Synthesis and Electronic Structure of Bis(imino)pyridine Iron Metallacyclic Intermediates in Iron-Catalyzed Cyclization Reactions
Jordan M. Hoyt; Kevin T. Sylvester; Scott P. Semproni; Paul J. Chirik; Journal of the American Chemical Society 135 (2013) 4862–4877; doi:10.1021/ja400895j

data_4119505
_publ_section_title
;
 Synthesis and Electronic Structure of Bis(imino)pyridine Iron
 Metallacyclic Intermediates in Iron-Catalyzed Cyclization Reactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4862
_journal_page_last               4877
_journal_paper_doi               10.1021/ja400895j
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C43 H57 Fe N3'
_chemical_formula_weight         671.77
_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                90.000
_cell_angle_beta                 97.324(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   8.709(5)
_cell_length_b                   16.587(5)
_cell_length_c                   24.956(5)
_cell_measurement_reflns_used    8793
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.80
_cell_measurement_theta_min      3.21
_cell_volume                     3576(2)
_computing_cell_refinement       'BRUKER, APEX II SOFTWARE SUITE'
_computing_data_collection       'BRUKER, APEX II SOFTWARE SUITE'
_computing_data_reduction        'BRUKER, APEX II SOFTWARE SUITE'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Giacovazzo, 1994)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17495
_diffrn_reflns_theta_full        65.98
_diffrn_reflns_theta_max         65.98
_diffrn_reflns_theta_min         3.21
_exptl_absorpt_coefficient_mu    3.627
_exptl_absorpt_correction_T_max  0.7527
_exptl_absorpt_correction_T_min  0.6502
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       rectangle
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.864
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         6103
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0735
_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^)+(0.0505P)^2^+15.4228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1934
_refine_ls_wR_factor_ref         0.1980
_reflns_number_gt                5262
_reflns_number_total             6103
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja400895j_si_001_1.cif
_cod_data_source_block           jmh7
_cod_database_code               4119505