Synthesis, Characterization, and O2 Reactivity of Iridium(I) Complexes Supported by Guanidinato Ligands
Jan-Uwe Rohde; Matthew R. Kelley; Wei-Tsung Lee; Inorganic Chemistry 47 (2008) 11461–11463; doi:10.1021/ic801867r

data_4306827
_publ_section_title
;
Synthesis, Characterization, and O2 Reactivity of Iridium(I) Complexes
Supported by Guanidinato Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11461
_journal_page_last               11463
_journal_paper_doi               10.1021/ic801867r
_journal_volume                  47
_journal_year                    2008
_chemical_formula_iupac          '[Ir (C17 H20 N3) (C8 H12)]'
_chemical_formula_moiety         'C25 H32 Ir N3'
_chemical_formula_structural     '(Ir (C17 H20 N3) (C8 H12))'
_chemical_formula_sum            'C25 H32 Ir N3'
_chemical_formula_weight         566.74
_chemical_name_systematic
; 
(\h^4^-Cyclooctadiene)(<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           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.034(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2528(11)
_cell_length_b                   17.8077(19)
_cell_length_c                   12.6997(14)
_cell_measurement_reflns_used    10100
_cell_measurement_temperature    209(2)
_cell_measurement_theta_max      27.89
_cell_measurement_theta_min      3.03
_cell_volume                     2217.0(4)
_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      209(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  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19485
_diffrn_reflns_theta_full        27.89
_diffrn_reflns_theta_max         27.89
_diffrn_reflns_theta_min         3.03
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.038
_exptl_absorpt_correction_T_max  0.8637
_exptl_absorpt_correction_T_min  0.4267
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL-2000 (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             1120
_exptl_crystal_recrystallization_method 'n-pentane, -30 \%C'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.922
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         5287
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0164P)^2^+0.7902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0472
_refine_ls_wR_factor_ref         0.0505
_reflns_number_gt                4310
_reflns_number_total             5287
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic801867r_si_001.cif
_cod_data_source_block           roh87
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4306827