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_4085221
_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         'C30 H31 Ir N6'
_chemical_formula_sum            'C30 H31 Ir N6'
_chemical_formula_weight         667.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_am44a
_audit_creation_date
;
'Tue Jul 01 12:25:52 2014'
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Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_audit_update_record
'08.10.2014 16:57:10 CEST UTC+02:00  encif 1.23'
_cell_angle_alpha                90
_cell_angle_beta                 100.1809(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.77689(15)
_cell_length_b                   13.04053(19)
_cell_length_c                   23.0986(4)
_cell_measurement_reflns_used    27925
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      28.7060
_cell_measurement_theta_min      3.6010
_cell_volume                     2602.13(7)
_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
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
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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)'
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'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 0.997
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_details
;
  1 omega   -8.00   50.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -79.0000   30.4076 116

  2 omega    4.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000  -90.0000 90

  3 omega  -12.00   87.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   77.0000   90.0000 198

  4 omega   -1.00   84.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   57.0000    0.0000 170

  5 omega  -49.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000  150.0000 196

  6 omega   36.00   79.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   57.0000  -90.0000 86

  7 omega  -11.00   86.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   77.0000 -150.0000 194

  8 omega  -27.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000   90.0000 152

  9 omega   55.00   81.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   57.0000   30.0000 52

 10 omega  -44.00    1.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000  -30.0000 90

 11 omega   20.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000  -30.0000 58

 12 omega   18.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000 -180.0000 62

 13 omega   18.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000  -60.0000 62

 14 omega  -30.00   40.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.6161   57.0000 -120.0000 140

 15 omega   12.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.6161   77.0000  -30.0000 74

 16 omega  -12.00   89.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   77.0000 -120.0000 202

 17 omega  -50.00   40.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -57.0000  120.0000 180

 18 omega  -50.00   40.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -57.0000 -150.0000 180

 19 omega  -44.00  -12.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.6161   38.0000    0.0000 64

;
_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      -0.0537801000
_diffrn_orient_matrix_UB_12      0.0384267000
_diffrn_orient_matrix_UB_13      0.0045909000
_diffrn_orient_matrix_UB_21      -0.0180750000
_diffrn_orient_matrix_UB_22      0.0086899000
_diffrn_orient_matrix_UB_23      -0.0307633000
_diffrn_orient_matrix_UB_31      -0.0593288000
_diffrn_orient_matrix_UB_32      -0.0375156000
_diffrn_orient_matrix_UB_33      -0.0023909000
_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  0.0476
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            60836
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.956
_diffrn_reflns_theta_min         3.250
_diffrn_source                   'microfocus X-Ray tube'
_exptl_absorpt_coefficient_mu    5.162
_exptl_absorpt_correction_T_max  0.806
_exptl_absorpt_correction_T_min  0.435
_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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_description       plate
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.2179
_exptl_crystal_size_mid          0.1649
_exptl_crystal_size_min          0.0544
_refine_diff_density_max         3.671
_refine_diff_density_min         -1.866
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         6552
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.202
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0115P)^2^+12.2772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0664
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6086
_reflns_number_total             6552
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501138t_si_004.cif
_cod_data_source_block           ga_am44a
_cod_depositor_comments
'Adding full bibliography for 4085217--4085232.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4085221
_audit_block_refno               2085
_audit_block_usercomment         'AM179, plate, black'
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C33 H31 Ir N6'
_chemical_oxdiff_usercomment     'AM179, plate, black'
_shelx_estimated_absorpt_t_max   0.747
_shelx_estimated_absorpt_t_min   0.383
_reflns_odcompleteness_completeness 99.68
_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.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)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), 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              47205
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            8.77762(12)
_cell_oxdiff_length_b            13.03821(18)
_cell_oxdiff_length_c            23.0981(4)
_cell_oxdiff_angle_alpha         89.9533(12)
_cell_oxdiff_angle_beta          100.1432(12)
_cell_oxdiff_angle_gamma         90.0347(11)
_cell_oxdiff_volume              2602.13(6)
_cell_oxdiff_measurement_reflns_used 27925