(N-Phosphinoamidinate)Iron Pre-Catalysts for the Room Temperature Hydrosilylation of Carbonyl Compounds with Broad Substrate Scope at Low Loadings
Ruddy, Adam J.; Kelly, Colin M.; Crawford, Sarah M.; Wheaton, Craig A.; Sydora, Orson L.; Small, Brooke L.; Stradiotto, Mark; Turculet, Laura; Organometallics 32 (2013) 5581–; doi:10.1021/om400883u

data_4081702
_publ_section_title
;
 (N-Phosphinoamidinate)Iron Pre-Catalysts for the Room Temperature
 Hydrosilylation of Carbonyl Compounds with Broad Substrate Scope at Low
 Loadings
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5581
_journal_paper_doi               10.1021/om400883u
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C27 H41 N2 P'
_chemical_formula_weight         424.59
_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                 104.4940(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.6183(7)
_cell_length_b                   11.6578(5)
_cell_length_c                   29.7284(12)
_cell_measurement_reflns_used    9537
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      43.481
_cell_measurement_theta_min      4.412
_cell_volume                     5240.5(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            74295
_diffrn_reflns_theta_full        26.44
_diffrn_reflns_theta_max         26.44
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    0.120
_exptl_absorpt_correction_T_max  0.9746
_exptl_absorpt_correction_T_min  0.9360
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.076
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         10794
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+2.1870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1010
_refine_ls_wR_factor_ref         0.1105
_reflns_number_gt                8416
_reflns_number_total             10794
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400883u_si_002.cif
_cod_data_source_block           1b
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4081702