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_7123099
_publ_section_title
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 Stable iridium(iv) complexes supported by tetradentate salen ligands.
 Synthesis, structures and reactivity
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC10220A
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C36 H52 Cl2 Ir N2 O2, 2(C H2 Cl2)'
_chemical_formula_sum            'C38 H56 Cl6 Ir N2 O2'
_chemical_formula_weight         977.74
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-17
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.02.24 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2018-12-08 deposited with the CCDC.    2019-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                81.8890(10)
_cell_angle_beta                 73.0200(10)
_cell_angle_gamma                65.1680(10)
_cell_formula_units_Z            2
_cell_length_a                   12.6783(7)
_cell_length_b                   12.9154(7)
_cell_length_c                   14.6274(8)
_cell_measurement_reflns_used    9839
_cell_measurement_temperature    100
_cell_measurement_theta_max      67.50
_cell_measurement_theta_min      3.98
_cell_volume                     2078.5(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            37568
_diffrn_reflns_point_group_measured_fraction_full 0.872
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        67.640
_diffrn_reflns_theta_max         67.640
_diffrn_reflns_theta_min         3.160
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.031
_exptl_absorpt_correction_T_max  0.5207
_exptl_absorpt_correction_T_min  0.3098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1010 before and 0.0683 after correction.
The Ratio of minimum to maximum transmission is 0.5950.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_description       plate
_exptl_crystal_F_000             986
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.372
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details
;
 Flack x determined using 5582 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.035(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     907
_refine_ls_number_reflns         13132
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0608P)^2^+1.4244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0904
_reflns_Friedel_coverage         0.779
_reflns_Friedel_fraction_full    0.764
_reflns_Friedel_fraction_max     0.764
_reflns_number_gt                12986
_reflns_number_total             13132
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc10220a2.cif
_cod_data_source_block           cxy418_0m
_cod_database_code               7123099
_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.a Ternary CH refined with riding coordinates:
 C8(H8), C13(H13), C44(H44), C49(H49)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C45(H45A,H45B),
 C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C75(H75A,H75B), C74(H74A,H74B),
  C73(H73A,H73B), C76(H76A,H76B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C14(H14), C16(H16), C18(H18), C39(H39), C41(H41),
 C43(H43), C50(H50), C52(H52), C54(H54)
2.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C),
 C36(H36A,H36B,H36C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,
 H60C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C66(H66A,
 H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C70(H70A,H70B,H70C),
 C71(H71A,H71B,H71C), C72(H72A,H72B,H72C)
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_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'