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_4518336
_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         'C32 H16 F10 Ir N5'
_chemical_formula_sum            'C32 H16 F10 Ir N5'
_chemical_formula_weight         852.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yac'
_space_group_name_H-M_alt        'C 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-11-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.187(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.6250(6)
_cell_length_b                   17.8886(5)
_cell_length_c                   17.9372(6)
_cell_measurement_reflns_used    3495
_cell_measurement_temperature    293.80(10)
_cell_measurement_theta_max      27.4570
_cell_measurement_theta_min      3.7550
_cell_volume                     6287.4(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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      293.80(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  -48.00   46.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867  -57.0000    0.0000 94

  2 omega   -1.00   91.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867   57.0000  150.0000 92

  3 omega   -8.00   46.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867   77.0000  -30.0000 54
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0144928000
_diffrn_orient_matrix_UB_12      0.0130685000
_diffrn_orient_matrix_UB_13      0.0346851000
_diffrn_orient_matrix_UB_21      0.0251522000
_diffrn_orient_matrix_UB_22      -0.0284236000
_diffrn_orient_matrix_UB_23      -0.0003980000
_diffrn_orient_matrix_UB_31      0.0216430000
_diffrn_orient_matrix_UB_32      0.0243292000
_diffrn_orient_matrix_UB_33      -0.0191282000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0655
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            12695
_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         3.453
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.338
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62024
_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 green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_description       block
_exptl_crystal_F_000             3280
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.734
_refine_diff_density_min         -1.215
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6177
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0447P)^2^+50.2368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1283
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4787
_reflns_number_total             6177
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c05005_si_004.cif
_cod_data_source_block           hej(3)_1029
_cod_original_sg_symbol_Hall     '-C 2ybc'
_cod_database_code               4518336
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.624
_shelx_estimated_absorpt_t_min   0.526
_reflns_odcompleteness_completeness 99.71
_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:
 C7(H7), C14(H14), C18(H18), C19(H19), C22(H22), C23(H23), C32(H32), C33(H33),
 C35(H35), C36(H36), C37(H37), C40(H40), C41(H41), C48(H48), C52(H52), C1(H1)
;
_shelx_res_checksum              60944
_shelx_hkl_checksum              46377
_olex2_date_sample_data_collection 2018-10-29
_olex2_submission_special_instructions 'No special instructions were received'