Oxidation and Reduction of Bis(imino)pyridine Iron Dicarbonyl Complexes
Aaron M. Tondreau; Carsten Milsmann; Emil Lobkovsky; Paul J. Chirik; Inorganic Chemistry 50 (2011) 9888–9895; doi:10.1021/ic200730k

data_4326455
_publ_section_title
;
 Oxidation and Reduction of Bis(imino)pyridine Iron Dicarbonyl Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9888
_journal_page_last               9895
_journal_paper_doi               10.1021/ic200730k
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C32 H12 B F24, C35 H43 Fe N3 O2'
_chemical_formula_sum            'C67 H55 B F24 Fe N3 O2'
_chemical_formula_weight         1456.80
_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                 106.010(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.4932(11)
_cell_length_b                   18.0250(11)
_cell_length_c                   22.4714(13)
_cell_measurement_reflns_used    9947
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.82
_cell_measurement_theta_min      2.20
_cell_volume                     6810.7(7)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            56881
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.66
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.332
_exptl_absorpt_correction_T_max  0.9836
_exptl_absorpt_correction_T_min  0.8785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_description       plate
_exptl_crystal_F_000             2964
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
;
_refine_diff_density_max         0.934
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1069
_refine_ls_number_reflns         13914
_refine_ls_number_restraints     396
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.311
_refine_ls_shift/su_mean         0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0765P)^2^+7.5512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1577
_refine_ls_wR_factor_ref         0.1731
_reflns_number_gt                9499
_reflns_number_total             13914
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200730k_si_001.cif
_cod_data_source_block           amt32
_cod_database_code               4326455