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_4086806
_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_moiety         'C40.50 H27 Cl Fe N4 O4'
_chemical_formula_sum            'C40.5 H27 Cl Fe N4 O4'
_chemical_formula_weight         724.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   'calculated positions'
_atom_sites_solution_primary     'Patterson method'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 108.03(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.144(1)
_cell_length_b                   22.421(1)
_cell_length_c                   12.280(1)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      1.82
_cell_volume                     3179.4(4)
_computing_cell_refinement       'IPDS 2T (Stoe)'
_computing_data_collection       'IPDS 2T (Stoe)'
_computing_data_reduction        'IPDS 2T (Stoe)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'IPDS 2T (Stoe)'
_diffrn_measurement_method       'IPDS 2T (Stoe)'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16645
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.902
_diffrn_reflns_theta_min         1.817
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.611
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-red32/X-area (Stoe)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_description       plates
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.902
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         6130
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0380P)^2^+1.5476P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0787
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5436
_reflns_number_total             6130
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00765_si_003.cif
_cod_data_source_block           shelx
_cod_original_formula_sum        'C40.50 H27 Cl Fe N4 O4'
_cod_database_code               4086806
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              63473
_shelx_hkl_checksum              134