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_4085217
_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 H30 Ir N5, C H2 Cl2'
_chemical_formula_sum            'C31 H32 Cl2 Ir N5'
_chemical_formula_weight         737.71
_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_am43
_audit_creation_date
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'Mon Jun 23 14:42:26 2014'
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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
'08.10.2014 16:14:32 CEST UTC+02:00  encif 1.23'
_cell_angle_alpha                90
_cell_angle_beta                 93.5666(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.73269(13)
_cell_length_b                   10.32253(12)
_cell_length_c                   23.9590(2)
_cell_measurement_reflns_used    28185
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      28.8910
_cell_measurement_theta_min      3.9290
_cell_volume                     2896.08(5)
_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
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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)'
_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 0.950
_diffrn_measurement_details
;
  1 omega   12.00   50.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -79.0000 -145.5848 76

  2 omega    7.00   85.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   57.0000 -120.0000 156

  3 omega  -21.00   49.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000   60.0000 140

  4 omega  -49.00   49.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000  -60.0000 196

  5 omega  -11.00   89.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   77.0000  -30.0000 200

  6 omega  -49.00   49.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000  120.0000 196

  7 omega   -9.00   78.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   77.0000   90.0000 174

  8 omega   -3.00   68.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   57.0000 -180.0000 142

  9 omega  -36.00   49.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000    0.0000 170

 10 omega  -40.00   -6.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000 -120.0000 68

 11 omega   23.00   49.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000 -120.0000 52

 12 omega  -40.00  -14.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000  150.0000 52

 13 omega   17.00   49.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000  150.0000 64

 14 omega   -3.00   30.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   57.0000  -30.0000 66

 15 omega   23.00   49.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000 -180.0000 52

 16 omega  -45.00  -19.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -79.0000 -145.5848 52

 17 omega  -50.00   40.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -57.0000  120.0000 180

 18 omega   -3.00   22.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   57.0000   60.0000 50

 19 omega   -7.00   91.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   38.0000 -180.0000 196

;
_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      -0.0129908000
_diffrn_orient_matrix_UB_12      -0.0637606000
_diffrn_orient_matrix_UB_13      -0.0094059000
_diffrn_orient_matrix_UB_21      0.0473569000
_diffrn_orient_matrix_UB_22      -0.0240366000
_diffrn_orient_matrix_UB_23      0.0167392000
_diffrn_orient_matrix_UB_31      -0.0354825000
_diffrn_orient_matrix_UB_32      -0.0087040000
_diffrn_orient_matrix_UB_33      0.0226134000
_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  0.0502
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            64322
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.963
_diffrn_reflns_theta_min         3.193
_diffrn_source                   'microfocus X-Ray tube'
_exptl_absorpt_coefficient_mu    4.825
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65859
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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    1.692
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.2862
_exptl_crystal_size_mid          0.1297
_exptl_crystal_size_min          0.0355
_refine_diff_density_max         1.396
_refine_diff_density_min         -1.306
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         7278
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0168P)^2^+4.8397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0571
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6767
_reflns_number_total             7278
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501138t_si_004.cif
_cod_data_source_block           ga_am43
_cod_depositor_comments
'Adding full bibliography for 4085217--4085232.cif.'
_cod_original_cell_volume        2896.08(6)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4085217
_audit_block_refno               2069
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C31 H32 Cl2 Ir1 N5'
_shelx_estimated_absorpt_t_max   0.644
_shelx_estimated_absorpt_t_min   0.644
_reflns_odcompleteness_completeness 99.71
_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. Restrained distances
 C31A-Cl1A \\sim C31A-Cl2 \\sim C31B-Cl1B \\sim C31B-Cl2
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1A \\sim Cl1B \\sim Cl2: within 1A with sigma of 0.04 and sigma for terminal
atoms of 0.04
4. Others
 Sof(C31B)=Sof(H31C)=Sof(H31D)=Sof(Cl1B)=1-FVAR(1)
 Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(Cl1A)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C31A(H31A,H31B), C31B(H31C,H31D)
5.b 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)
5.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)
;
_shelx_res_checksum              48596
_audit_block_usercomment         AM684_2
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            11.7307(2)
_cell_oxdiff_length_b            10.32544(17)
_cell_oxdiff_length_c            23.9570(4)
_cell_oxdiff_angle_alpha         90.0164(13)
_cell_oxdiff_angle_beta          93.5897(14)
_cell_oxdiff_angle_gamma         89.9831(14)
_cell_oxdiff_volume              2896.08(8)
_cell_oxdiff_measurement_reflns_used 28185