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_4086621
_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         'C42 H47 Ir2 N2, C F3 O3 S, 2(C H2 Cl2)'
_chemical_formula_sum            'C45 H51 Cl4 F3 Ir2 N2 O3 S'
_chemical_formula_weight         1283.14
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 120.899(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9779(9)
_cell_length_b                   23.2754(19)
_cell_length_c                   21.0040(13)
_cell_measurement_reflns_used    9180
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      34.03
_cell_measurement_theta_min      2.26
_cell_volume                     4605.1(6)
_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 0.997
_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  0.0333
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            74913
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.048
_diffrn_reflns_theta_min         1.429
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    6.105
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.6242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.851
_exptl_crystal_description       prism
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.300
_refine_diff_density_max         3.404
_refine_diff_density_min         -2.827
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         18826
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0210P)^2^+18.0829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0831
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15330
_reflns_number_total             18826
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00248_si_002.cif
_cod_data_source_block           5_OTf
_cod_database_code               4086621
_shelx_estimated_absorpt_t_min   0.194
_shelx_estimated_absorpt_t_max   0.262
_shelxl_version_number           2013-4
_shelx_res_checksum              7280
_shelx_hkl_checksum              88405