Phosphinite-Iminopyridine Iron Catalysts for Chemoselective Alkene Hydrosilylation
Dongjie Peng; Yanlu Zhang; Xiaoyong Du; Lei Zhang; Xuebing Leng; Marc D. Walter; Zheng Huang; Journal of the American Chemical Society 135 (2013) 19154–19166; doi:10.1021/ja404963f

data_4121375
_publ_section_title
;
 Phosphinite-Iminopyridine Iron Catalysts for Chemoselective Alkene
 Hydrosilylation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19154
_journal_page_last               19166
_journal_paper_doi               10.1021/ja404963f
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C29 H41 Fe N2 O3 P'
_chemical_formula_weight         552.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.045(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.4863(17)
_cell_length_b                   10.2818(9)
_cell_length_c                   16.1659(13)
_cell_measurement_reflns_used    2902
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      66.54
_cell_measurement_theta_min      5.00
_cell_volume                     2877.9(4)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1259
_diffrn_reflns_av_sigmaI/netI    0.1065
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22249
_diffrn_reflns_theta_full        70.03
_diffrn_reflns_theta_max         70.03
_diffrn_reflns_theta_min         5.11
_exptl_absorpt_coefficient_mu    4.972
_exptl_absorpt_correction_T_max  0.9520
_exptl_absorpt_correction_T_min  0.6918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       plate
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.990
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         5289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1306
_refine_ls_R_factor_gt           0.0779
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1228P)^2^+1.8661P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1931
_refine_ls_wR_factor_ref         0.2290
_reflns_number_gt                3150
_reflns_number_total             5289
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja404963f_si_003_3.cif
_cod_data_source_block           dm13260
_cod_database_code               4121375