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_4129961
_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            'C192.99 H160.09 F12 Fe8 N29.4 O24.67 S4'
_chemical_formula_weight         4088.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/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                 95.8456(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.3192(13)
_cell_length_b                   30.6264(16)
_cell_length_c                   24.9005(14)
_cell_measurement_reflns_used    9269
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.71
_cell_measurement_theta_min      2.23
_cell_volume                     18449.7(17)
_computing_cell_refinement       'SAINT v8.34A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 v2014.11-0 (Bruker-AXS, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker-AXS, 2007)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013/1 (She ldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0771
_diffrn_reflns_av_unetI/netI     0.0658
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            102679
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.023
_diffrn_reflns_theta_max         25.023
_diffrn_reflns_theta_min         2.230
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6426
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/5 (Sheldrick, 2014)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             8405
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.023
_refine_diff_density_min         -0.921
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1596
_refine_ls_number_reflns         16143
_refine_ls_number_restraints     1597
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.1263
_refine_ls_R_factor_gt           0.0773
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1363P)^2^+94.9319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2051
_refine_ls_wR_factor_ref         0.2440
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10454
_reflns_number_total             16143
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b12214_si_001.cif
_cod_data_source_block           P14254
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C192.99 H160.09 F12 Fe8 N29.40 O24.67 S4'
_cod_database_code               4129961
_shelxl_version_number           2014-2
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.865
_shelx_res_checksum              53153
_shelx_hkl_checksum              84852
_shelx_shelxl_version_number     2014/7