Synthesis and Structure of PNP-Supported Iridium Silyl and Silylene Complexes: Catalytic Hydrosilation of Alkenes
Elisa Calimano; T. Don Tilley; Journal of the American Chemical Society 131 (2009) 11161–11173; doi:10.1021/ja903737j

data_4104822
_publ_section_title
;
 Synthesis and Structure of PNP-Supported Iridium Silyl and Silylene
 Complexes: Catalytic Hydrosilation of Alkenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11161
_journal_page_last               11173
_journal_paper_doi               10.1021/ja903737j
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C50 H67 Ir N P2 Si, 0.704(C8)'
_chemical_formula_sum            'C55.63 H67 Ir N P2 Si'
_chemical_formula_weight         1031.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 119.15(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   49.248(10)
_cell_length_b                   9.3164(19)
_cell_length_c                   26.135(5)
_cell_measurement_reflns_used    22647
_cell_measurement_temperature    178(2)
_cell_measurement_theta_max      36.915
_cell_measurement_theta_min      4.480
_cell_volume                     10472(5)
_computing_cell_refinement       'Bruker SAINT v7.07'
_computing_data_collection       'Bruker SMART v5.631'
_computing_data_reduction        'Bruker SAINT v7.07'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      178(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Apex'
_diffrn_measurement_method       '/w scans'
_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  0.0823
_diffrn_reflns_av_sigmaI/netI    0.1039
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            21819
_diffrn_reflns_theta_full        23.40
_diffrn_reflns_theta_max         23.40
_diffrn_reflns_theta_min         0.95
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.668
_exptl_absorpt_correction_T_max  0.9242
_exptl_absorpt_correction_T_min  0.7762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       block
_exptl_crystal_F_000             4224
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.860
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         7595
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0970
_reflns_number_gt                5239
_reflns_number_total             7595
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja903737j_si_002.cif
_cod_data_source_block           ec13as
_cod_original_cell_volume        10472(4)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4104822