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_4335493
_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            'C23 H43 Fe N2 O2'
_chemical_formula_weight         435.44
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   constr
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                68.873(4)
_cell_angle_beta                 84.357(4)
_cell_angle_gamma                73.185(4)
_cell_formula_units_Z            2
_cell_length_a                   8.4491(5)
_cell_length_b                   11.0002(6)
_cell_length_c                   15.0329(9)
_cell_measurement_temperature    100(2)
_cell_volume                     1247.52(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(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  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10797
_diffrn_reflns_theta_full        24.82
_diffrn_reflns_theta_max         24.82
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_T_max  0.9695
_exptl_absorpt_correction_T_min  0.7887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_description       block
_exptl_crystal_F_000             474
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         4265
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+0.4351P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0767
_reflns_number_gt                3552
_reflns_number_total             4265
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401096p_si_001_1.cif
_cod_data_source_block           Complex_3
_cod_database_code               4335493