Mechanism of the Bis(imino)pyridine-Iron-Catalyzed Hydromagnesiation of Styrene Derivatives.
Neate, Peter G. N.; Greenhalgh, Mark D.; Brennessel, William W.; Thomas, Stephen P.; Neidig, Michael L.; Journal of the American Chemical Society 141 (2019) 10099–10108; doi:10.1021/jacs.9b04869

data_4128290
_publ_section_title
;
 Mechanism of the Bis(imino)pyridine-Iron-Catalyzed Hydromagnesiation of
 Styrene Derivatives.
;
_journal_issue                   25
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10099
_journal_page_last               10108
_journal_paper_doi               10.1021/jacs.9b04869
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety
'C37 H52 Fe N3, C20 H40 Br0.67 Cl0.33 Mg O5, 2.5(C4 H8 O)'
_chemical_formula_sum            'C67 H112 Br0.67 Cl0.33 Fe Mg N3 O7.5'
_chemical_formula_weight         1224.99
_chemical_name_common            neipn01
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90
_cell_angle_beta                 99.122(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4045(18)
_cell_length_b                   22.533(4)
_cell_length_c                   26.176(4)
_cell_measurement_reflns_used    3719
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      33.18
_cell_measurement_theta_min      2.74
_cell_volume                     6641.6(19)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2014)'
_computing_publication_material  'SHELXTL (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0801
_diffrn_reflns_av_unetI/netI     0.0606
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
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_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            149257
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        33.729
_diffrn_reflns_theta_max         33.762
_diffrn_reflns_theta_min         1.807
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.706
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.5750
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2015a)'
_exptl_crystal_colour            yellow-brown
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_description       block
_exptl_crystal_F_000             2648
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_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.978
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     812
_refine_ls_number_reflns         26483
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0473P)^2^+2.9327P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1224
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17987
_reflns_number_total             26483
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04869_si_002.cif
_cod_data_source_block           neipn01
_cod_original_cell_volume        6641.8(18)
_cod_original_formula_sum        'C67 H112 Br0.67 Cl0.33 Fe Mg N3 O7.50'
_cod_database_code               4128290
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.728
_shelx_estimated_absorpt_t_max   0.895
_shelx_res_checksum              48258
_shelx_hkl_checksum              81113