Mild, Reversible Reaction of Iridium(III) Amido Complexes with Carbon Dioxide
Graham E. Dobereiner; Jianguo Wu; Michael G. Manas; Nathan D. Schley; Michael K. Takase; Robert H. Crabtree; Nilay Hazari; Feliu Maseras; Ainara Nova; Inorganic Chemistry 51 (2012) 9683–9693; doi:10.1021/ic300923c

data_4330326
_publ_contact_author_email       robert.crabtree@yale.edu
_publ_contact_author_fax         '+203 432 6144'
_publ_contact_author_name        'Dr. Robert H Crabtree'
_publ_contact_author_phone       '+203 432 3925'
_publ_section_title
;
 Mild, Reversible Reaction of Iridium(III) Amido Complexes with Carbon
 Dioxide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9683
_journal_page_last               9693
_journal_paper_doi               10.1021/ic300923c
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'Ir C45.50 H44 N2 O2 P2 Cl5'
_chemical_formula_sum            'C45.5 H44 Cl5 Ir N2 O2 P2'
_chemical_formula_weight         1082.29
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                66.345(20)
_cell_angle_beta                 71.92(2)
_cell_angle_gamma                78.945(19)
_cell_formula_units_Z            2
_cell_length_a                   13.269(9)
_cell_length_b                   13.481(8)
_cell_length_c                   14.591(11)
_cell_measurement_reflns_used    4158
_cell_measurement_temperature    223
_cell_measurement_theta_max      27.79
_cell_measurement_theta_min      3.15
_cell_volume                     2266(3)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r12'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r12 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r12'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      223
_diffrn_detector_area_resol_mean 6.849
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  SCX-MINI
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21588
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.359
_exptl_absorpt_correction_T_max  0.715
_exptl_absorpt_correction_T_min  0.285
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1078.00
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.520
_refine_diff_density_min         -0.860
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     539
_refine_ls_number_reflns         9893
_refine_ls_number_restraints     32
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0380P)^2^+4.9516P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1150
_reflns_number_gt                8089
_reflns_number_total             9893
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic300923c_si_002_7.cif
_cod_data_source_block           (11-PPh3)
_cod_original_formula_sum        'Ir C45.50 H44 N2 O2 P2 Cl5'
_cod_database_code               4330326