In Situ Synthesis of Hexadentate Cyclometalated Ir(III) Complexes as Photocatalysts for the Oxidation of Sulfides into Sulfoxides in Water
Fan, Jing-Yan; Yao, Su-Yang; Ye, Bao-Hui; Inorganics 12 (2024) 73–; doi:10.3390/inorganics12030073

data_1571117
_publ_section_title
;
 In Situ Synthesis of Hexadentate Cyclometalated Ir(III) Complexes as
 Photocatalysts for the Oxidation of Sulfides into Sulfoxides in Water
;
_journal_issue                   3
_journal_name_full               Inorganics
_journal_page_first              73
_journal_paper_doi               10.3390/inorganics12030073
_journal_volume                  12
_journal_year                    2024
_chemical_formula_moiety         'C34 H32 Ir N4 O2, F6 P'
_chemical_formula_sum            'C34 H32 F6 Ir N4 O2 P'
_chemical_formula_weight         865.80
_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     iterative
_audit_creation_date             2023-08-24
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_cell_angle_alpha                81.202(2)
_cell_angle_beta                 84.247(2)
_cell_angle_gamma                82.229(2)
_cell_formula_units_Z            2
_cell_length_a                   10.6791(3)
_cell_length_b                   12.5175(4)
_cell_length_c                   13.8170(4)
_cell_measurement_reflns_used    8057
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      72.8660
_cell_measurement_theta_min      4.1620
_cell_volume                     1802.52(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      149.99
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w   -105.00 -13.00   1.00    3.00    --  -41.39 -57.00-180.00   92
  2  \w   -113.00 -21.00   1.00    3.00    --  -41.39 -57.00 -60.00   92
  3  \w    -69.00  30.00   1.00    3.00    --  -41.39  57.00  90.00   99
  4  \w     51.00  87.00   1.00    3.00    --   41.39-125.00-120.00   36
  5  \w     43.00 109.00   1.00   12.00    --  105.29-125.00-150.00   66
  6  \w     80.00 106.00   1.00   12.00    --  105.29 -94.00  60.00   26
  7  \w     99.00 163.00   1.00   12.00    --  105.29 125.00  30.00   64
  8  \w     90.00 129.00   1.00   12.00    --  105.29  45.00 150.00   39
  9  \w     77.00 178.00   1.00   12.00    --  105.29  30.00  90.00  101
 10  \w    147.00 178.00   1.00   12.00    --  105.29  45.00 150.00   31
 11  \w     43.00  88.00   1.00   12.00    --  105.29 -61.00-180.00   45
 12  \w    103.00 128.00   1.00   12.00    --  105.29 -61.00-180.00   25
 13  \w    108.00 172.00   1.00   12.00    --  105.29  77.00   0.00   64
 14  \w    151.00 177.00   1.00   12.00    --  105.29  77.00-120.00   26
 15  \w     50.00  87.00   1.00   12.00    --  105.29-125.00  30.00   37
 16  \w     33.00 134.00   1.00   12.00    --  105.29 -61.00   0.00  101
 17  \w     81.00 111.00   1.00   12.00    --  105.29-125.00 -30.00   30
 18  \w     79.00 111.00   1.00   12.00    --  105.29-125.00  60.00   32
 19  \w     81.00 106.00   1.00   12.00    --  105.29 -94.00-180.00   25
 20  \w     76.00 177.00   1.00   12.00    --  105.29  61.00 -30.00  101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12809
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.055
_diffrn_reflns_theta_min         3.247
_exptl_absorpt_coefficient_mu    8.171
_exptl_absorpt_correction_T_max  0.18934
_exptl_absorpt_correction_T_min  0.08968
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_description       plate
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_size_rad          0.203
_refine_diff_density_max         1.510
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         6987
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0341P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0807
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6429
_reflns_number_total             6987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            3a.cif
_cod_data_source_block           a23061303a0229
_cod_database_code               1571117
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H17-H3A
 2.1 with sigma of 0.02
 H3A-H17
 2.1 with sigma of 0.02
 H2-H4A
 2.4 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B), N4(H4A,H4B), C33(H33A,H33B), C34(H34A,H34B)
3.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C17(H17), C30(H30), C28(H28), C15(H15), C14(H14), C2(H2), C5(H5),
 C31(H31), C4(H4), C3(H3), C18(H18), C8(H8), C24(H24), C20(H20), C19(H19),
 C23(H23), C7(H7)
3.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              9632
_shelx_hkl_checksum              30529
_shelx_fab_checksum              30086
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;