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_4335495
_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            'C52 H104 Fe Li N4 O8'
_chemical_formula_weight         976.18
_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                 108.316(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.260(6)
_cell_length_b                   19.428(6)
_cell_length_c                   16.840(6)
_cell_measurement_temperature    150(2)
_cell_volume                     5982(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.1438
_diffrn_reflns_av_sigmaI/netI    0.0943
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19556
_diffrn_reflns_theta_full        23.41
_diffrn_reflns_theta_max         23.41
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.300
_exptl_absorpt_correction_T_max  0.887
_exptl_absorpt_correction_T_min  0.836
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.084
_exptl_crystal_description       block
_exptl_crystal_F_000             2148
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         4368
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.1017
_refine_ls_R_factor_gt           0.0755
_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^)+(0.0800P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1882
_refine_ls_wR_factor_ref         0.2000
_reflns_number_gt                3190
_reflns_number_total             4368
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401096p_si_001_3.cif
_cod_data_source_block           Complex_5
_cod_database_code               4335495