Bis(imino)pyridine Iron Alkyls Containing β-Hydrogens: Synthesis, Evaluation of Kinetic Stability, and Decomposition Pathways Involving Chelate Participation
Ryan J. Trovitch; Emil Lobkovsky; Paul J. Chirik; Journal of the American Chemical Society 130 (2008) 11631–11640; doi:10.1021/ja803296f

data_4108263
_publ_section_title
;
 Bis(imino)pyridine Iron Alkyls Containing \b-Hydrogens: Synthesis,
 Evaluation of Kinetic Stability, and Decomposition Pathways Involving
 Chelate Participation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11631
_journal_page_last               11640
_journal_paper_doi               10.1021/ja803296f
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C37 H50 Br Fe N3 O'
_chemical_formula_sum            'C37 H50 Br Fe N3 O'
_chemical_formula_weight         688.56
_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                 100.634(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2777(3)
_cell_length_b                   15.6945(6)
_cell_length_c                   22.1373(7)
_cell_measurement_reflns_used    2528
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20.75
_cell_measurement_theta_min      2.28
_cell_volume                     3509.5(2)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0790
_diffrn_reflns_av_sigmaI/netI    0.0651
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24922
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    1.600
_exptl_absorpt_correction_T_max  0.9243
_exptl_absorpt_correction_T_min  0.6905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         5047
_refine_ls_number_restraints     175
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.375
_refine_ls_shift/su_mean         0.024
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0572P)^2^+1.9774P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1065
_refine_ls_wR_factor_ref         0.1244
_reflns_number_gt                3336
_reflns_number_total             5047
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja803296f-file002.cif
_cod_data_source_block           rt35
_cod_database_code               4108263