Guanidinato Complexes of Iridium: Ligand-Donor Strength, O2 Reactivity, and (Alkene)peroxoiridium(III) Intermediates
Matthew R. Kelley; Jan-Uwe Rohde; Inorganic Chemistry 52 (2013) 2564–2580; doi:10.1021/ic302570s

data_4334021
_publ_contact_author_name        'Jan-Uwe Rohde'
_publ_section_title
;
 Guanidinato Complexes of Iridium: Ligand-Donor Strength, O2 Reactivity,
 and (Alkene)peroxoiridium(III) Intermediates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2564
_journal_page_last               2580
_journal_paper_doi               10.1021/ic302570s
_journal_volume                  52
_journal_year                    2013
_chemical_formula_iupac          '[Ir (C19 H24 N3) (C8 H12)]'
_chemical_formula_moiety         'C27 H36 Ir N3'
_chemical_formula_structural     '(Ir (C19 H24 N3) (C8 H12))'
_chemical_formula_sum            'C27 H36 Ir N3'
_chemical_formula_weight         594.79
_chemical_name_systematic
; 
(\h^4^-Cyclooctadiene)(<i>N</i>,<i>N</i>-diethyl-<i>N'</i>,<i>N''</i>-
bis(4-methylphenyl)guanidinato-\k^2^<i>N'</i>,<i>N''</i>)iridium(I)
;
_chemical_properties_physical    air-sensitive
_space_group_IT_number           2
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.444(5)
_cell_angle_beta                 89.343(5)
_cell_angle_gamma                74.719(5)
_cell_formula_units_Z            2
_cell_length_a                   9.5336(11)
_cell_length_b                   9.6634(11)
_cell_length_c                   13.6109(15)
_cell_measurement_reflns_used    5525
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      3.00
_cell_volume                     1208.4(2)
_computing_cell_refinement       'HKL-2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'HKL-2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Diamond 3.2 (Crystal Impact, 1997-2012)'
_computing_publication_material  'SHELXTL v6.1 (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXTL v6.1 (Bruker AXS, 2001)'
_computing_structure_solution    'SHELXTL v6.1 (Bruker AXS, 2001)'
_diffrn_ambient_temperature      210(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       'area detector, \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed x-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0166
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10816
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         3.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.543
_exptl_absorpt_correction_T_max  0.4708
_exptl_absorpt_correction_T_min  0.3160
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL-2000 (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_description       prism
_exptl_crystal_F_000             592
_exptl_crystal_recrystallization_method
;
n-pentane, -30 deg C
;
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.108
_refine_diff_density_min         -1.175
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         5740
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0225
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+0.5741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0516
_refine_ls_wR_factor_ref         0.0531
_reflns_number_gt                5298
_reflns_number_total             5740
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic302570s_si_002_2.cif
_cod_data_source_block           roh811
_cod_database_code               4334021