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_4085231
_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, 3.5(C H2 Cl2), C24 H20 B'
_chemical_formula_sum            'C63.5 H70 B Cl7 Ir N5'
_chemical_formula_weight         1354.40
_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   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_am14
_audit_creation_date             2014-10-14
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_audit_update_record
'14.10.2014 11:46:23 CEST UTC+02:00  encif 1.24'
_cell_angle_alpha                105.595(7)
_cell_angle_beta                 104.010(12)
_cell_angle_gamma                101.462(12)
_cell_formula_units_Z            2
_cell_length_a                   12.856(5)
_cell_length_b                   15.116(6)
_cell_length_c                   17.523(8)
_cell_measurement_reflns_used    7592
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.10
_cell_measurement_theta_min      2.23
_cell_volume                     3053(2)
_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 V8.27B (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 0.929
_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  0.0312
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            78336
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.547
_diffrn_reflns_theta_min         1.583
_diffrn_source                   'sealed X-Ray tube (Mo)'
_diffrn_source_type              'fine focus tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.537
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6142
_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    1.473
_exptl_crystal_description       block
_exptl_crystal_F_000             1374
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.035
_refine_diff_density_min         -2.197
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         20598
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+4.8840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0779
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18999
_reflns_number_total             20598
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501138t_si_003.cif
_cod_data_source_block           ga_am14
_cod_depositor_comments
'Adding full bibliography for 4085217--4085232.cif.'
_cod_original_formula_sum        'C63.50 H70 B Cl7 Ir N5'
_cod_database_code               4085231
_audit_block_refno               1718
_audit_block_usercomment         AM345_3
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.687
_shelx_estimated_absorpt_t_min   0.537
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C73-Cl76 \\sim C73-Cl77
 with sigma of 0.02
 C74-Cl78 \\sim C74-Cl78_$1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl76 \\sim Cl77: within 0.8A with sigma of 0.02 and sigma for terminal atoms of
0.02
4. Same fragment restrains
{Cl71, Cl72, C71}
as
{Cl75, Cl76, C73}
{Cl71, Cl72, C71}
as
{Cl73, Cl74, C72}
5. Others
 Sof(H73C)=Sof(H73D)=Sof(Cl77)=1-FVAR(1)
 Sof(Cl76)=Sof(H73A)=Sof(H73B)=FVAR(1)
 Fixed Sof: C74(0.5) H74A(0.5) H74B(0.5)
6.a Riding coordinates:
 C74(H74A,H74B)
6.b Secondary CH2 refined with riding coordinates:
 C71(H71A,H71B), C73(H73A,H73B), C73(H73C,H73D), C72(H72A,H72B)
6.c 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), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C48(H48),
  C49(H49), C50(H50), C51(H51), C52(H52), C54(H54), C55(H55), C56(H56),
 C57(H57), C58(H58), C60(H60), C62(H62), C63(H63), C64(H64), C61(H61)
6.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), 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              25807
_olex2_submission_special_instructions 'No special instructions were received'