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_4334020
_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 (C17 H20 N3) (C O)2]'
_chemical_formula_moiety         'C19 H20 Ir N3 O2'
_chemical_formula_structural     '(Ir (C17 H20 N3) (C O)2)'
_chemical_formula_sum            'C19 H20 Ir N3 O2'
_chemical_formula_weight         514.58
_chemical_name_systematic
; 
Dicarbonyl(<i>N</i>,<i>N</i>-diethyl-<i>N'</i>,<i>N''</i>-
diphenylguanidinato-\k^2^<i>N'</i>,<i>N''</i>)iridium(I)
;
_chemical_properties_physical    air-sensitive
_space_group_IT_number           118
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      118
_symmetry_space_group_name_Hall  'P -4 -2n'
_symmetry_space_group_name_H-M   'P -4 n 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.3359(18)
_cell_length_b                   17.3359(18)
_cell_length_c                   6.1770(7)
_cell_measurement_reflns_used    8035
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      3.32
_cell_volume                     1856.4(3)
_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      190(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0175
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            11591
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         3.32
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.209
_exptl_absorpt_correction_T_max  0.5963
_exptl_absorpt_correction_T_min  0.1812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL-2000 (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.841
_exptl_crystal_description       rod
_exptl_crystal_F_000             992
_exptl_crystal_recrystallization_method
;
n-pentane, -30 deg C
;
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.281
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.156
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.08(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         2215
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0275
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0275P)^2^+12.4333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0873
_reflns_number_gt                2052
_reflns_number_total             2215
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic302570s_si_002_1.cif
_cod_data_source_block           roh103
_cod_database_code               4334020