Diastereoselective Oxidative Addition of Dihydrogen to IrI(CO)((R)-BINAP) and [Ir(CO)2((R)-BINAP)][SbF6]
Abdurrahman Ç. Atesin; Simon B. Duckett; Christine Flaschenriem; William W. Brennessel; Richard Eisenberg; Inorganic Chemistry 46 (2007) 1196–1204; doi:10.1021/ic061471a

data_4306990
_publ_section_title
;
Diastereoselective Oxidative Addition of Dihydrogen to IrI(CO)((R)-BINAP)
and [Ir(CO)2((R)-BINAP)][SbF6]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1196
_journal_page_last               1204
_journal_paper_doi               10.1021/ic061471a
_journal_volume                  46
_journal_year                    2007
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C45 H32 I Ir O P2'
_chemical_formula_sum            'C45 H32 I Ir O P2'
_chemical_formula_weight         969.75
_chemical_name_common            eisaa03
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_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            4
_cell_length_a                   12.0023(10)
_cell_length_b                   12.0023(10)
_cell_length_c                   26.132(4)
_cell_measurement_reflns_used    3221
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      26.92
_cell_measurement_theta_min      2.40
_cell_volume                     3764.5(7)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'APEX2, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       'area detector, \w scans per \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            59810
_diffrn_reflns_theta_full        30.99
_diffrn_reflns_theta_max         30.99
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    4.486
_exptl_absorpt_correction_T_max  0.8409
_exptl_absorpt_correction_T_min  0.3523
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
'Flack H D (1983), 2449 Friedel pairs, Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.004(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         5921
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0146P)^2^+5.4380P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0689
_reflns_number_gt                3969
_reflns_number_total             5921
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061471asi20060804_105049_2.cif
_cod_data_source_block           eisaa03
_cod_original_cell_volume        3764.4(7)
_cod_database_code               4306990