Trapping a Highly Reactive Nonheme Iron Intermediate That Oxygenates Strong C-H Bonds with Stereoretention.
Serrano-Plana, Joan; Oloo, Williamson N.; Acosta-Rueda, Laura; Meier, Katlyn K.; Verdejo, Begoña; García-España, Enrique; Basallote, Manuel G.; Münck, Eckard; Que, Jr, Lawrence; Company, Anna; Costas, Miquel; Journal of the American Chemical Society 137 (2015) 15833–15842; doi:10.1021/jacs.5b09904

data_4129720
_publ_section_title
;
 Trapping a Highly Reactive Nonheme Iron Intermediate That Oxygenates
 Strong C-H Bonds with Stereoretention.
;
_journal_issue                   50
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15833
_journal_page_last               15842
_journal_paper_doi               10.1021/jacs.5b09904
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C19 H34 Fe N5 O2, 2(Cl O4)'
_chemical_formula_sum            'C19 H34 Cl2 Fe N5 O10'
_chemical_formula_weight         619.26
_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
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 93.329(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.875(4)
_cell_length_b                   10.538(3)
_cell_length_c                   21.741(7)
_cell_measurement_reflns_used    1619
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      22.51
_cell_measurement_theta_min      2.15
_cell_volume                     2944.8(16)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXS'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 'ACTA 50'
_diffrn_measured_fraction_theta_max 0.777
_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  0.0711
_diffrn_reflns_av_unetI/netI     0.1015
_diffrn_reflns_Laue_measured_fraction_full 0.856
_diffrn_reflns_Laue_measured_fraction_max 0.777
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            11887
_diffrn_reflns_point_group_measured_fraction_full 0.856
_diffrn_reflns_point_group_measured_fraction_max 0.777
_diffrn_reflns_theta_full        'ACTA 50'
_diffrn_reflns_theta_max         28.289
_diffrn_reflns_theta_min         1.877
_exptl_absorpt_coefficient_mu    0.748
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.729360
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'sadabs v2.10 bruker  2001'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       plate
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.863
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         5675
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.2100
_refine_ls_R_factor_gt           0.1179
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1876P)^2^+6.7445P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3203
_refine_ls_wR_factor_ref         0.3844
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2545
_reflns_number_total             5675
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b09904_si_003.cif
_cod_data_source_block           jsl7p31_sq_s
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4129720
_shelxl_version_number           2013-3
_shelx_res_checksum              20322
_shelx_hkl_checksum              80005
_shelx_fab_checksum              40048