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_7707513
_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         'C41 H52 Cl3 Hg Ir2 N, C H2 Cl2'
_chemical_formula_sum            'C42 H54 Cl5 Hg Ir2 N'
_chemical_formula_weight         1335.10
_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     heavy
_audit_creation_date             2018-12-07
_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                70.906(4)
_cell_angle_beta                 79.811(3)
_cell_angle_gamma                88.663(3)
_cell_formula_units_Z            2
_cell_length_a                   11.4169(5)
_cell_length_b                   11.6904(5)
_cell_length_c                   16.8087(7)
_cell_measurement_reflns_used    7495
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.8160
_cell_measurement_theta_min      3.9230
_cell_volume                     2085.13(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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.980
_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     36.00 137.00   1.00    3.00    --  106.99 -61.00-150.00  101
  2  \w    -91.00  -2.00   1.00    2.00    --  -40.57 125.00 150.00   89
  3  \w    -67.00  33.00   1.00    2.00    --  -40.57  37.00 120.00  100
  4  \w   -117.00 -14.00   1.00    2.00    --  -40.57 -37.00 -60.00  103
  5  \w     36.00  99.00   1.00    3.00    --  106.99 -94.00-150.00   63
  6  \w     82.00 150.00   1.00    3.00    --  106.99  30.00 150.00   68
  7  \w     32.00 125.00   1.00    3.00    --  106.99 -30.00 -60.00   93
  8  \w     78.00 107.00   1.00    3.00    --  106.99-125.00   0.00   29
  9  \w     40.00  66.00   1.00    3.00    --  106.99-125.00   0.00   26
 10  \w     54.00 117.00   1.00    3.00    --  106.99-125.00  90.00   63
 11  \w     33.00 120.00   1.00    3.00    --  106.99 -61.00  60.00   87
 12  \w     26.00 166.00   1.00    3.00    --  106.99 -15.00 120.00  140
;
_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      -0.0961108000
_diffrn_orient_matrix_UB_12      -0.0317426000
_diffrn_orient_matrix_UB_13      0.0815099000
_diffrn_orient_matrix_UB_21      0.0749883000
_diffrn_orient_matrix_UB_22      0.0676958000
_diffrn_orient_matrix_UB_23      0.0394099000
_diffrn_orient_matrix_UB_31      -0.0629424000
_diffrn_orient_matrix_UB_32      0.1178283000
_diffrn_orient_matrix_UB_33      -0.0390103000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11532
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         67.498
_diffrn_reflns_theta_min         4.004
_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    21.753
_exptl_absorpt_correction_T_max  0.93985
_exptl_absorpt_correction_T_min  0.93985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
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    2.126
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.151
_refine_diff_density_min         -2.357
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         7357
_refine_ls_number_restraints     339
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0480P)^2^+12.3940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0876
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6915
_reflns_number_total             7357
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01269j2.cif
_cod_data_source_block           wai220cult
_cod_depositor_comments
'Adding full bibliography for 7707513--7707520.cif.'
_cod_original_cell_volume        2085.12(16)
_cod_database_code               7707513
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.561
_shelx_estimated_absorpt_t_min   0.220
_reflns_odcompleteness_completeness 98.60
_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
2. Restrained distances
 C18-C17 \\sim C20-C17 \\sim C19-C17
 with sigma of 0.02
 C18A-C17 \\sim C20A-C17 \\sim C19A-C17
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C7) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C10) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C2)
\\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C21) \\sim Ueq,
Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C16) \\sim Ueq,
Uanis(C15) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq:
with sigma of 0.003 and sigma for terminal atoms of 0.002
Uanis(N1) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.002
Uanis(C41) \\sim Ueq, Uanis(C45) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.002
Uanis(C42) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.002
Uanis(C34) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C31)
\\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C36) \\sim Ueq,
Uanis(C35) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.002
Uanis(Cl2) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.002
Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.001
4. Rigid body (RIGU) restrains
 C17, C18A, C19A, C20A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C17, C18, C19, C20
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Hg1, Ir1, Ir2, Cl1, N1, C1, C35, C36
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: C18(0.5) H18A(0.5) H18B(0.5) H18C(0.5) C18A(0.5) H18D(0.5)
 H18E(0.5) H18F(0.5) C19(0.5) H19A(0.5) H19B(0.5) H19C(0.5) C19A(0.5) H19D(0.5)
 H19E(0.5) H19F(0.5) C20(0.5) H20A(0.5) H20B(0.5) H20C(0.5) C20A(0.5) H20D(0.5)
 H20E(0.5) H20F(0.5)
6.a Ternary CH refined with riding coordinates:
 C31(H31), C32(H32), C35(H35), C36(H36), C41(H41), C42(H42), C45(H45), C46(H46)
6.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C34(H34A,H34B), C37(H37A,H37B), C38(H38A,H38B), C43(H43A,
 H43B), C44(H44A,H44B), C47(H47A,H47B), C48(H48A,H48B), C1S(H1SA,H1SB)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C11(H11), C13(H13), C14(H14), C16(H16), C22(H22),
 C23(H23), C24(H24)
6.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C18(H18A,H18B,H18C),
 C18A(H18D,H18E,H18F), C19(H19A,H19B,H19C), C19A(H19D,H19E,H19F), C20(H20A,H20B,
 H20C), C20A(H20D,H20E,H20F)
;
_shelx_res_checksum              58059
_shelx_hkl_checksum              24127
_olex2_date_sample_data_collection 2018-11-09
_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 1.564
_oxdiff_exptl_absorpt_empirical_full_min 0.756