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_4121374
_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            'C19 H25 Br2 Fe N2 O P'
_chemical_formula_weight         544.05
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                107.715(4)
_cell_angle_beta                 90.048(4)
_cell_angle_gamma                90.537(5)
_cell_formula_units_Z            4
_cell_length_a                   10.111(2)
_cell_length_b                   12.582(3)
_cell_length_c                   18.628(4)
_cell_measurement_reflns_used    4131
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      29.10
_cell_measurement_theta_min      2.31
_cell_volume                     2257.3(9)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_sigmaI/netI    0.0772
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15892
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    4.289
_exptl_absorpt_correction_T_max  0.8471
_exptl_absorpt_correction_T_min  0.5123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.840
_refine_diff_density_min         -1.542
_refine_diff_density_rms         0.278
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         8789
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.1109
_refine_ls_R_factor_gt           0.0850
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1183P)^2^+32.7433P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2439
_refine_ls_wR_factor_ref         0.2650
_reflns_number_gt                6528
_reflns_number_total             8789
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja404963f_si_003_2.cif
_cod_data_source_block           dm13015
_cod_database_code               4121374