[FeIV=O(TBC)(CH3CN)]2+: Comparative Reactivity of Iron(IV)-Oxo Species with Constrained Equatorial Cyclam Ligation
Samuel A. Wilson; Junying Chen; Seungwoo Hong; Yong-Min Lee; Martin Clémancey; Ricardo Garcia-Serres; Takashi Nomura; Takashi Ogura; Jean-Marc Latour; Britt Hedman; Keith O. Hodgson; Wonwoo Nam; Edward I. Solomon; Journal of the American Chemical Society 134 (2012) 11791–11806; doi:10.1021/ja3046298

data_4118277
_publ_section_title
;
 [FeIV=O(TBC)(CH3CN)]2+: Comparative Reactivity of Iron(IV)-Oxo Species
 with Constrained Equatorial Cyclam Ligation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11791
_journal_page_last               11806
_journal_paper_doi               10.1021/ja3046298
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C46 H57 F6 Fe N7 O6 S2'
_chemical_formula_sum            'C46 H57 F6 Fe N7 O6 S2'
_chemical_formula_weight         1037.96
_chemical_name_common            'iron(II) TBC triflate'
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                67.041(8)
_cell_angle_beta                 72.676(9)
_cell_angle_gamma                67.039(8)
_cell_formula_units_Z            2
_cell_length_a                   12.1461(18)
_cell_length_b                   13.876(2)
_cell_length_c                   17.131(3)
_cell_measurement_reflns_used    8280
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.60
_cell_volume                     2411.5(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.1296
_diffrn_reflns_av_sigmaI/netI    0.1596
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22851
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_T_max  0.8700
_exptl_absorpt_correction_T_min  0.8700
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       Block
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         2.186
_refine_diff_density_min         -3.930
_refine_diff_density_rms         0.243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         8905
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.2378
_refine_ls_R_factor_gt           0.0803
_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^)+(0.2000P)^2^+0.6546P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2050
_refine_ls_wR_factor_ref         0.3209
_reflns_number_gt                5438
_reflns_number_total             8905
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3046298_si_003.cif
_cod_data_source_block           CCDC-875224
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'Constr' changed to 'constr'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2411.7(6)
_cod_database_code               4118277