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_7707518
_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         'C33 H39 Cl Ir N, C H4 O'
_chemical_formula_sum            'C34 H43 Cl Ir N O'
_chemical_formula_weight         709.34
_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             2019-02-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2021-03-25 deposited with the CCDC.	2021-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                118.782(5)
_cell_angle_beta                 105.993(4)
_cell_angle_gamma                100.339(3)
_cell_formula_units_Z            2
_cell_length_a                   12.0649(4)
_cell_length_b                   12.2041(5)
_cell_length_c                   12.5489(6)
_cell_measurement_reflns_used    6037
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.8290
_cell_measurement_theta_min      4.1430
_cell_volume                     1446.00(16)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.984
_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     76.00 178.00   1.00    4.00    --  106.99  30.00 -60.00  102
  2  \w   -117.00 -15.00   1.00    2.00    --  -40.57 -37.00 120.00  102
  3  \w    -74.00  26.00   1.00    2.00    --  -40.57  77.00  30.00  100
  4  \w    -62.00  26.00   1.00    2.00    --  -40.57  37.00 -60.00   88
  5  \w    117.00 178.00   1.00    4.00    --  106.99  61.00-150.00   61
  6  \w     33.00 117.00   1.00    4.00    --  106.99-125.00-120.00   84
  7  \w    108.00 141.00   1.00    4.00    --  106.99 -77.00  30.00   33
  8  \w     28.00 104.00   1.00    4.00    --  106.99 -77.00  30.00   76
  9  \w     90.00 175.00   1.00    4.00    --  106.99  45.00   0.00   85
 10  \w     35.00 115.00   1.00    4.00    --  106.99-125.00  60.00   80
 11  \w    109.00 152.00   1.00    4.00    --  106.99 125.00-120.00   43
 12  \w     33.00 135.00   1.00    4.00    --  106.99 -61.00-150.00  102
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0936435000
_diffrn_orient_matrix_UB_12      0.0733634000
_diffrn_orient_matrix_UB_13      -0.0284800000
_diffrn_orient_matrix_UB_21      -0.0562072000
_diffrn_orient_matrix_UB_22      0.1097246000
_diffrn_orient_matrix_UB_23      0.0314374000
_diffrn_orient_matrix_UB_31      0.0923174000
_diffrn_orient_matrix_UB_32      0.0813741000
_diffrn_orient_matrix_UB_33      0.1483786000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8101
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         67.500
_diffrn_reflns_theta_min         4.104
_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    9.986
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.629
_exptl_crystal_description       plate
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.341
_refine_diff_density_min         -1.156
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         5132
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0207
_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^)+(0.0340P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0521
_refine_ls_wR_factor_ref         0.0526
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4939
_reflns_number_total             5132
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01269j2.cif
_cod_data_source_block           wai226cult
_cod_depositor_comments
'Adding full bibliography for 7707513--7707520.cif.'
_cod_original_cell_volume        1445.99(12)
_cod_database_code               7707518
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 98.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C7(H7A,H7B), C8(H8A,H8B)
2.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C23(H23), C24(H24), C26(H26), C33(H33),
 C34(H34), C36(H36)
2.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C2S(H2SA,H2SB,H2SC)
2.e Idealised tetrahedral OH refined as rotating group:
 O1S(H1S)
;
_shelx_res_checksum              10193
_shelx_hkl_checksum              226
_olex2_date_sample_data_collection 2019-02-13
_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 1.391
_oxdiff_exptl_absorpt_empirical_full_min 0.761