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_4518340
_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         'C38 H21 F10 Ir N5, F6 P'
_chemical_formula_sum            'C38 H21 F16 Ir N5 P'
_chemical_formula_weight         1074.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-09-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 107.616(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.3077(7)
_cell_length_b                   20.7973(8)
_cell_length_c                   18.9412(7)
_cell_measurement_reflns_used    4295
_cell_measurement_temperature    293.63(10)
_cell_measurement_theta_max      26.4360
_cell_measurement_theta_min      3.9040
_cell_volume                     7624.6(5)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293.63(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  -16.00   10.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4273  -99.0000   30.0000 26

  2 omega   -1.00   67.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867   57.0000   60.0000 68

  3 omega  -34.00   81.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867   19.0000    0.0000 115

  4 omega   71.00  104.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867 -178.0000   30.0000 33
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0046134000
_diffrn_orient_matrix_UB_12      -0.0300202000
_diffrn_orient_matrix_UB_13      0.0156631000
_diffrn_orient_matrix_UB_21      -0.0033336000
_diffrn_orient_matrix_UB_22      0.0160265000
_diffrn_orient_matrix_UB_23      0.0317745000
_diffrn_orient_matrix_UB_31      -0.0362131000
_diffrn_orient_matrix_UB_32      0.0023330000
_diffrn_orient_matrix_UB_33      -0.0169505000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0718
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15251
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.37
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.660
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43223
_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    1.873
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4160
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.018
_refine_diff_density_min         -1.150
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         7493
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0126P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0589
_refine_ls_wR_factor_ref         0.0682
_reflns_number_gt                5719
_reflns_number_total             7493
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs0c05005_si_005.cif
_cod_data_source_block           pc12
_cod_database_code               4518340
_chemical_oxdiff_formula         'C H'
_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. Uiso/Uaniso restraints and constraints
Uanis(F14) \\sim Ueq, Uanis(F14B) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F13B)
\\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F16B) \\sim Ueq, Uanis(F15B) \\sim Ueq,
Uanis(F15) \\sim Ueq, Uanis(F4B) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F5B)
\\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F3B) \\sim Ueq, Uanis(F3) \\sim Ueq: with
sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: F3(0.6) F4(0.6) F5(0.6) F3B(0.4) F4B(0.4) F5B(0.4) F13(0.5)
 F14(0.5) F15(0.5) F16(0.5) F13B(0.5) F14B(0.5) F15B(0.5) F16B(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C8(H8), C9(H9), C11(H11), C14(H14), C16(H16), C20(H20),
 C21(H21), C23(H23), C25(H25), C26(H26), C27(H27), C28(H28), C31(H31), C32(H32),
  C34(H34), C35(H35), C36(H36), C37(H37), C38(H38)
;
_olex2_date_sample_data_collection 2018-07-30
_olex2_submission_special_instructions 'No special instructions were received'