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_4119507
_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            'C55 H74 Fe N4 O3 S'
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_chemical_name_systematic
;
 ?
;
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_cell_angle_gamma                85.9630(10)
_cell_formula_units_Z            2
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_cell_length_b                   14.9302(2)
_cell_length_c                   15.2417(2)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    100(2)
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_cell_measurement_theta_min      3.66
_cell_volume                     2515.73(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP3 (Farraguia, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacavazzo, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 'ACTA 50'
_diffrn_measured_fraction_theta_max 0.939
_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     1.54178
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0361
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_diffrn_reflns_limit_k_min       -17
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_diffrn_reflns_limit_l_min       -17
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_diffrn_reflns_theta_full        'ACTA 50'
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_exptl_absorpt_correction_T_min  0.6055
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (BrukeR AXS)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       block
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.167
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_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.928
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         8267
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_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0854P)^2^+0.9875P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_threshold_expression     >2\s(I)
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_cod_database_code               4119507