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_1571119
_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         'C32 H26 F2 Ir N4, 2(F3 P0.5)'
_chemical_formula_sum            'C32 H26 F8 Ir N4 P'
_chemical_formula_weight         841.74
_chemical_name_systematic        F-yea
_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                76.136(4)
_cell_angle_beta                 84.487(3)
_cell_angle_gamma                77.048(3)
_cell_formula_units_Z            2
_cell_length_a                   8.3615(3)
_cell_length_b                   10.6980(5)
_cell_length_c                   19.2560(7)
_cell_measurement_reflns_used    7136
_cell_measurement_temperature    149.98(10)
_cell_measurement_theta_max      72.9210
_cell_measurement_theta_min      4.3140
_cell_volume                     1628.11(12)
_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 0.998
_diffrn_measured_fraction_theta_max 0.969
_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   -113.00 -14.00   1.00    1.00    --  -41.14 -57.00-120.00   99
  2  \w    -12.00  28.00   1.00    1.00    --  -41.14  57.00  30.00   40
  3  \w    -62.00 -17.00   1.00    1.00    --  -41.14  57.00  30.00   45
  4  \w    -33.00  66.00   1.00    1.00    --   41.14 -38.00  90.00   99
  5  \w     56.00  89.00   1.00    1.00    --   41.14-125.00-180.00   33
  6  \w     27.00  53.00   1.00    1.00    --   41.14-125.00  90.00   26
  7  \w     29.00 130.00   1.00    1.00    --  105.29 -77.00 150.00  101
  8  \w     43.00 101.00   1.00    1.00    --  105.29-125.00  60.00   58
  9  \w    108.00 160.00   1.00    1.00    --  105.29 125.00  90.00   52
 10  \w     25.00 106.00   1.00    1.00    --  105.29 -94.00 -60.00   81
 11  \w    107.00 177.00   1.00    1.00    --  105.29  77.00 -30.00   70
 12  \w    106.00 165.00   1.00    1.00    --  105.29  77.00-180.00   59
 13  \w    109.00 168.00   1.00    1.00    --  105.29  77.00 120.00   59
 14  \w     65.00 112.00   1.00    1.00    --  105.29-125.00 -90.00   47
 15  \w     82.00 108.00   1.00    1.00    --  105.29-125.00-180.00   26
 16  \w     33.00 119.00   1.00    1.00    --  105.29 -45.00  30.00   86
 17  \w     77.00 177.00   1.00    1.00    --  105.29  30.00 -90.00  100
 18  \w     52.00 107.00   1.00    1.00    --  105.29 -98.00  64.63   55
;
_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      0.0201465000
_diffrn_orient_matrix_UB_12      0.1425174000
_diffrn_orient_matrix_UB_13      -0.0315199000
_diffrn_orient_matrix_UB_21      -0.1771089000
_diffrn_orient_matrix_UB_22      0.0516091000
_diffrn_orient_matrix_UB_23      0.0260662000
_diffrn_orient_matrix_UB_31      0.0635575000
_diffrn_orient_matrix_UB_32      0.0046727000
_diffrn_orient_matrix_UB_33      0.0716326000
_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  0.0540
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11552
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.953
_diffrn_reflns_theta_min         4.352
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.072
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53379
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_description       plate
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.889
_refine_diff_density_min         -2.026
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         6299
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0446P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.0930
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5831
_reflns_number_total             6299
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1a.cif
_cod_data_source_block           a23061302a0229
_cod_database_code               1571119
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNFIr
_chemical_oxdiff_usercomment     '8 F-yea-j'
_olex2_refinement_description
;
1. Restrained distances
 H2-H3A
 2.1 with sigma of 0.02
 H3A-H2
 2.2 with sigma of 0.02
 H17-H4A
 2.3 with sigma of 0.02
 H4A-H17
 2.3 with sigma of 0.02
2.a Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B), N4(H4A,H4B), C32(H32A,H32B), C31(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C23(H23), C7(H7), C12(H12), C22(H22), C15(H15), C2(H2), C8(H8),
 C20(H20), C29(H29), C30(H30), C17(H17), C14(H14), C5(H5), C3(H3), C19(H19),
 C18(H18), C4(H4)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              32851
_shelx_hkl_checksum              78164
_shelx_fab_checksum              68362
_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 1.922
_oxdiff_exptl_absorpt_empirical_full_min 0.706