Synthesis and Reactivity of Low-Coordinate Iron(II) Fluoride Complexes and Their Use in the Catalytic Hydrodefluorination of Fluorocarbons
Javier Vela; Jeremy M. Smith; Ying Yu; Nicole A. Ketterer; Christine J. Flaschenriem; Rene J. Lachicotte; Patrick L. Holland; Journal of the American Chemical Society 127 (2005) 7857–7870; doi:10.1021/ja042672l

data_4111705
_publ_section_title
;
 Synthesis and Reactivity of Low-Coordinate Iron(II) Fluoride Complexes
 and Their Use in the Catalytic Hydrodefluorination of Fluorocarbons
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7857
_journal_page_last               7870
_journal_paper_doi               10.1021/ja042672l
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C35 H53 F Fe N2'
_chemical_formula_weight         576.64
_chemical_name_common            2
_chemical_name_systematic
;
 (diketiminate)iron(ii) fluoride
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 108.491(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.480(3)
_cell_length_b                   8.5555(11)
_cell_length_c                   17.105(2)
_cell_measurement_reflns_used    2279
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_volume                     3258.7(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'SMART APEX'
_diffrn_measurement_method       hemisphere
_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  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0493
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16800
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    0.493
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.888
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_description       plate
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         4062
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+0.9679P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0965
_reflns_number_gt                3177
_reflns_number_total             4062
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja042672lsi20041206_123821_02.cif
_cod_data_source_block           2
_cod_database_code               4111705