Reactivity and Mössbauer Spectroscopic Characterization of an Fe(IV) Ketimide Complex and Reinvestigation of an Fe(IV) Norbornyl Complex
Richard A. Lewis; Danil E. Smiles; Jonathan M. Darmon; S. Chantal E. Stieber; Guang Wu; Trevor W. Hayton; Inorganic Chemistry 52 (2013) 8218–8227; doi:10.1021/ic401096p

data_4335494
_publ_section_title
;
 Reactivity and M\"ossbauer Spectroscopic Characterization of an Fe(IV)
 Ketimide Complex and Reinvestigation of an Fe(IV) Norbornyl Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8218
_journal_page_last               8227
_journal_paper_doi               10.1021/ic401096p
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C28 H44 Fe'
_chemical_formula_weight         436.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           31
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac -2'
_symmetry_space_group_name_H-M   'P m n 21'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.7710(5)
_cell_length_b                   10.0996(4)
_cell_length_c                   9.7652(4)
_cell_measurement_temperature    100(2)
_cell_volume                     1160.91(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0141
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13440
_diffrn_reflns_theta_full        23.91
_diffrn_reflns_theta_max         23.91
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.661
_exptl_absorpt_correction_T_max  0.9368
_exptl_absorpt_correction_T_min  0.7778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_description       block
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.461
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.228
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.16(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     80
_refine_ls_number_reflns         1902
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.1353
_refine_ls_R_factor_gt           0.1339
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.3500P)^2^+0.0400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3560
_refine_ls_wR_factor_ref         0.3659
_reflns_number_gt                1860
_reflns_number_total             1902
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401096p_si_001_2.cif
_cod_data_source_block           Complex_4
_cod_database_code               4335494