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_7707514
_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 H51 Cl2 Hg Ir2 N'
_chemical_formula_sum            'C41 H51 Cl2 Hg Ir2 N'
_chemical_formula_weight         1213.71
_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             2020-04-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-03-25 deposited with the CCDC.	2021-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                69.278(4)
_cell_angle_beta                 72.867(4)
_cell_angle_gamma                83.902(3)
_cell_formula_units_Z            2
_cell_length_a                   10.6104(4)
_cell_length_b                   12.0252(5)
_cell_length_c                   16.6227(8)
_cell_measurement_reflns_used    8127
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      71.8560
_cell_measurement_theta_min      2.9450
_cell_volume                     1895.68(15)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_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 0.982
_diffrn_measured_fraction_theta_max 0.947
_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     27.00 126.00   1.00    3.00    --  105.39 -61.00 150.00   99
  2  \w   -130.00  53.00   1.00    2.00    --  -37.73   0.00-120.00  183
  3  \w     27.00  82.00   1.00    2.00    --   37.73-125.00-180.00   55
  4  \w     27.00  61.00   1.00    2.00    --   37.73-125.00  90.00   34
  5  \w     28.00  88.00   1.00    2.00    --   37.73-125.00 -30.00   60
  6  \w    103.00 175.00   1.00    3.00    --  105.39  77.00 150.00   72
  7  \w     34.00 109.00   1.00    3.00    --  105.39-111.00 -30.00   75
  8  \w     20.00 107.00   1.00    3.00    --  105.39 -94.00 120.00   87
  9  \w    105.00 178.00   1.00    3.00    --  105.39 111.00 120.00   73
 10  \w     79.00 172.00   1.00    3.00    --  105.39  45.00 -60.00   93
 11  \w     69.00 175.00   1.00    3.00    --  105.39  30.00-120.00  106
 12  \w     33.00 113.00   1.00    3.00    --  105.39-133.00 106.00   80
;
_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      -0.1073631000
_diffrn_orient_matrix_UB_12      -0.0770709000
_diffrn_orient_matrix_UB_13      0.0794866000
_diffrn_orient_matrix_UB_21      -0.0619586000
_diffrn_orient_matrix_UB_22      -0.0229382000
_diffrn_orient_matrix_UB_23      -0.0656486000
_diffrn_orient_matrix_UB_31      0.0878578000
_diffrn_orient_matrix_UB_32      -0.1108847000
_diffrn_orient_matrix_UB_33      0.0015646000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10545
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.932
_diffrn_reflns_theta_min         2.957
_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    21.942
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53422
_exptl_absorpt_correction_type   multi-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    2.126
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.325
_refine_diff_density_min         -1.804
_refine_diff_density_rms         0.138
_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     523
_refine_ls_number_reflns         7056
_refine_ls_number_restraints     128
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0245
_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^)+(0.0340P)^2^+3.0616P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0637
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6636
_reflns_number_total             7056
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01269j2.cif
_cod_data_source_block           wai252_173k
_cod_depositor_comments
'Adding full bibliography for 7707513--7707520.cif.'
_cod_original_cell_volume        1895.69(15)
_cod_database_code               7707514
_shelx_shelxl_version_number     2014/7
_diffrn_oxdiff_digest_frames
;
01f351406aaf6dcd27e3e81f9eacf003ed000289fdb
;
_diffrn_oxdiff_digest_hkl
;
01197a37759465d848e20c79bff56b7e86f885
;
_reflns_odcompleteness_completeness 98.43
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C43-C42 = C43-C44 = C45-C44
 1.52 with sigma of 0.02
 Ir2-Cl2A \\sim Ir2-Cl2
 with sigma of 0.02
 C18-C21 \\sim C18-C19 \\sim C18-C20
 with sigma of 0.02
 C20A-C18A \\sim C19A-C18A \\sim C21A-C18A
 with sigma of 0.02
 C18-C3 \\sim C3-C18A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C21A) \\sim Ueq, Uanis(C19A) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.01
Uanis(C18A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.003
Uanis(C18) \\sim Ueq, Uanis(C20A) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 C41, C42, C43, C44, C45, C46, C47, C48
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C41, C42A, C43A, C44A, C45A, C46A, C47, C48
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: Cl2(0.5) Cl2A(0.5) C18(0.65) C18A(0.35) C19(0.65) H19A(0.65)
 H19B(0.65) H19C(0.65) C19A(0.35) H19D(0.35) H19E(0.35) H19F(0.35) C20(0.65)
 H20A(0.65) H20B(0.65) H20C(0.65) C20A(0.35) H20D(0.35) H20E(0.35) H20F(0.35)
 C21(0.65) H21A(0.65) H21B(0.65) H21C(0.65) C21A(0.35) H21D(0.35) H21E(0.35)
 H21F(0.35) H41(0.5) H41A(0.5) C42(0.5) H42(0.5) C42A(0.5) H42A(0.5) C43(0.5)
 H43A(0.5) H43B(0.5) C43A(0.5) H43C(0.5) H43D(0.5) C44(0.5) H44A(0.5) H44B(0.5)
 C44A(0.5) H44C(0.5) H44D(0.5) C45(0.5) H45(0.5) C45A(0.5) H45A(0.5) C46(0.5)
 H46(0.5) C46A(0.5) H46A(0.5) H47A(0.5) H47B(0.5) H47C(0.5) H47D(0.5)
6.a Ternary CH refined with riding coordinates:
 C31(H31), C32(H32), C35(H35), C36(H36), C41(H41), C41(H41A), C42(H42),
 C42A(H42A), C45(H45), C45A(H45A), C46(H46), C46A(H46A)
6.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C34(H34A,H34B), C37(H37A,H37B), C38(H38A,H38B), C43(H43A,
 H43B), C43A(H43C,H43D), C44(H44A,H44B), C44A(H44C,H44D), C47(H47A,H47B),
 C47(H47C,H47D), C48(H48A,H48B)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14), C16(H16)
6.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C19A(H19D,H19E,H19F), C20(H20A,H20B,H20C), C20A(H20D,
 H20E,H20F), C21(H21A,H21B,H21C), C21A(H21D,H21E,H21F), C23(H23A,H23B,H23C),
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              89705
_shelx_hkl_checksum              14446
_olex2_date_sample_data_collection 2020-04-16
_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 1.384
_oxdiff_exptl_absorpt_empirical_full_min 0.752