Isolation and Structural Characterization of Anionic and Neutral Compounds Resulting from the Oxidative Addition of HI or CH~3~I to [IrI~2~(CO)~2~]^-^
Samuel Gautron; Robert Giordano; Carole Le Berre; Joël Jaud; Jean-Claude Daran; Philippe Serp; Philippe Kalck; Inorganic Chemistry 42 (2003) 5523–5530; doi:10.1021/ic0340938

data_4314145
_publ_contact_author             'Jean-Claude Daran'
_publ_contact_author_address
;
Laboratoire de Chimie de Coordination
UPR-CNRS 8241
205, route de Narbonne
31077 Toulouse cedex, France
;
_publ_contact_author_email       ' daran@lcc-toulouse.fr '
_publ_contact_author_fax         ' (33) 5 61 55 30 03 '
_publ_contact_author_phone       ' (33) 5 61 33 31 74 '
_publ_section_title
;
 Isolation and Structural Characterization of Anionic and Neutral
 Compounds Resulting from the Oxidative Addition of HI or CH~3~I to
 [IrI~2~(CO)~2~]^-^
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5523
_journal_page_last               5530
_journal_paper_doi               10.1021/ic0340938
_journal_volume                  42
_journal_year                    2003
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C3 H3 I2 Ir1 O2'
_chemical_formula_sum            'C3 H3 I2 Ir O2'
_chemical_formula_weight         517.05
_chemical_name_systematic
;
  ?
;
_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
_audit_creation_date             2003-01-27T13:58:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                102.94(2)
_cell_angle_beta                 110.72(3)
_cell_angle_gamma                90.52(2)
_cell_formula_units_Z            2
_cell_length_a                   6.6629(18)
_cell_length_b                   7.6766(19)
_cell_length_c                   8.710(2)
_cell_measurement_reflns_used    1936
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      4.07
_cell_measurement_wavelength     0.71073
_cell_volume                     404.2(2)
_computing_cell_refinement       'CRYSALIS 169 (Oxford-Diffraction, 2001)'
_computing_data_collection       'CRYSALIS 169 (Oxford-Diffraction, 2001)'
_computing_data_reduction        'CRYSALIS 169 (Oxford-Diffraction, 2001)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'Oxfod-Diffraction Xcalibur'
_diffrn_measurement_method       \w-\f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2468
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         4.07
_diffrn_standards_decay_%        0.01
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    24.078
_exptl_absorpt_correction_T_max  0.2578
_exptl_absorpt_correction_T_min  0.0726
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
         (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.057
_refine_diff_density_max         1.437
_refine_diff_density_min         -1.875
_refine_diff_density_rms         0.293
_refine_ls_extinction_coef       0.0042(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         1541
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+1.1163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.09
_reflns_number_gt                1365
_reflns_number_total             1541
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic0340938_1.cif
_cod_data_source_block           4
_cod_original_cell_volume        404.19(18)
_cod_original_formula_sum        'C3 H3 I2 Ir1 O2'
_cod_database_code               4314145