45 H44 Au Cl6 F2 N3, F6 Sb, C4 H8 O, C6 H12'
_chemical_formula_sum            'C55 H64 Au Cl6 F8 N3 O Sb'
_chemical_formula_weight         1466.50
_chemical_name_systematic        '4SbF6 THF cyclohexane'
_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             2021-11-12
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2021-11-17 deposited with the CCDC.	2022-01-25 downloaded from the CCDC.
;
_cell_angle_alpha                90.337(6)
_cell_angle_beta                 95.247(7)
_cell_angle_gamma                91.396(6)
_cell_formula_units_Z            4
_cell_length_a                   12.4979(2)
_cell_length_b                   21.0791(4)
_cell_length_c                   22.2535(4)
_cell_measurement_reflns_used    53552
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.06
_cell_volume                     5836.07(19)
_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_temperature      103.15
_diffrn_detector                 'Rigaku curved IP area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'Imaging plate area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku VariMax RAPID'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            67463
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.351
_diffrn_reflns_theta_min         1.802
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              'MicroMax 007'
_exptl_absorpt_coefficient_mu    3.315
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_description       prism
_exptl_crystal_F_000             2908
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF, cyclohexane'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.979
_refine_diff_density_min         -1.191
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1333
_refine_ls_number_reflns         21345
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0534P)^2^+19.8440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1237
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17684
_reflns_number_total             21345
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06555f2.cif
_cod_data_source_block           shelxl_CCDC1
_cod_database_code               7129643
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.673
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(O2A)=Sof(C111)=Sof(H11C)=Sof(H11D)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C1B)=
 Sof(H1BA)=Sof(H1BB)=Sof(C1C)=Sof(H1CA)=Sof(H1CB)=1-FVAR(1)
 Sof(O2)=Sof(C109)=Sof(H10O)=Sof(H10P)=Sof(C110)=Sof(H11A)=Sof(H11B)=Sof(C107)=
 Sof(H10Q)=Sof(H10R)=Sof(C108)=Sof(H10S)=Sof(H10T)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C31(H31), C43(H43), C85(H85), C40(H40), C28(H28), C76(H76), C88(H88), C73(H73)
3.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C66(H66A,H66B), C65(H65A,H65B), C20(H20A,H20B), C99(H99A,
 H99B), C100(H10M,H10N), C96(H96A,H96B), C97(H97A,H97B), C98(H98A,H98B),
 C109(H10O,H10P), C93(H93A,H93B), C95(H95A,H95B), C91(H91A,H91B), C101(H10A,
 H10B), C104(H10C,H10D), C94(H94A,H94B), C103(H10E,H10F), C92(H92A,H92B),
 C110(H11A,H11B), C102(H10G,H10H), C107(H10Q,H10R), C105(H10I,H10J), C106(H10K,
 H10L), C108(H10S,H10T), C111(H11C,H11D), C1A(H1AA,H1AB), C1B(H1BA,H1BB),
 C1C(H1CA,H1CB)
3.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C26(H26), C60(H60), C11(H11), C62(H62), C9(H9), C82(H82), C83(H83),
 C37(H37), C81(H81), C24(H24), C36(H36), C70(H70), C69(H69), C1(H1), C38(H38),
 C50(H50), C5(H5), C54(H54), C46(H46), C71(H71), C15(H15), C56(H56), C17(H17)
3.d Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C89(H89A,H89B,H89C), C29(H29A,H29B,
 H29C), C44(H44A,H44B,H44C), C30(H30A,H30B,H30C), C87(H87A,H87B,H87C), C41(H41A,
 H41B,H41C), C86(H86A,H86B,H86C), C90(H90A,H90B,H90C), C42(H42A,H42B,H42C),
 C45(H45A,H45B,H45C), C78(H78A,H78B,H78C), C75(H75A,H75B,H75C), C77(H77A,H77B,
 H77C), C74(H74A,H74B,H74C)
;
_shelx_res_checksum              60351
_shelx_hkl_checksum              56469
_olex2_submission_special_instructions 'No special instructions were received'