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_7707519
_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 Hg Ir N, 1.375(C H2 Cl2), 0.375(C6 H14) '
_chemical_formula_sum            'C36.625 H47 Cl3.75 Hg Ir N'
_chemical_formula_weight         1026.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2020-05-05
_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                90
_cell_angle_beta                 104.7030(11)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.7337(2)
_cell_length_b                   11.72515(11)
_cell_length_c                   29.5201(3)
_cell_measurement_reflns_used    18524
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.8310
_cell_measurement_theta_min      4.0710
_cell_volume                     7276.30(13)
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3577
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     34.00 116.00   1.00    5.00    --  106.99-125.00 120.00   82
  2  \w   -113.00 -21.00   1.00    2.00    --  -40.57 -57.00-120.00   92
  3  \w    -68.00  26.00   1.00    2.00    --  -40.57  57.00  30.00   94
  4  \w    -67.00  28.00   1.00    2.00    --  -40.57  37.00-180.00   95
  5  \w     27.00  82.00   1.00    2.00    --   40.57 -99.00-180.00   55
  6  \w     79.00 178.00   1.00    5.00    --  106.99  61.00-120.00   99
  7  \w     94.00 178.00   1.00    5.00    --  106.99 125.00 120.00   84
  8  \w     79.00 177.00   1.00    5.00    --  106.99  77.00-180.00   98
  9  \w     73.00 162.00   1.00    5.00    --  106.99  77.00 -60.00   89
 10  \w     32.00 117.00   1.00    5.00    --  106.99-125.00 -30.00   85
 11  \w     34.00 133.00   1.00    5.00    --  106.99 -77.00 120.00   99
;
_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      -0.0317534000
_diffrn_orient_matrix_UB_12      0.0472091000
_diffrn_orient_matrix_UB_13      0.0372379000
_diffrn_orient_matrix_UB_21      -0.0660142000
_diffrn_orient_matrix_UB_22      -0.0236023000
_diffrn_orient_matrix_UB_23      -0.0328846000
_diffrn_orient_matrix_UB_31      0.0005201000
_diffrn_orient_matrix_UB_32      -0.1203273000
_diffrn_orient_matrix_UB_33      0.0210563000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            39147
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         67.500
_diffrn_reflns_theta_min         4.076
_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    17.162
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31086
_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    1.875
_exptl_crystal_description       needle
_exptl_crystal_F_000             3956
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.774
_refine_diff_density_min         -1.567
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     814
_refine_ls_number_reflns         13080
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0315P)^2^+40.2256P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0830
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11326
_reflns_number_total             13080
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01269j2.cif
_cod_data_source_block           wai221cult
_cod_depositor_comments
'Adding full bibliography for 7707513--7707520.cif.'
_cod_database_code               7707519
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.725
_shelx_estimated_absorpt_t_min   0.148
_reflns_odcompleteness_completeness 99.82
_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
 Cl12-C1S = Cl11-C1S
 1.72 with sigma of 0.02
 Cl13-C2S
 1.72 with sigma of 0.02
 Cl14-C2S
 1.72 with sigma of 0.02
 Cl15-C3S = Cl17-C4S = Cl18-C4S = Cl16-C3S
 1.72 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C2S) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
Uanis(C4S) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
4. Rigid body (RIGU) restrains
 Cl13, Cl14, C2S
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
 Cl15, Cl16, C3S
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
 Cl19, Cl20, C5S
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
 Cl17, Cl18, C4S
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: Cl15(0.6) Cl16(0.6) C3S(0.6) H3SA(0.6) H3SB(0.6) Cl13(0.2)
 Cl14(0.2) C2S(0.2) H2SA(0.2) H2SB(0.2) Cl17(0.4) Cl18(0.4) C4S(0.4) H4SA(0.4)
 H4SB(0.4) Cl11(0.8) Cl12(0.8) C1S(0.8) H1SA(0.8) H1SB(0.8) Cl19(0.75)
 Cl20(0.75) C5S(0.75) H5SA(0.75) H5SB(0.75)
6.a Ternary CH refined with riding coordinates:
 C31(H31), C32(H32), C35(H35), C36(H36), C31A(H31A), C32A(H32A), C35A(H35A),
 C36A(H36A)
6.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C34(H34A,H34B), C37(H37A,H37B), C38(H38A,H38B), C33A(H33C,
 H33D), C34A(H34C,H34D), C37A(H37C,H37D), C38A(H38C,H38D), C3S(H3SA,H3SB),
 C2S(H2SA,H2SB), C4S(H4SA,H4SB), C1S(H1SA,H1SB), C5S(H5SA,H5SB)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C13(H13), C14(H14), C16(H16), C22(H22), C23(H23),
 C24(H24), C3A(H3A), C4A(H4A), C6A(H6A), C13A(H13A), C14A(H14A), C16A(H16A),
 C22A(H22A), C23A(H23A), C24A(H24A)
6.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,
 H9AC), C10A(H10D,H10E,H10F), C18A(H18D,H18E,H18F), C19A(H19D,H19E,H19F),
 C20A(H20D,H20E,H20F)
;
_smtbx_masks_special_details
;
162 electrons from 4 voids which account for about 3 molecules 
of hexane in a unit cell, or 0.375 molecule of hexane per 
asymmetric unit with Z equals to 8.  
;
_shelx_res_checksum              23528
_shelx_hkl_checksum              47196
_shelx_fab_checksum              42957
_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 2.635
_oxdiff_exptl_absorpt_empirical_full_min 0.636