Synthesis and Electronic Structure of Cationic, Neutral, and Anionic Bis(imino)pyridine Iron Alkyl Complexes: Evaluation of Redox Activity in Single-Component Ethylene Polymerization Catalysts
Aaron M. Tondreau; Carsten Milsmann; Andrew D. Patrick; Helen M. Hoyt; Emil Lobkovsky; Karl Wieghardt; Paul J. Chirik; Journal of the American Chemical Society 132 (2010) 15046–15059; doi:10.1021/ja106575b

data_4103351
_publ_section_title
;
 Synthesis and Electronic Structure of Cationic, Neutral, and Anionic
 Bis(imino)pyridine Iron Alkyl Complexes: Evaluation of Redox Activity in
 Single-Component Ethylene Polymerization Catalysts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15046
_journal_page_last               15059
_journal_paper_doi               10.1021/ja106575b
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C34 H46 Fe N3, C24 H20 B'
_chemical_formula_sum            'C58 H66 B Fe N3'
_chemical_formula_weight         871.80
_chemical_name_systematic
; 
 ? 
;
_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                90.00
_cell_angle_beta                 109.125(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.6102(12)
_cell_length_b                   10.5514(7)
_cell_length_c                   26.7885(18)
_cell_measurement_reflns_used    3793
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.16
_cell_measurement_theta_min      2.98
_cell_volume                     4970.0(6)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT+'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0607
_diffrn_reflns_av_sigmaI/netI    0.0751
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            23655
_diffrn_reflns_theta_full        22.46
_diffrn_reflns_theta_max         22.46
_diffrn_reflns_theta_min         1.61
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.343
_exptl_absorpt_correction_T_max  0.9915
_exptl_absorpt_correction_T_min  0.8749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         6417
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0986
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+3.8731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1253
_reflns_number_gt                4095
_reflns_number_total             6417
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja106575b_si_001_3.cif
_cod_data_source_block           ap7
_cod_database_code               4103351