Iridium Half-Sandwich Complexes with Di- and Tridentate Bis(pyridylimino)isoindolato Ligands: Stoichiometric and Catalytic Reactivity
Müller, Astrid L.; Bleith, Tim; Roth, Torsten; Wadepohl, Hubert; Gade, Lutz H.; Organometallics 34 (2015) 2326–; doi:10.1021/om501138t

data_4085219
_publ_section_title
;
 Iridium Half-Sandwich Complexes with Di- and Tridentate
 Bis(pyridylimino)isoindolato Ligands: Stoichiometric and Catalytic
 Reactivity
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2326
_journal_paper_doi               10.1021/om501138t
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C48 H46 Ir N5 P, F6 P, 2.5(C6 D6)'
_chemical_formula_sum            'C63 H46 D15 F6 Ir N5 P2'
_chemical_formula_weight         1271.40
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_am34
_audit_creation_date
;
'Fri Apr 11 12:00:41 2014'
;
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_audit_update_record
'08.10.2014 16:36:38 CEST UTC+02:00  encif 1.23'
_cell_angle_alpha                78.011(3)
_cell_angle_beta                 84.049(4)
_cell_angle_gamma                79.146(3)
_cell_formula_units_Z            2
_cell_length_a                   12.1901(5)
_cell_length_b                   13.7161(4)
_cell_length_c                   17.3715(8)
_cell_measurement_reflns_used    12968
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      25.9020
_cell_measurement_theta_min      3.5960
_cell_volume                     2784.03(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-14); encifer 1.4 (CCDC, 2011)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_details
;
  1 omega  -25.00    2.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.7723   57.0000  -30.0000 54

  2 omega  -81.00  -54.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.7723  -38.0000  -90.0000 54

  3 omega   16.00   43.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.7723   57.0000  -60.0000 54

  4 omega  -49.00   50.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.9286  -78.0000  120.3981 198

  5 omega   -1.00   79.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.9286   57.0000  -90.0000 160

  6 omega  -10.00   89.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.9286   77.0000   30.0000 198

  7 omega  -11.00   89.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.9286   77.0000  150.0000 200

  8 omega  -44.00   49.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.9286  -77.0000   30.0000 186

  9 omega   -1.00   54.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.9286   57.0000    0.0000 110

 10 omega   20.00   50.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.9286  -79.0000  -44.0318 60

 11 omega   23.00   49.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.9286  -77.0000 -150.0000 52

 12 omega   23.00   49.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.9286  -77.0000   60.0000 52

 13 omega  -49.00   50.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.9286  -78.0000  179.2265 198

 14 omega  -46.00   51.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.9286  -80.0000  -85.1327 194

 15 omega   -2.00   88.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.9286   57.0000 -180.0000 180

 16 omega  -50.00  -25.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.9286  -57.0000   30.0000 50

 17 omega  -50.00   40.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.9286  -57.0000 -150.0000 180

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_UB_11      -0.0101133000
_diffrn_orient_matrix_UB_12      -0.0211660000
_diffrn_orient_matrix_UB_13      0.0404091000
_diffrn_orient_matrix_UB_21      -0.0508597000
_diffrn_orient_matrix_UB_22      -0.0122263000
_diffrn_orient_matrix_UB_23      -0.0085434000
_diffrn_orient_matrix_UB_31      0.0289322000
_diffrn_orient_matrix_UB_32      -0.0477698000
_diffrn_orient_matrix_UB_33      -0.0066635000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0775
_diffrn_reflns_av_unetI/netI     0.0720
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            60776
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.074
_diffrn_reflns_theta_min         3.217
_diffrn_source                   'microfocus X-Ray tube'
_exptl_absorpt_coefficient_mu    2.521
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
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    1.517
_exptl_crystal_description       needle
_exptl_crystal_F_000             1270
_exptl_crystal_size_max          0.2934
_exptl_crystal_size_mid          0.0702
_exptl_crystal_size_min          0.0321
_refine_diff_density_max         2.833
_refine_diff_density_min         -1.218
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         13683
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0411P)^2^+5.2139P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1054
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11902
_reflns_number_total             13683
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501138t_si_004.cif
_cod_data_source_block           ga_am34
_cod_depositor_comments
'Adding full bibliography for 4085217--4085232.cif.'
_cod_original_cell_volume        2784.0(2)
_cod_database_code               4085219
_audit_block_refno               2012
_audit_block_usercomment         'AM678_1, needle, yellow'
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C63 H46 D15 F6 Ir1 N5 P2'
_chemical_oxdiff_usercomment     'AM678_1, needle, yellow'
_shelx_estimated_absorpt_t_max   0.787
_shelx_estimated_absorpt_t_min   0.787
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 P2-F1 \\sim P2-F2 \\sim P2-F3 \\sim P2-F6 \\sim P2-F5 \\sim P2-F4
 with sigma of 0.01
 F1-F2 \\sim F1-F3 \\sim F1-F4 \\sim F1-F5 \\sim F2-F3 \\sim F2-F5 \\sim F2-F6
\\sim F3-F4 \\sim F3-F6 \\sim F4-F5
 \\sim F4-F6 \\sim F5-F6
 with sigma of 0.02
 C71-C72 \\sim C72-C73 \\sim C71-C73_$1 \\sim C73-C71_$1
 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12), C16(H16),
 C17(H17), C18(H18), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38),
  C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46),
 C47(H47), C48(H48), C61(D61), C62(D62), C63(D63), C64(D64), C65(D65), C66(D66),
  C51(D51), C52(D52), C53(D53), C54(D54), C55(D55), C56(D56), C71(D71),
 C72(D72), C73(D73)
3.b Idealised Me refined as rotating group:
 C1A(H1AA,H1AB,H1AC), C20(H20A,H20B,H20C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              55856
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            12.1901(5)
_cell_oxdiff_length_b            13.7161(4)
_cell_oxdiff_length_c            17.3715(8)
_cell_oxdiff_angle_alpha         78.011(3)
_cell_oxdiff_angle_beta          84.049(4)
_cell_oxdiff_angle_gamma         79.146(3)
_cell_oxdiff_volume              2784.03(19)
_cell_oxdiff_measurement_reflns_used 12968