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_4085226
_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         'C36 H39 Cl Ir N5, C H2 Cl2'
_chemical_formula_sum            'C37 H41 Cl3 Ir N5'
_chemical_formula_weight         854.30
_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
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'Fri Jun 21 18:17:50 2013'
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Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
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_audit_update_record
'15.10.2014 14:20:59 CEST UTC+02:00  encif 1.24'
_cell_angle_alpha                80.6647(10)
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_cell_formula_units_Z            2
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_cell_measurement_reflns_used    21315
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      27.4720
_cell_measurement_theta_min      3.7250
_cell_volume                     1717.78(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_diffrn_ambient_temperature      110(1)
_diffrn_detector                 'CCD plate'
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_diffrn_measurement_details
;
  1 omega  -50.00  -10.00   0.5000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -16.8347   79.0000  -96.2910 80

  2 omega  -13.00   88.00   0.5000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       16.8347   77.0000  -60.0000 202

  3 omega  -52.00   36.00   0.5000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       16.8347  -57.0000  -90.0000 176

  4 omega   21.00   65.00   0.5000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       16.8347   57.0000 -120.0000 88

  5 omega  -29.00   44.00   0.5000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       16.8347  -77.0000    0.0000 146

  6 omega  -54.00   48.00   0.5000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       16.8347  -77.0000   90.0000 204

  7 omega    5.00   86.00   0.5000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       16.8347   57.0000   60.0000 162

  8 omega  -11.00   88.00   0.5000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       16.8347   77.0000  150.0000 198

  9 omega   23.00   48.00   0.5000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       16.8347  -77.0000   30.0000 50

 10 omega  -46.00   50.00   0.5000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       16.8347  -80.0000 -172.8454 192

 11 omega   -5.00   86.00   0.5000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       16.8347   57.0000 -180.0000 182

 12 omega  -52.00   38.00   0.5000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       16.8347  -57.0000   30.0000 180

 13 omega   -5.00   86.00   0.5000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       16.8347   57.0000   90.0000 182

 14 omega  -52.00   38.00   0.5000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       16.8347  -57.0000  -60.0000 180

 15 omega  -54.00   48.00   0.5000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       16.8347  -77.0000   90.0000 204

 16 omega  -52.00   38.00   0.5000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       16.8347  -57.0000  150.0000 180

;
_diffrn_measurement_device       '\k-geometry 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      -0.0018796000
_diffrn_orient_matrix_UB_12      -0.0730323000
_diffrn_orient_matrix_UB_13      0.0149409000
_diffrn_orient_matrix_UB_21      0.0762746000
_diffrn_orient_matrix_UB_22      -0.0247307000
_diffrn_orient_matrix_UB_23      -0.0165167000
_diffrn_orient_matrix_UB_31      0.0414970000
_diffrn_orient_matrix_UB_32      0.0153669000
_diffrn_orient_matrix_UB_33      0.0223103000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            40982
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.670
_diffrn_reflns_theta_min         3.233
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.155
_exptl_absorpt_correction_T_max  0.703
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_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_description       irregular
_exptl_crystal_F_000             852
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_exptl_crystal_size_mid          0.1274
_exptl_crystal_size_min          0.1137
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         7378
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0248
_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^)+(0.0208P)^2^+0.5593P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0487
_refine_ls_wR_factor_ref         0.0503
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6800
_reflns_number_total             7378
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501138t_si_003.cif
_cod_data_source_block           ga_am17
_cod_depositor_comments
'Adding full bibliography for 4085217--4085232.cif.'
_cod_database_code               4085226
_audit_block_refno               1786
_audit_block_usercomment         'AM400_3, irregular, orange'
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C37 H41 Cl3 Ir1 N5'
_chemical_oxdiff_usercomment     'AM400_3, irregular, orange'
_shelx_estimated_absorpt_t_max   0.681
_shelx_estimated_absorpt_t_min   0.681
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_reflns_odcompleteness_theta     24.97
_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:
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C23(H23A,H23B), C24(H24A,
 H24B), C25(H25A,H25B), C51(H51A,H51B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C19(H19)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C26(H26A,H26B,H26C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              81789
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            8.38257(11)
_cell_oxdiff_length_b            9.26625(12)
_cell_oxdiff_length_c            23.0041(3)
_cell_oxdiff_angle_alpha         80.6647(10)
_cell_oxdiff_angle_beta          80.9008(10)
_cell_oxdiff_angle_gamma         79.3838(11)
_cell_oxdiff_volume              1717.78(4)
_cell_oxdiff_measurement_reflns_used 21315