Spectroscopic and DFT Characterization of a Highly Reactive Nonheme Fe<sup>V</sup>-Oxo Intermediate.
Fan, Ruixi; Serrano-Plana, Joan; Oloo, Williamson N.; Draksharapu, Apparao; Delgado-Pinar, Estefanía; Company, Anna; Martin-Diaconescu, Vlad; Borrell, Margarida; Lloret-Fillol, Julio; García-España, Enrique; Guo, Yisong; Bominaar, Emile L.; Que, Jr, Lawrence; Costas, Miquel; Münck, Eckard; Journal of the American Chemical Society 140 (2018) 3916–3928; doi:10.1021/jacs.7b11400

data_4131826
_publ_section_title
;
 Spectroscopic and DFT Characterization of a Highly Reactive Nonheme
 Fe<sup>V</sup>-Oxo Intermediate.
;
_journal_issue                   11
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3916
_journal_page_last               3928
_journal_paper_doi               10.1021/jacs.7b11400
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C17 H26 F6 Fe N4 O7 S2'
_chemical_formula_sum            'C17 H26 F6 Fe N4 O7 S2'
_chemical_formula_weight         632.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9397(19)
_cell_length_b                   10.0271(10)
_cell_length_c                   13.5393(14)
_cell_measurement_reflns_used    6134
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.33
_cell_volume                     2435.5(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            36725
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.323
_diffrn_reflns_theta_min         2.271
_exptl_absorpt_coefficient_mu    0.884
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.858336
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS v2.10 BRUKER 2001'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_description       plate
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 2654 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).

 B-alert requesting for doing a TWIN/BASF refinement is reported.
 The twin refinement was done, with a result of a basf parameter
 of 0.016, which we think is meaningless
;
_refine_ls_abs_structure_Flack   0.017(5)
_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     337
_refine_ls_number_reflns         6034
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0384P)^2^+0.1529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0614
_refine_ls_wR_factor_ref         0.0620
_reflns_Friedel_coverage         0.913
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                5836
_reflns_number_total             6034
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b11400_si_002.cif
_cod_data_source_block           jsl8p76
_cod_database_code               4131826
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              62066
_shelx_hkl_checksum              29216