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_4085230
_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 H43 Ir N5, C F3 O3 S, 3(C3 D3)'
_chemical_formula_sum            'C46 H43 D9 F3 Ir N5 O3 S'
_chemical_formula_weight         1013.24
_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_am11
_audit_creation_date             2014-10-15
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_audit_update_record
'15.10.2014 14:14:23 CEST UTC+02:00  encif 1.24'
_cell_angle_alpha                74.956(12)
_cell_angle_beta                 77.965(11)
_cell_angle_gamma                77.858(10)
_cell_formula_units_Z            2
_cell_length_a                   8.950(3)
_cell_length_b                   15.477(6)
_cell_length_c                   16.608(6)
_cell_measurement_reflns_used    8019
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.24
_cell_measurement_theta_min      2.57
_cell_volume                     2142.9(14)
_computing_cell_refinement
;
SAINT (see _computing_data_reduction). Includes estimated systematic errors
 of the unit cell constants from Monte Carlo simulations.
;
_computing_data_collection       'SMART-5.631 (Bruker AXS, 2003)'
_computing_data_reduction
'SAINT V8.18C (Bruker AXS, 1997-2013), SADABS-2012_1 (Sheldrick and Bruker AXS, 1997-2014)'
_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      'perfluoro polyether oil'
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.19
_diffrn_detector_type            CCD-PXL-KAF2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker AXS Smart 1000'
_diffrn_measurement_method       '\f- and \w-scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            54341
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.384
_diffrn_reflns_theta_min         1.287
_diffrn_source                   'sealed X-Ray tube (Mo)'
_diffrn_source_type              'fine focus tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.224
_exptl_absorpt_correction_T_max  0.6352
_exptl_absorpt_correction_T_min  0.5143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements (Blessing 1995)
SADABS (see _computing_data_reduction)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       block
_exptl_crystal_F_000             1014
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.954
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         14334
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0215
_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^)+(0.0227P)^2^+2.3241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0514
_refine_ls_wR_factor_ref         0.0580
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13237
_reflns_number_total             14334
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501138t_si_003.cif
_cod_data_source_block           ga_am11
_cod_depositor_comments
'Adding full bibliography for 4085217--4085232.cif.'
_cod_original_cell_volume        2143.0(14)
_cod_database_code               4085230
_audit_block_refno               1664
_audit_block_usercomment         AMFM17_3
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.739
_shelx_estimated_absorpt_t_min   0.524
_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
 C19-C20A \\sim C19-C21A \\sim C19-C22A \\sim C19-C20B \\sim C19-C21B \\sim
C19-C22B
 with sigma of 0.01
 C20A-C21A \\sim C20A-C22A \\sim C21A-C22A \\sim C20B-C21B \\sim C20B-C22B
\\sim C21B-C22B
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C20A \\sim C21A \\sim C22A \\sim C20B \\sim C21B \\sim C22B: within 1A with
sigma of 0.02 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C19, C20A, C21A, C22A, C20B, C21B, C22B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C21A)=Sof(H21D)=Sof(H21E)=
 Sof(H21F)=Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(1)
 Sof(C20B)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21B)=Sof(H21A)=Sof(H21B)=
 Sof(H21C)=Sof(C22B)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(1)
6.a Me refined with riding coordinates:
 C20B(H20A,H20B,H20C), C21B(H21A,H21B,H21C), C22B(H22A,H22B,H22C), C20A(H20D,
 H20E,H20F), C21A(H21D,H21E,H21F), C22A(H22D,H22E,H22F)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13), C15(H15),
 C17(H17), C18(H18), C81(D81), C82(D82), C83(D83), C91(D91), C92(D92), C93(D93),
  C94(D94), C95(D95), C96(D96)
6.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), 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              49708
_olex2_submission_special_instructions 'No special instructions were received'