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_4518337
_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         'C18 H15 N O3 S2'
_chemical_formula_sum            'C18 H15 N O3 S2'
_chemical_formula_weight         357.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
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Olex2 1.2
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_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)
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_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)'
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_diffrn_ambient_temperature      293.75(10)
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_diffrn_measurement_details
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  1 omega -102.00  -77.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4273  178.0000  -30.0000 25

  2 omega    1.00   86.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867   57.0000 -180.0000 85

  3 omega   -9.00   96.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867   38.0000   90.0000 105

  4 omega   39.00   70.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7867  178.0000  -30.0000 31
;
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_diffrn_measurement_method       '\w scans'
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_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_unetI/netI     0.0570
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_diffrn_reflns_theta_min         3.377
_diffrn_source                   'SuperNova (Mo) X-ray Source'
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_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57303
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_exptl_absorpt_process_details
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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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
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_refine_diff_density_max         0.207
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_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3278
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
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'w=1/[\s^2^(Fo^2^)+(0.0412P)^2^] where P=(Fo^2^+2Fc^2^)/3'
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_reflns_threshold_expression     'I > 2\s(I)'
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_cod_original_cell_volume        1667.35(17)
_cod_database_code               4518337
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.945
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18),
 C19(H19), C20(H20), C22(H22)
2.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C)
;
_shelx_res_checksum              46749
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_olex2_date_sample_data_collection 2018-11-08
_olex2_submission_special_instructions 'No special instructions were received'