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_4085232
_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         'C33 H36 Ir N6, C24 H20 B'
_chemical_formula_sum            'C57 H56 B Ir N6'
_chemical_formula_weight         1028.08
_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_am42
_audit_creation_date
;
'Mon Jun 23 15:39:06 2014'
;
_audit_update_record             'Mon Jun 23 15:48:59 CEST 2014'
_cell_angle_alpha                70.497(4)
_cell_angle_beta                 82.773(3)
_cell_angle_gamma                68.559(4)
_cell_formula_units_Z            2
_cell_length_a                   11.9752(4)
_cell_length_b                   13.4730(7)
_cell_length_c                   16.3477(5)
_cell_measurement_reflns_used    20510
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      28.2580
_cell_measurement_theta_min      3.8600
_cell_volume                     2314.15(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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      120(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 0.901
_diffrn_measurement_details
;
  1 omega  -30.00   50.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -79.0000   47.9152 160

  2 omega   -3.00   87.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   57.0000 -150.0000 180

  3 omega   24.00   50.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -79.0000   71.2779 52

  4 omega   -9.00   83.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   77.0000  -60.0000 184

  5 omega    2.00   49.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000  120.0000 94

  6 omega  -33.00   49.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000 -120.0000 164

  7 omega  -44.00   49.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000  -60.0000 186

  8 omega   -8.00   89.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   77.0000   60.0000 194

  9 omega  -49.00  -24.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000 -180.0000 50

 10 omega   21.00   49.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000 -180.0000 56

 11 omega  -52.00  -13.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000  120.0000 78

 12 omega  -54.00  -28.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.6161  -61.0000 -150.0000 52

 13 omega    6.00   32.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.6161   77.0000  -30.0000 52

 14 omega  -49.00  -10.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.6161   77.0000  -30.0000 78

 15 omega  -39.00    2.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.6161  -57.0000   60.0000 82

 16 omega  -13.00   51.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.6161   38.0000 -150.0000 128

 17 omega   -7.00   35.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   38.0000  150.0000 84

 18 omega   -3.00   87.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   57.0000   30.0000 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      0.0204943000
_diffrn_orient_matrix_UB_12      0.0449729000
_diffrn_orient_matrix_UB_13      -0.0053179000
_diffrn_orient_matrix_UB_21      -0.0409982000
_diffrn_orient_matrix_UB_22      0.0163042000
_diffrn_orient_matrix_UB_23      0.0323912000
_diffrn_orient_matrix_UB_31      0.0441426000
_diffrn_orient_matrix_UB_32      -0.0354266000
_diffrn_orient_matrix_UB_33      0.0322690000
_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  0.0574
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            46926
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.015
_diffrn_reflns_theta_min         3.208
_diffrn_source                   'microfocus X-Ray tube'
_exptl_absorpt_coefficient_mu    2.931
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_correction_T_min  0.730
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.1406
_exptl_crystal_size_mid          0.0934
_exptl_crystal_size_min          0.0709
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.971
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     594
_refine_ls_number_reflns         11110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0157P)^2^+1.4903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0610
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10321
_reflns_number_total             11110
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501138t_si_003.cif
_cod_data_source_block           ga_am42
_cod_depositor_comments
'Adding full bibliography for 4085217--4085232.cif.'
_cod_original_cell_volume        2314.15(17)
_cod_database_code               4085232
_audit_block_refno               2064
_audit_block_usercomment         'AM686_2, irregular, red'
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C57 H56 B1 Ir1 N6'
_chemical_oxdiff_usercomment     'AM686_2, irregular, red'
_shelx_estimated_absorpt_t_max   0.758
_shelx_estimated_absorpt_t_min   0.758
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12), C15(H15),
 C16(H16), C17(H17), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C58(H58),
  C59(H59), C60(H60), C61(H61), C62(H62), C64(H64), C65(H65), C66(H66),
 C67(H67), C68(H68), C70(H70), C71(H71), C72(H72), C73(H73), C74(H74)
2.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C33(H33A,
 H33B,H33C)
;
_shelx_res_checksum              85262
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            11.9752(4)
_cell_oxdiff_length_b            13.4730(6)
_cell_oxdiff_length_c            16.3477(5)
_cell_oxdiff_angle_alpha         70.497(3)
_cell_oxdiff_angle_beta          82.773(3)
_cell_oxdiff_angle_gamma         68.559(4)
_cell_oxdiff_volume              2314.15(15)
_cell_oxdiff_measurement_reflns_used 20510