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_7707520
_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'
_chemical_formula_sum            'C51 H55 Ir N2 O'
_chemical_formula_weight         904.17
_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     dual
_audit_creation_date             2020-12-11
_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                 91.5588(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.78531(10)
_cell_length_b                   12.98197(13)
_cell_length_c                   28.0763(2)
_cell_measurement_reflns_used    10445
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      72.5940
_cell_measurement_theta_min      3.1360
_cell_volume                     4293.99(6)
_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 0.989
_diffrn_measured_fraction_theta_max 0.958
_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     31.00 133.00   1.00    8.00    --  103.43 -61.00  60.00  102
  2  \w   -114.00 -13.00   1.00    3.00    --  -41.26 -57.00 120.00  101
  3  \w    -87.00  -6.00   1.00    3.00    --  -41.26 125.00-180.00   81
  4  \w    103.00 178.00   1.00    8.00    --  103.43  77.00  60.00   75
  5  \w     21.00 106.00   1.00    8.00    --  103.43 -94.00   0.00   85
  6  \w     32.00 106.00   1.00    8.00    --  103.43 -94.00 -60.00   74
  7  \w     84.00 172.00   1.00    8.00    --  103.43  45.00-150.00   88
;
_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      -0.0007570000
_diffrn_orient_matrix_UB_12      0.1181856000
_diffrn_orient_matrix_UB_13      -0.0051112000
_diffrn_orient_matrix_UB_21      0.1304413000
_diffrn_orient_matrix_UB_22      0.0001379000
_diffrn_orient_matrix_UB_23      -0.0025132000
_diffrn_orient_matrix_UB_31      -0.0095846000
_diffrn_orient_matrix_UB_32      -0.0109339000
_diffrn_orient_matrix_UB_33      -0.0545660000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            16314
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.648
_diffrn_reflns_theta_min         3.149
_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    6.304
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85957
_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    1.399
_exptl_crystal_description       plate
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.756
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     538
_refine_ls_number_reflns         8191
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0233
_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^)+(0.0251P)^2^+1.5028P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0565
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7466
_reflns_number_total             8191
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01269j2.cif
_cod_data_source_block           wai262_173k
_cod_depositor_comments
'Adding full bibliography for 7707513--7707520.cif.'
_cod_original_cell_volume        4293.99(7)
_cod_database_code               7707520
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.884
_shelx_estimated_absorpt_t_min   0.632
_diffrn_oxdiff_digest_frames
;
0121fab847af4456d270f0a1743d0c45fa00027f6ba
;
_diffrn_oxdiff_digest_hkl
;
01f0de7549158e26fda870a19b216c87886f07
;
_reflns_odcompleteness_completeness 98.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 C40, C47, C48, C49
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C40, C47A, C48A, C49A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Fixed Sof: C47(0.815) H47A(0.815) H47B(0.815) H47C(0.815) C48(0.815)
 H48A(0.815) H48B(0.815) H48C(0.815) C49(0.815) H49A(0.815) H49B(0.815)
 H49C(0.815) C47A(0.185) H47D(0.185) H47E(0.185) H47F(0.185) C48A(0.185)
 H48D(0.185) H48E(0.185) H48F(0.185) C49A(0.185) H49D(0.185) H49E(0.185)
 H49F(0.185)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C12(H12), C13(H13), C15(H15), C16(H16), C23(H23),
 C25(H25), C26(H26), C33(H33), C34(H34), C35(H35), C43(H43), C45(H45), C46(H46),
  C53(H53), C55(H55), C56(H56)
4.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C), C49(H49A,H49B,H49C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C),
 C59(H59A,H59B,H59C), C47A(H47D,H47E,H47F), C48A(H48D,H48E,H48F), C49A(H49D,
 H49E,H49F)
;
_shelx_res_checksum              2887
_shelx_hkl_checksum              90226
_olex2_date_sample_data_collection 2020-11-23
_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 1.233
_oxdiff_exptl_absorpt_empirical_full_min 0.858