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_7707516
_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         'C51 H55 Ir N2 O, C6 H14'
_chemical_formula_sum            'C57 H69 Ir N2 O'
_chemical_formula_weight         990.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-02-26
_audit_creation_method
;
Olex2 1.3-beta
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-03-25 deposited with the CCDC.	2021-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.5650(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.19411(12)
_cell_length_b                   13.27153(11)
_cell_length_c                   26.6663(2)
_cell_measurement_reflns_used    21289
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.2980
_cell_measurement_theta_min      3.1040
_cell_volume                     5018.30(7)
_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 1.3-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3-beta (Bourhis et al., 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 0.998
_diffrn_measured_fraction_theta_max 0.978
_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     67.00 146.00   1.00    5.00    --  112.00 178.00  60.00   79
  2  \w    -69.00  32.00   1.00    2.00    --  -41.01  57.00 120.00  101
  3  \w   -108.00 -74.00   1.00    2.00    --  -41.01-149.00  73.00   34
  4  \w   -112.00 -17.00   1.00    2.00    --  -41.01 -37.00-120.00   95
  5  \w   -115.00 -27.00   1.00    2.00    --  -41.01 -37.00 -30.00   88
  6  \w     43.00  96.00   1.00    2.00    --   41.01-123.00-123.00   53
  7  \w    111.00 137.00   1.00    5.00    --  112.00 111.00  30.00   26
  8  \w     92.00 176.00   1.00    5.00    --  112.00  45.00-150.00   84
  9  \w    104.00 178.00   1.00    5.00    --  112.00  77.00 150.00   74
 10  \w     40.00 132.00   1.00    5.00    --  112.00 -30.00  30.00   92
 11  \w     39.00 109.00   1.00    5.00    --  112.00-111.00-120.00   70
 12  \w    149.00 178.00   1.00    5.00    --  112.00 111.00  30.00   29
 13  \w     36.00 109.00   1.00    5.00    --  112.00-111.00  30.00   73
 14  \w     36.00 144.00   1.00    5.00    --  112.00 -77.00  60.00  108
 15  \w     41.00 134.00   1.00    5.00    --  112.00 -30.00-180.00   93
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1071899000
_diffrn_orient_matrix_UB_12      -0.0165246000
_diffrn_orient_matrix_UB_13      0.0073190000
_diffrn_orient_matrix_UB_21      0.0074801000
_diffrn_orient_matrix_UB_22      -0.0120099000
_diffrn_orient_matrix_UB_23      -0.0571566000
_diffrn_orient_matrix_UB_31      0.0161823000
_diffrn_orient_matrix_UB_32      0.1142207000
_diffrn_orient_matrix_UB_33      -0.0050192000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            31708
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.402
_diffrn_reflns_theta_min         4.451
_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    5.438
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61842
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       plate
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         10304
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0210
_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^)+(0.0234P)^2^+3.5793P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0514
_refine_ls_wR_factor_ref         0.0530
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9572
_reflns_number_total             10304
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01269j2.cif
_cod_data_source_block           wai263a_173k
_cod_depositor_comments
'Adding full bibliography for 7707513--7707520.cif.'
_cod_database_code               7707516
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Ir P4 Cl4 O4 C80 H78 '
_reflns_odcompleteness_completeness 99.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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
 C5SA-C6SA = C4SA-C5SA = C3SA-C4SA = C2SA-C3SA = C1SA-C2SA
 1.52 with sigma of 0.02
 C5S-C6S = C4S-C5S = C3S-C4S = C2S-C3S = C1S-C2S
 1.52 with sigma of 0.02
 C5S-C3S
 2.45 with sigma of 0.04
 C3S-C1S
 2.45 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C4S) \\sim Ueq, Uanis(C3S) \\sim Ueq, Uanis(C4SA) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 C1S, C2S, C3S, C4S, C5S, C6S
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1SA, C2SA, C3SA, C4SA, C5SA, C6SA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: C1S(0.5) H1SA(0.5) H1SB(0.5) H1SC(0.5) C2S(0.5) H2SA(0.5)
 H2SB(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5) C4S(0.5) H4SA(0.5) H4SB(0.5) C5S(0.5)
 H5SA(0.5) H5SB(0.5) C6S(0.5) H6SA(0.5) H6SB(0.5) H6SC(0.5) C1SA(0.5) H1SD(0.5)
 H1SE(0.5) H1SF(0.5) C2SA(0.5) H2SC(0.5) H2SD(0.5) C3SA(0.5) H3SC(0.5)
 H3SD(0.5) C4SA(0.5) H4SC(0.5) H4SD(0.5) C5SA(0.5) H5SC(0.5) H5SD(0.5)
 C6SA(0.5) H6SD(0.5) H6SE(0.5) H6SF(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C2S(H2SA,H2SB), C3S(H3SA,H3SB), C4S(H4SA,H4SB), C5S(H5SA,H5SB), C2SA(H2SC,
 H2SD), C3SA(H3SC,H3SD), C4SA(H4SC,H4SD), C5SA(H5SC,H5SD)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C13(H13), C15(H15), C16(H16), C23(H23), C25(H25),
 C26(H26), C32(H32), C33(H33), C34(H34), C43(H43), C45(H45), C46(H46), C52(H52),
  C53(H53), C55(H55), C56(H56)
6.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C48(H48A,H48B,H48C), C49(H49A,
 H49B,H49C), C50(H50A,H50B,H50C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C),
 C60(H60A,H60B,H60C), C1S(H1SA,H1SB,H1SC), C6S(H6SA,H6SB,H6SC), C1SA(H1SD,H1SE,
 H1SF), C6SA(H6SD,H6SE,H6SF)
;
_shelx_res_checksum              37762
_shelx_hkl_checksum              74574
_olex2_date_sample_data_collection 2021-02-24
_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 1.524
_oxdiff_exptl_absorpt_empirical_full_min 0.776