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_4111942
_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            'C53 H86 Fe Li N3 O4 Si'
_chemical_formula_weight         920.13
_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                 97.75(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.998(19)
_cell_length_b                   27.61(3)
_cell_length_c                   24.90(3)
_cell_measurement_reflns_used    113
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      21.97
_cell_measurement_theta_min      1.47
_cell_volume                     10898(2)
_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      213(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0676
_diffrn_reflns_av_sigmaI/netI    0.0572
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            60282
_diffrn_reflns_theta_full        21.97
_diffrn_reflns_theta_max         21.97
_diffrn_reflns_theta_min         1.47
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.342
_exptl_absorpt_correction_T_max  0.9195
_exptl_absorpt_correction_T_min  0.9045
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            dk_red
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_description       block
_exptl_crystal_F_000             4000
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1135
_refine_ls_number_reflns         13249
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0688
_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^)+(0.0773P)^2^+15.2965P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1518
_refine_ls_wR_factor_ref         0.1685
_reflns_number_gt                9417
_reflns_number_total             13249
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja054152bsi20050627_052614_4.cif
_cod_data_source_block           complex
_cod_original_cell_volume        10902(22)
_cod_database_code               4111942