Stable iridium(iv) complexes supported by tetradentate salen ligands. Synthesis, structures and reactivity
Lee, Chi Lun; Wu, Liangliang; Huang, Jie-Sheng; Che, Chi-Ming; Chemical Communications  (2019) –; doi:10.1039/C8CC10220A

data_7123096
_publ_section_title
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 Stable iridium(iv) complexes supported by tetradentate salen ligands.
 Synthesis, structures and reactivity
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC10220A
_journal_year                    2019
_chemical_formula_moiety         'C50 H54 Cl2 Ir N2 O2, 2.41(C H Cl3)'
_chemical_formula_sum            'C52.41 H56.41 Cl9.23 Ir N2 O2'
_chemical_formula_weight         1265.58
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-05-10
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2018-12-08 deposited with the CCDC.    2019-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.226(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.7754(14)
_cell_length_b                   14.4960(8)
_cell_length_c                   16.5663(9)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    100
_cell_measurement_theta_max      66.64
_cell_measurement_theta_min      3.54
_cell_volume                     5888.5(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0983
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.946
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            83040
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.241
_diffrn_reflns_theta_min         1.802
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.537
_exptl_absorpt_correction_T_max  0.77
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       needle
_exptl_crystal_F_000             2539
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.168
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         10085
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.094
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+47.8853P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1274
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9487
_reflns_number_total             10085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc10220a2.cif
_cod_data_source_block           cxy88_p-1
_cod_database_code               7123096
_shelxl_version_number           2013-4
_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. Restrained distances
 Cl10-C53 = Cl11-C53 = Cl9-C53
 1.76 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C53) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(Cl10)=Sof(Cl9)=Sof(Cl11)=Sof(C53)=Sof(H53)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C52(H52), C51(H51), C53(H53)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C25(H25), C30(H30), C28(H28), C32(H32), C22(H22), C21(H21),
 C26(H26), C5(H5), C3(H3), C10(H10), C14(H14), C13(H13), C23(H23), C12(H12),
 C15(H15), C20(H20)
5.c Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C49(H49A,H49B,
 H49C), C45(H45A,H45B,H45C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C37(H37A,
 H37B,H37C), C38(H38A,H38B,H38C), C50(H50A,H50B,H50C), C36(H36A,H36B,H36C),
 C48(H48A,H48B,H48C)
;
_shelx_res_checksum              63149