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_4086618
_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         'C23 H26 Ir N2, B F4, C H2 Cl2'
_chemical_formula_sum            'C24 H28 B Cl2 F4 Ir N2'
_chemical_formula_weight         694.39
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-11-18 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 119.400(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6676(5)
_cell_length_b                   12.8597(4)
_cell_length_c                   15.8707(4)
_cell_measurement_reflns_used    9963
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.00
_cell_measurement_theta_min      2.57
_cell_volume                     2608.02(15)
_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 0.998
_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  0.0250
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35077
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.022
_diffrn_reflns_theta_min         1.594
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    5.368
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6270
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_description       prism
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.739
_refine_diff_density_min         -1.436
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         9049
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0174P)^2^+6.0988P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0580
_refine_ls_wR_factor_ref         0.0627
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7606
_reflns_number_total             9049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00248_si_002.cif
_cod_data_source_block           2_BF4
_cod_original_cell_volume        2608.02(14)
_cod_database_code               4086618
_shelx_estimated_absorpt_t_min   0.296
_shelx_estimated_absorpt_t_max   0.413
_shelxl_version_number           2013-4
_shelx_res_checksum              30284
_shelx_hkl_checksum              2781