Stabilization of Iridium(IV) by Monoanionic Dialkyldiarylguanidinato Ligands
Jan-Uwe Rohde; Wei-Tsung Lee; Journal of the American Chemical Society 131 (2009) 9162–9163; doi:10.1021/ja9033445

data_4104653
_publ_section_title
;
 Stabilization of Iridium(IV) by Monoanionic Dialkyldiarylguanidinato
 Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9162
_journal_page_last               9163
_journal_paper_doi               10.1021/ja9033445
_journal_volume                  131
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_formula_iupac          '[Ir (C15 H16 N3)3] P F6'
_chemical_formula_moiety         'C45 H48 Ir N9 1+, F6 P 1-'
_chemical_formula_structural     '(Ir (C15 H16 N3)3) (P F6)'
_chemical_formula_sum            'C45 H48 F6 Ir N9 P'
_chemical_formula_weight         1052.09
_chemical_name_systematic
; 
tris(<i>N</i>,<i>N</i>-dimethyl-<i>N'</i>,<i>N''</i>-
diphenylguanidinato-\k^2^<i>N'</i>,<i>N''</i>)iridium(IV) hexafluorophosphate
;
_space_group_IT_number           197
_symmetry_cell_setting           cubic
_symmetry_Int_Tables_number      197
_symmetry_space_group_name_Hall  'I 2 2 3'
_symmetry_space_group_name_H-M   'I 2 3'
_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            8
_cell_length_a                   20.745(3)
_cell_length_b                   20.745(3)
_cell_length_c                   20.745(3)
_cell_measurement_reflns_used    20595
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      27.86
_cell_measurement_theta_min      3.11
_cell_volume                     8928(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 3.1 (Crystal Impact, 2008)'
_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  0.0865
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            39519
_diffrn_reflns_theta_full        27.86
_diffrn_reflns_theta_max         27.86
_diffrn_reflns_theta_min         3.11
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.095
_exptl_absorpt_correction_T_max  0.7370
_exptl_absorpt_correction_T_min  0.5299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL-2000 (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_description       prism
_exptl_crystal_F_000             4216
_exptl_crystal_recrystallization_method
;
dichloromethane, vapor diffusion of n-pentane
;
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.517
_refine_diff_density_min         -1.056
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3559
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          3.373
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+9.4168P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0674
_reflns_number_gt                3218
_reflns_number_total             3559
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja9033445_si_001.cif
_cod_data_source_block           roh92
_cod_database_code               4104653