Intramolecular C-H and C-F Bond Oxygenation Mediated by a Putative Terminal Oxo Species in Tetranuclear Iron Complexes.
de Ruiter, Graham; Thompson, Niklas B.; Takase, Michael K.; Agapie, Theodor; Journal of the American Chemical Society 138 (2016) 1486–1489; doi:10.1021/jacs.5b12214

data_4129963
_publ_section_title
;
 Intramolecular C-H and C-F Bond Oxygenation Mediated by a Putative
 Terminal Oxo Species in Tetranuclear Iron Complexes.
;
_journal_issue                   5
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1486
_journal_page_last               1489
_journal_paper_doi               10.1021/jacs.5b12214
_journal_volume                  138
_journal_year                    2016
_chemical_formula_sum            'C97.52 H75.28 F12 Fe4 N15.76 O11 S2'
_chemical_formula_weight         2159.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 96.7988(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.6768(14)
_cell_length_b                   17.6060(11)
_cell_length_c                   24.2443(14)
_cell_measurement_reflns_used    9701
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      2.23
_cell_volume                     9611.4(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker-AXS, 2013)'
_computing_data_collection       'APEX2 v2014.11-0 (Bruker-AXS, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker-AXS, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
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_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker KAPPA APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 1.000
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_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            166656
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.492
_diffrn_reflns_theta_min         1.640
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.727
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/5 (Sheldrick, 2014)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             4411
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.260
_refine_diff_density_max         1.587
_refine_diff_density_min         -1.027
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1536
_refine_ls_number_reflns         22043
_refine_ls_number_restraints     1414
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.1075
_refine_ls_R_factor_gt           0.0792
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1310P)^2^+30.2212P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2235
_refine_ls_wR_factor_ref         0.2467
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16102
_reflns_number_total             22043
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b12214_si_001.cif
_cod_data_source_block           A15114
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4129963
_shelxl_version_number           2014-2
_shelx_estimated_absorpt_t_max   0.833
_shelx_estimated_absorpt_t_min   0.785
_shelx_res_checksum              88042
_shelx_hkl_checksum              55406
_shelx_shelxl_version_number     2014/7