The mechanism of oxidative addition of Pd(0) to Si‒H bonds: electronic effects, reaction mechanism, and hydrosilylation
Hurst, Michael R.; Zakharov, Lev N.; Cook, Amanda K.; Chemical Science  (2021) –; doi:10.1039/D1SC04419B

data_1564637
_publ_section_title
;
 The mechanism of oxidative addition of Pd(0) to Si--H bonds: electronic
 effects, reaction mechanism, and hydrosilylation
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC04419B
_journal_year                    2021
_chemical_formula_sum            'C47 H61 F9 P2 Pd Si'
_chemical_formula_weight         993.38
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-05-27 deposited with the CCDC.	2021-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.3966(6)
_cell_length_b                   21.9565(7)
_cell_length_c                   22.9636(7)
_cell_measurement_reflns_used    9796
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      66.54
_cell_measurement_theta_min      3.68
_cell_volume                     9275.6(5)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            54242
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.634
_diffrn_reflns_theta_max         66.634
_diffrn_reflns_theta_min         3.678
_diffrn_source                   'Incoatec I\mS'
_exptl_absorpt_coefficient_mu    4.716
_exptl_absorpt_correction_T_max  0.5842
_exptl_absorpt_correction_T_min  0.4569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       cut-block
_exptl_crystal_F_000             4112
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         8175
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+6.5302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0715
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7340
_reflns_number_total             8175
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04419b2.cif
_cod_data_source_block           cu_cook1_0m
_cod_database_code               1564637
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.501
_shelx_estimated_absorpt_t_max   0.704
_shelx_res_checksum              18873
_shelx_hkl_checksum              83300