Highly Efficient Iridium-Based Photosensitizers for Thia-Paternò‒Büchi Reaction and Aza-Photocyclization
He, Jian; Bai, Zhi-Qin; Yuan, Pan-Feng; Wu, Li-Zhu; Liu, Qiang; ACS Catalysis  (2020) 446–455; doi:10.1021/acscatal.0c05005

data_4518335
_publ_section_title
;
 Highly Efficient Iridium-Based Photosensitizers for
 Thia-Patern\`o--B\"uchi Reaction and Aza-Photocyclization
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              446
_journal_page_last               455
_journal_paper_doi               10.1021/acscatal.0c05005
_journal_year                    2020
_chemical_formula_moiety         'C37 H20 F10 Ir N6, F6 P'
_chemical_formula_sum            'C37 H20 F16 Ir N6 P'
_chemical_formula_weight         1075.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-10-29
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_cell_length_c                   19.3081(9)
_cell_measurement_reflns_used    3779
_cell_measurement_temperature    293.73(10)
_cell_measurement_theta_max      25.6220
_cell_measurement_theta_min      3.9110
_cell_volume                     3822.9(3)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.73(10)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   -4.00   25.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4273  -99.0000 -150.0000 29

  2 omega   40.00  102.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867  178.0000    0.0000 62

  3 omega   65.00   96.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867   38.0000   60.0000 31

  4 omega    6.00   94.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867   38.0000   30.0000 88

  5 omega   30.00   63.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867  -99.0000   30.0000 33
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0079895000
_diffrn_orient_matrix_UB_12      -0.0399220000
_diffrn_orient_matrix_UB_13      0.0189237000
_diffrn_orient_matrix_UB_21      0.0013385000
_diffrn_orient_matrix_UB_22      0.0217910000
_diffrn_orient_matrix_UB_23      0.0325712000
_diffrn_orient_matrix_UB_31      -0.0549258000
_diffrn_orient_matrix_UB_32      -0.0052470000
_diffrn_orient_matrix_UB_33      -0.0085952000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0752
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14974
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         3.434
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.651
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.869
_exptl_crystal_description       block
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.740
_refine_diff_density_min         -1.156
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         7521
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0320P)^2^+2.8328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.1043
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5510
_reflns_number_total             7521
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c05005_si_007.cif
_cod_data_source_block           hej(4)_1029
_cod_database_code               4518335
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.668
_shelx_estimated_absorpt_t_min   0.576
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C18(H18), C20(H20), C23(H23), C26(H26), C34(H34), C35(H35),
 C36(H36), C37(H37), C39(H39), C40(H40), C42(H42), C43(H43), C56(H56), C59(H59),
  C60(H60), C2AA(H2AA), C1AA(H1AA), C1(H1), C5AA(H5AA)
;
_shelx_res_checksum              52244
_shelx_hkl_checksum              92633
_olex2_date_sample_data_collection 2018-10-29
_olex2_submission_special_instructions 'No special instructions were received'