Evidence of a Donor‒Acceptor (Ir‒H)→SiR3Interaction in a Trapped Ir(III) Silane Catalytic Intermediate
Hamdaoui, Mustapha; Ney, Marjolaine; Sarda, Vivien; Karmazin, Lydia; Bailly, Corinne; Sieffert, Nicolas; Dohm, Sebastian; Hansen, Andreas; Grimme, Stefan; Djukic, Jean-Pierre; Organometallics 35 (2016) 2207–; doi:10.1021/acs.organomet.6b00248

data_4086620
_publ_section_title
;
 Evidence of a Donor--Acceptor (Ir--H)\\rightarrow SiR3Interaction in a
 Trapped Ir(III) Silane Catalytic Intermediate
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              2207
_journal_paper_doi               10.1021/acs.organomet.6b00248
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C32 H12 B F24, C27 H39 Ir N Si, 0.5(C6 H14)'
_chemical_formula_sum            'C62 H58 B F24 Ir N Si'
_chemical_formula_weight         1504.19
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                81.064(5)
_cell_angle_beta                 71.685(5)
_cell_angle_gamma                79.438(5)
_cell_formula_units_Z            2
_cell_length_a                   12.614(5)
_cell_length_b                   13.698(5)
_cell_length_c                   19.789(5)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.86
_cell_measurement_theta_min      2.52
_cell_volume                     3173.5(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            83067
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.052
_diffrn_reflns_theta_min         1.521
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    2.232
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_description       block
_exptl_crystal_F_000             1498
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_platon_squeeze_details
;
 The residual electron density was assigned to two molecules of water
 [38/2 = 19 e per asymmetric unit; two molecules of H2O would give 20e].
;
_refine_diff_density_max         1.693
_refine_diff_density_min         -1.291
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     820
_refine_ls_number_reflns         22017
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+2.3317P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0767
_refine_ls_wR_factor_ref         0.0791
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19600
_reflns_number_total             22017
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00248_si_002.cif
_cod_data_source_block           3_BARF24_pentane
_cod_database_code               4086620
_shelxl_version_number           2013-4
_shelx_res_checksum              92171
_shelx_hkl_checksum              61988