Synthesis, structure and reactivity of iridium complexes containing a bis-cyclometalated tridentate C^N^C ligand.
Cheung, Wai-Man; Chong, Man-Chun; Sung, Herman H.-Y.; Cheng, Shun-Cheung; Williams, Ian D.; Ko, Chi-Chiu; Leung, Wa-Hung; Dalton transactions (Cambridge, England : 2003) 50 (2021) 8512–8523; doi:10.1039/d1dt01269j

data_7707517
_publ_section_title
;
 Synthesis, structure and reactivity of iridium complexes containing a
 bis-cyclometalated tridentate C^N^C ligand.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8512
_journal_page_last               8523
_journal_paper_doi               10.1039/d1dt01269j
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C58 H63 Ir N2 O4 S'
_chemical_formula_sum            'C58 H63 Ir N2 O4 S'
_chemical_formula_weight         1076.36
_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     dual
_audit_creation_date             2021-03-03
_audit_creation_method
;
Olex2 1.3-beta
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-03-25 deposited with the CCDC.	2021-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                94.912(3)
_cell_angle_beta                 99.262(3)
_cell_angle_gamma                105.162(3)
_cell_formula_units_Z            2
_cell_length_a                   10.3452(4)
_cell_length_b                   15.7451(6)
_cell_length_c                   16.1341(6)
_cell_measurement_reflns_used    12477
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.8050
_cell_measurement_theta_min      3.7630
_cell_volume                     2480.87(17)
_computing_cell_refinement       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1788
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.956
_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     59.00 141.00   1.00    4.00    --  113.00 -45.00  90.00   82
  2  \w   -116.00 -14.00   1.00    2.00    --  -39.95 -37.00-120.00  102
  3  \w    -61.00  -6.00   1.00    2.00    --  -39.95 125.00  60.00   55
  4  \w    -83.00  -6.00   1.00    2.00    --  -39.95 125.00 -30.00   77
  5  \w   -116.00 -27.00   1.00    2.00    --  -39.95 -37.00 150.00   89
  6  \w     45.00  97.00   1.00    2.00    --   39.95-125.00-120.00   52
  7  \w    138.00 178.00   1.00    4.00    --  113.00  30.00 120.00   40
  8  \w     41.00 136.00   1.00    4.00    --  113.00 -61.00 -30.00   95
  9  \w     84.00 122.00   1.00    4.00    --  113.00  30.00 120.00   38
 10  \w     83.00 176.00   1.00    4.00    --  113.00  61.00 -90.00   93
 11  \w     67.00 109.00   1.00    4.00    --  113.00-111.00-150.00   42
 12  \w     35.00  61.00   1.00    4.00    --  113.00-111.00-150.00   26
 13  \w     39.00 109.00   1.00    4.00    --  113.00-111.00   0.00   70
 14  \w     62.00 171.00   1.00    4.00    --  113.00  15.00  60.00  109
 15  \w     47.00 109.00   1.00    4.00    --  113.00-111.00 150.00   62
 16  \w     50.00 143.00   1.00    4.00    --  113.00 -61.00-180.00   93
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0782764000
_diffrn_orient_matrix_UB_12      0.0097701000
_diffrn_orient_matrix_UB_13      0.0915783000
_diffrn_orient_matrix_UB_21      -0.0420511000
_diffrn_orient_matrix_UB_22      0.0848217000
_diffrn_orient_matrix_UB_23      0.0221885000
_diffrn_orient_matrix_UB_31      -0.1296426000
_diffrn_orient_matrix_UB_32      -0.0563400000
_diffrn_orient_matrix_UB_33      0.0255334000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16355
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.966
_diffrn_reflns_theta_min         2.934
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Cu
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    5.981
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71305
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.69a (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    1.441
_exptl_crystal_description       plate
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.898
_refine_diff_density_min         -1.136
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         10011
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+0.3907P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0638
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9437
_reflns_number_total             10011
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01269j2.cif
_cod_data_source_block           wai264cu_173k
_cod_depositor_comments
'Adding full bibliography for 7707513--7707520.cif.'
_cod_database_code               7707517
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Ir N2 C40 H38 O Cl2 S'
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.510
_reflns_odcompleteness_completeness 98.52
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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. Rigid body (RIGU) restrains
 C34, C37, C38, C39, C40
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C34, C37A, C38A, C39A, C40A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Fixed Sof: C37(0.64) C37A(0.36) C38(0.64) H38A(0.64) H38B(0.64) H38C(0.64)
 C38A(0.36) H38D(0.36) H38E(0.36) H38F(0.36) C39(0.64) H39A(0.64) H39B(0.64)
 H39C(0.64) C39A(0.36) H39D(0.36) H39E(0.36) H39F(0.36) C40(0.64) H40A(0.64)
 H40B(0.64) H40C(0.64) C40A(0.36) H40D(0.36) H40E(0.36) H40F(0.36)
4.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C23(H23), C25(H25), C26(H26), C32(H32),
 C33(H33), C35(H35), C36(H36), C42(H42), C43(H43), C44(H44), C53(H53), C55(H55),
  C56(H56), C62(H62), C63(H63), C65(H65), C66(H66), C72(H72), C73(H73),
 C75(H75), C76(H76)
4.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C38(H38A,H38B,
 H38C), C38A(H38D,H38E,H38F), C39(H39A,H39B,H39C), C39A(H39D,H39E,H39F),
 C40(H40A,H40B,H40C), C40A(H40D,H40E,H40F), C58(H58A,H58B,H58C), C59(H59A,H59B,
 H59C), C60(H60A,H60B,H60C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C70(H70A,
 H70B,H70C), C77(H77A,H77B,H77C)
;
_shelx_res_checksum              90092
_shelx_hkl_checksum              39561
_olex2_date_sample_data_collection 2021-02-26
_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 2.255
_oxdiff_exptl_absorpt_empirical_full_min 0.752