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_4111941
_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            'C45 H66 Cl Fe Li N3 O3'
_chemical_formula_weight         795.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.094(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.574(3)
_cell_length_b                   18.331(5)
_cell_length_c                   21.787(5)
_cell_measurement_reflns_used    117
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      19.59
_cell_measurement_theta_min      1.46
_cell_volume                     4596(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      208(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.1090
_diffrn_reflns_av_sigmaI/netI    0.0816
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19173
_diffrn_reflns_theta_full        19.59
_diffrn_reflns_theta_max         19.59
_diffrn_reflns_theta_min         1.46
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.425
_exptl_absorpt_correction_T_max  0.9587
_exptl_absorpt_correction_T_min  0.9012
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker (2000)'
_exptl_crystal_colour            dk_brown
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_description       block
_exptl_crystal_F_000             1708
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         3986
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1129
_refine_ls_R_factor_gt           0.0783
_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^)+(0.0658P)^2^+9.9676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1540
_refine_ls_wR_factor_ref         0.1686
_reflns_number_gt                2999
_reflns_number_total             3986
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja054152bsi20050627_052614_3.cif
_cod_data_source_block           complex-4
_cod_original_cell_volume        4596.3(19)
_cod_database_code               4111941