Si-H Activation in an Iridium Nitrido Complex-A Mechanistic and Theoretical Study
Daniel Sieh; Peter Burger; Journal of the American Chemical Society 135 (2013) 3971–3982; doi:10.1021/ja311905h

data_4119454
_publ_contact_author_address
;Institut fuer Anorganische und Angewandte Chemie
Universitaet Hamburg
Martin-Luther-King-Platz 6
D-20146 Hamburg 
;
_publ_contact_author_email       burger@chemie.uni-hamburg.de
_publ_contact_author_name        'Peter Burger'
_publ_section_title
;
 Si-H Activation in an Iridium Nitrido Complex-A Mechanistic and
 Theoretical Study
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3971
_journal_page_last               3982
_journal_paper_doi               10.1021/ja311905h
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C39 H57 Ir N4 Si'
_chemical_formula_sum            'C39 H57 Ir N4 Si'
_chemical_formula_weight         802.18
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 104.79
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1165(5)
_cell_length_b                   14.0913(5)
_cell_length_c                   18.6829(6)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.9
_cell_measurement_theta_min      2.26
_cell_volume                     3847.8(2)
_computing_cell_refinement       'SAINT (Bruker AXS, 2008)'
_computing_data_collection       'SMART (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT (Bruker AXS, 2008)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997-2005 Glasgow)'
_computing_publication_material  'SHELXTL (Bruker AXS, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Smart APEX CCD area detector'
_diffrn_measurement_method       omega-scan
_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  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            42511
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.83
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    3.532
_exptl_absorpt_correction_T_max  0.8488
_exptl_absorpt_correction_T_min  0.5385
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       plate
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.229
_refine_diff_density_min         -1.024
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         8787
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+8.8780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0937
_reflns_number_gt                6502
_reflns_number_total             8787
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja311905h_si_003.cif
_cod_data_source_block           25bwp21n
_cod_database_code               4119454