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_4121373
_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            'C28 H43 Cl4 Fe N2 O P'
_chemical_formula_weight         652.26
_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                101.281(5)
_cell_angle_beta                 97.097(4)
_cell_angle_gamma                90.207(5)
_cell_formula_units_Z            4
_cell_length_a                   10.068(3)
_cell_length_b                   15.684(4)
_cell_length_c                   20.994(6)
_cell_measurement_reflns_used    2121
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      23.47
_cell_measurement_theta_min      2.38
_cell_volume                     3224.8(16)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.1427
_diffrn_reflns_av_sigmaI/netI    0.2433
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22266
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.872
_exptl_absorpt_correction_T_max  0.9828
_exptl_absorpt_correction_T_min  0.8588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       plate
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.188
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         12586
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1964
_refine_ls_R_factor_gt           0.0779
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1525
_refine_ls_wR_factor_ref         0.1851
_reflns_number_gt                5243
_reflns_number_total             12586
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja404963f_si_003_1.cif
_cod_data_source_block           mo_dm12616_0m
_cod_original_cell_volume        3225.0(15)
_cod_database_code               4121373