Metal versus Ligand Alkylation in the Reactivity of the (Bis-iminopyridinato)Fe Catalyst
Jennifer Scott; Sandro Gambarotta; Ilia Korobkov; Peter H. M. Budzelaar; Journal of the American Chemical Society 127 (2005) 13019–13029; doi:10.1021/ja054152b

data_4111940
_publ_section_title
;
 Metal versus Ligand Alkylation in the Reactivity of the
 (Bis-iminopyridinato)Fe Catalyst
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13019
_journal_page_last               13029
_journal_paper_doi               10.1021/ja054152b
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C41 H65 Fe N3 Si2'
_chemical_formula_weight         711.99
_chemical_name_systematic
; 
 ? 
;
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_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.135(5)
_cell_angle_beta                 85.805(6)
_cell_angle_gamma                66.610(5)
_cell_formula_units_Z            2
_cell_length_a                   9.610(3)
_cell_length_b                   10.865(3)
_cell_length_c                   22.115(7)
_cell_measurement_reflns_used    147
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      24.11
_cell_measurement_theta_min      1.85
_cell_volume                     2113.4(11)
_computing_cell_refinement       'SMART, Bruker (2000)'
_computing_data_collection       'SMART, Bruker (2000)'
_computing_data_reduction        'XPREP, Bruker (2000)'
_computing_molecular_graphics    'SHELXTL, Bruker (2000)'
_computing_publication_material  'SHELXTL, Bruker (2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      208(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0883
_diffrn_reflns_av_sigmaI/netI    0.1209
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19117
_diffrn_reflns_theta_full        24.11
_diffrn_reflns_theta_max         24.11
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.443
_exptl_absorpt_correction_T_max  0.9570
_exptl_absorpt_correction_T_min  0.8786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            dark_brown
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_description       plates
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.30
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_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         6695
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1298
_refine_ls_R_factor_gt           0.0721
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'calc w=1/[\s^2^(Fo^2^)+(0.0577P)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1272
_refine_ls_wR_factor_ref         0.1443
_reflns_number_gt                4196
_reflns_number_total             6695
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja054152bsi20050627_052614_2.cif
_cod_data_source_block           complex-3
_cod_original_cell_volume        2113.5(12)
_cod_database_code               4111940