Efficient Hydrosilylation of Acetophenone with a New Anthraquinonic Amide-Based Iron Precatalyst
Raya-Barón, Álvaro; Ortuño, Manuel A.; Oña-Burgos, Pascual; Rodríguez-Diéguez, Antonio; Langer, Robert; Cramer, Christopher J.; Kuzu, Istemi; Fernández, Ignacio; Organometallics  (2016) –; doi:10.1021/acs.organomet.6b00765

data_4086805
_publ_section_title
;
 Efficient Hydrosilylation of Acetophenone with a New Anthraquinonic
 Amide-Based Iron Precatalyst
;
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/acs.organomet.6b00765
_journal_year                    2016
_chemical_formula_sum            'C46 H38 Fe N4 O5.5'
_chemical_formula_weight         790.65
_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                62.57(1)
_cell_angle_beta                 71.99(1)
_cell_angle_gamma                67.97(1)
_cell_formula_units_Z            2
_cell_length_a                   11.870(1)
_cell_length_b                   13.363(1)
_cell_length_c                   14.023(1)
_cell_measurement_reflns_used    7500
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.95
_cell_measurement_theta_min      1.66
_cell_volume                     1804.8(3)
_computing_cell_refinement       'IPDS 2T (Stoe)'
_computing_data_collection       'IPDS 2T (Stoe)'
_computing_data_reduction        'IPDS 2T (Stoe)'
_computing_molecular_graphics    'WinGX (Farrugia, 1999)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution
;
 SIR-92 (Altomare, Cascarano, Giacovazzo, Guagliardi, Burla, Polidori,
        Camalli, 1992)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'IPDS 2T (Stoe)'
_diffrn_measurement_method       'IPDS 2T (Stoe)'
_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  0.1095
_diffrn_reflns_av_sigmaI/netI    0.1128
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15629
_diffrn_reflns_theta_full        25.95
_diffrn_reflns_theta_max         25.95
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.476
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'X-red32/X-area (Stoe)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.881
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         7014
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.0994
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0777P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1480
_reflns_number_gt                4579
_reflns_number_total             7014
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om6b00765_si_003.cif
_cod_data_source_block           Compound2
_cod_original_cell_volume        1804.8(2)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C46 H38 Fe N4 O5.50'
_cod_database_code               4086805