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_7707515
_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         'C54 H43 Cl Ir P3, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C54.5 H44 Cl2 Ir P3'
_chemical_formula_weight         1054.90
_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             2019-02-28
_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                76.851(3)
_cell_angle_beta                 88.011(3)
_cell_angle_gamma                69.189(4)
_cell_formula_units_Z            2
_cell_length_a                   10.7955(5)
_cell_length_b                   12.1139(4)
_cell_length_c                   18.5808(6)
_cell_measurement_reflns_used    7939
_cell_measurement_temperature    118(20)
_cell_measurement_theta_max      73.3220
_cell_measurement_theta_min      3.9970
_cell_volume                     2208.99(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      118(20)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.942
_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     32.00 138.00   1.00    3.00    --  106.99 -30.00 150.00  106
  2  \w    -69.00  31.00   1.00    2.00    --  -40.57  57.00-120.00  100
  3  \w    -74.00  26.00   1.00    2.00    --  -40.57  77.00   0.00  100
  4  \w    -66.00  36.00   1.00    2.00    --  -40.57  37.00 150.00  102
  5  \w     29.00 138.00   1.00    3.00    --  106.99 -30.00   0.00  109
  6  \w     28.00 139.00   1.00    3.00    --  106.99 -77.00 150.00  111
  7  \w     73.00 154.00   1.00    3.00    --  106.99  77.00 -30.00   81
  8  \w     94.00 177.00   1.00    3.00    --  106.99 125.00 150.00   83
  9  \w     32.00 117.00   1.00    3.00    --  106.99-125.00   0.00   85
 10  \w     46.00 109.00   1.00    3.00    --  106.99 -94.00  90.00   63
;
_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      -0.1404361000
_diffrn_orient_matrix_UB_12      0.0034120000
_diffrn_orient_matrix_UB_13      -0.0162797000
_diffrn_orient_matrix_UB_21      -0.0235246000
_diffrn_orient_matrix_UB_22      -0.0221913000
_diffrn_orient_matrix_UB_23      0.0834642000
_diffrn_orient_matrix_UB_31      -0.0555924000
_diffrn_orient_matrix_UB_32      0.1379934000
_diffrn_orient_matrix_UB_33      -0.0060686000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12789
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.999
_diffrn_reflns_theta_min         4.012
_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    8.280
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64245
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_description       plate
_exptl_crystal_F_000             1054
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.413
_refine_diff_density_min         -1.434
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         8465
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0430P)^2^+1.9410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7901
_reflns_number_total             8465
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01269j2.cif
_cod_data_source_block           wai228cult
_cod_depositor_comments
'Adding full bibliography for 7707513--7707520.cif.'
_cod_original_cell_volume        2208.99(15)
_cod_original_formula_sum        'C54.50 H44 Cl2 Ir P3'
_cod_database_code               7707515
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.852
_shelx_estimated_absorpt_t_min   0.491
_reflns_odcompleteness_completeness 98.61
_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
2. Restrained distances
 Cl2S-C1S = Cl1S-C1S
 1.72 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Cl2S) \\sim Ueq, Uanis(Cl1S) \\sim Ueq, Uanis(C1S) \\sim Ueq: with sigma
of 0.003 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: Cl1S(0.5) Cl2S(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C12(H12), C13(H13), C14(H14), C15(H15),
 C16(H16), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C33(H33), C34(H34),
  C35(H35), C36(H36), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46),
 C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C62(H62), C63(H63), C64(H64),
  C65(H65), C66(H66), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76),
 C82(H82), C83(H83), C84(H84), C85(H85), C86(H86)
;
_shelx_res_checksum              89373
_shelx_hkl_checksum              68362
_olex2_date_sample_data_collection 2019-02-22
_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 1.434
_oxdiff_exptl_absorpt_empirical_full_min 0.787