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_4111707
_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_moiety         'C38 H62 Fe N2 S Si'
_chemical_formula_sum            'C38 H62 Fe N2 S Si'
_chemical_formula_weight         662.90
_chemical_name_common            4
_chemical_name_systematic
;
 L(tBu)FeSSiMe3
;
_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                 97.3040(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.4030(8)
_cell_length_b                   26.3684(15)
_cell_length_c                   19.7988(11)
_cell_measurement_reflns_used    5304
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      23.2
_cell_measurement_theta_min      2.2
_cell_volume                     7976.1(8)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        XPREP
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    WinGX
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '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  0.0742
_diffrn_reflns_av_sigmaI/netI    0.0992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34970
_diffrn_reflns_theta_full        23.28
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.486
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.890
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_description       block
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.206
_refine_diff_density_min         -0.206
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.899
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     809
_refine_ls_number_reflns         11459
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.899
_refine_ls_R_factor_all          0.1248
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0952
_reflns_number_gt                5858
_reflns_number_total             11459
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja042672lsi20041206_123821_04.cif
_cod_data_source_block           4
_cod_database_code               4111707