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_4330324
_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 P2 N2 B F4 C42.21 H40.42 Cl2.42'
_chemical_formula_sum            'C42.21 H40.42 B Cl2.42 F4 Ir N2 P2'
_chemical_formula_weight         1002.50
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   19.2265(14)
_cell_length_b                   15.8767(12)
_cell_length_c                   15.0485(11)
_cell_measurement_reflns_used    38484
_cell_measurement_temperature    223
_cell_measurement_theta_max      27.18
_cell_measurement_theta_min      3.00
_cell_volume                     4593.6(6)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalClear
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0912
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            45610
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.171
_exptl_absorpt_correction_T_max  0.827
_exptl_absorpt_correction_T_min  0.593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       Chunk
_exptl_crystal_F_000             1987.28
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.530
_refine_diff_density_min         -1.590
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     295
_refine_ls_number_reflns         5240
_refine_ls_number_restraints     37
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0444P)^2^+12.4423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1174
_reflns_number_gt                4373
_reflns_number_total             5433
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic300923c_si_002_5.cif
_cod_data_source_block           (3-PPh3)
_cod_original_formula_sum        'Ir P2 N2 B F4 C42.21 H40.42 Cl2.42'
_cod_database_code               4330324