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_1571118
_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
'0.267(C34 H28 Ir N4 O2), 0.267(F6 P), 0.267[CHCl3]'
_chemical_formula_sum            'C34 H28 F6 Ir N4 O2 P'
_chemical_formula_weight         861.77
_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     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                90
_cell_angle_beta                 90.3740(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.58160(10)
_cell_length_b                   18.5399(2)
_cell_length_c                   17.3118(2)
_cell_measurement_reflns_used    11713
_cell_measurement_temperature    149.98(10)
_cell_measurement_theta_max      72.9190
_cell_measurement_theta_min      3.4180
_cell_volume                     3396.19(6)
_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_environment      N~2~
_diffrn_ambient_temperature      149.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_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    -77.00 -52.00   1.00    2.00    --  -41.39 125.00 -30.00   25
  2  \w    -66.00  32.00   1.00    2.00    --  -41.39  38.00 150.00   98
  3  \w     93.00 122.00   1.00    2.00    --   41.39 170.00 -33.00   29
  4  \w     12.00  50.00   1.00    2.00    --   41.39 -77.00 -90.00   38
  5  \w     42.00 110.00   1.00    8.00    --  105.29-125.00-180.00   68
  6  \w     86.00 147.00   1.00    8.00    --  105.29  45.00  30.00   61
  7  \w    111.00 161.00   1.00    8.00    --  105.29 125.00   0.00   50
  8  \w     32.00 104.00   1.00    8.00    --  105.29 -30.00-150.00   72
  9  \w    -64.00 -15.00   1.00    2.00    --  -41.39 125.00   0.00   49
 10  \w    -20.00  10.00   1.00    2.00    --   41.39 -77.00 -60.00   30
 11  \w    111.00 149.00   1.00    8.00    --  105.29  77.00 -60.00   38
 12  \w     73.00 111.00   1.00    8.00    --  105.29-125.00 -60.00   38
 13  \w     58.00  94.00   1.00    8.00    --  105.29-125.00   0.00   36
 14  \w    108.00 140.00   1.00    8.00    --  105.29  77.00 150.00   32
 15  \w    113.00 162.00   1.00    8.00    --  105.29  77.00-180.00   49
 16  \w     84.00 129.00   1.00    8.00    --  105.29 -45.00  90.00   45
 17  \w   -106.00 -70.00   1.00    2.00    --  -41.39 -57.00  60.00   36
 18  \w   -108.00 -34.00   1.00    2.00    --  -41.39 -38.00 -30.00   74
 19  \w    -47.00  -6.00   1.00    2.00    --  -41.39 125.00-180.00   41
 20  \w     52.00  91.00   1.00    2.00    --   41.39-125.00-180.00   39
 21  \w    148.00 178.00   1.00    8.00    --  105.29  77.00 -60.00   30
 22  \w     24.00  49.00   1.00    8.00    --  105.29 -94.00   0.00   25
 23  \w    114.00 150.00   1.00    8.00    --  105.29  77.00-120.00   36
 24  \w     23.00  59.00   1.00    8.00    --  105.29 -94.00-180.00   36
 25  \w    103.00 129.00   1.00    8.00    --  105.29  77.00 -60.00   26
 26  \w     75.00 106.00   1.00    8.00    --  105.29 -94.00-180.00   31
 27  \w     98.00 144.00   1.00    8.00    --  105.29 125.00-120.00   46
 28  \w    108.00 143.00   1.00    8.00    --  105.29  77.00  30.00   35
 29  \w     26.00 106.00   1.00    8.00    --  105.29 -94.00  90.00   80
 30  \w     47.00  73.00   1.00    8.00    --  105.29 -94.00 -60.00   26
 31  \w     81.00 106.00   1.00    8.00    --  105.29 -94.00 -60.00   25
 32  \w     81.00 106.00   1.00    8.00    --  105.29 -94.00   0.00   25
 33  \w     81.00 107.00   1.00    8.00    --  105.29-115.00-173.00   26
 34  \w     87.00 112.00   1.00    8.00    --  105.29-125.00 -60.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1089805000
_diffrn_orient_matrix_UB_12      -0.0515497000
_diffrn_orient_matrix_UB_13      0.0212843000
_diffrn_orient_matrix_UB_21      -0.0934632000
_diffrn_orient_matrix_UB_22      -0.0637349000
_diffrn_orient_matrix_UB_23      0.0014496000
_diffrn_orient_matrix_UB_31      0.0243306000
_diffrn_orient_matrix_UB_32      -0.0137119000
_diffrn_orient_matrix_UB_33      -0.0863617000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0694
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28356
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.048
_diffrn_reflns_theta_min         3.493
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           3.57
_diffrn_source_power             0.24954300000000001
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           69.9
_exptl_absorpt_coefficient_mu    8.674
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56223
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    1.685
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.134
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         6708
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0449P)^2^+8.4109P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1009
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5530
_reflns_number_total             6708
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            3.cif
_cod_data_source_block           exp_3482
_cod_database_code               1571118
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_usercomment     67B_18C6
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 N3(H3), N4(H4)
1.b Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C33(H33A,H33B)
1.c Aromatic/amide H refined with riding coordinates:
 C28(H28), C15(H15), C24(H24), C7(H7), C8(H8), C12(H12), C3(H3A), C14(H14),
 C31(H31), C21(H21), C23(H23), C4(H4A), C5(H5), C30(H30), C19(H19), C20(H20)
1.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C32(H32A,H32B,H32C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              56504
_shelx_hkl_checksum              75897
_shelx_fab_checksum              42542
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.632
_oxdiff_exptl_absorpt_empirical_full_min 0.346