Radical Rebound Hydroxylation Versus H-Atom Transfer in Non-Heme Iron(III)-Hydroxo Complexes: Reactivity and Structural Differentiation.
Drummond, Michael J.; Ford, Courtney L.; Gray, Danielle L.; Popescu, Codrina V.; Fout, Alison R.; Journal of the American Chemical Society 141 (2019) 6639–6650; doi:10.1021/jacs.9b01516

data_4128246
_publ_section_title
;
 Radical Rebound Hydroxylation Versus H-Atom Transfer in Non-Heme
 Iron(III)-Hydroxo Complexes: Reactivity and Structural Differentiation.
;
_journal_issue                   16
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6639
_journal_page_last               6650
_journal_paper_doi               10.1021/jacs.9b01516
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C41 H48 Fe N7 O, C F3 O3 S, C2 H3 N'
_chemical_formula_sum            'C44 H51 F3 Fe N8 O4 S'
_chemical_formula_weight         897.81
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-11-28
_audit_creation_method
; 
Olex2 1.2 
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) 
;
_cell_angle_alpha                90
_cell_angle_beta                 97.809(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4584(5)
_cell_length_b                   13.8392(5)
_cell_length_c                   22.8632(9)
_cell_measurement_reflns_used    9592
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.76
_cell_measurement_theta_min      2.32
_cell_volume                     4218.9(3)
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2005)'
_computing_data_collection       'APEX3 V2016.9-0 (Bruker, 2016)'
_computing_data_reduction
; 
SAINT V8.37A, XPREP v2014/2, SADABS V2014/7 (Bruker, 2014) 
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELX-2014-7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX-2014-7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  dd77h
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            85169
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.791
_diffrn_reflns_theta_min         2.195
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.474
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1381 before and 0.0641 after correction. 
The Ratio of minimum to maximum transmission is 0.9335. 
The \l/2 correction factor is Not present. 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1876
_exptl_crystal_id                dd77h
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N) to a 
0.3 mm cryo-loop (Hampton Research) with the (-1, -4, 0) 
scattering planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.316
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.797
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         9001
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0470P)^2^+3.3800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.1009
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7769
_reflns_number_total             9001
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01516_si_004.cif
_cod_data_source_block           dd77h
_cod_database_code               4128246
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.865
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups, All C(H,H) groups 
 At 1.5 times of: 
  All C(H,H,H) groups, All N(H) groups, All O(H) groups 
2. Restrained distances 
 N6-H6 
 0.88 with sigma of 0.01 
 N7-H7 
 0.88 with sigma of 0.01 
3.a Ternary CH refined with riding coordinates: 
 C60(H60), C70(H70) 
3.b Secondary CH2 refined with riding coordinates: 
 C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A, 
 H65B), C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B), 
 C75(H75A,H75B) 
3.c Aromatic/amide H refined with riding coordinates: 
 C00T(H00T), C2(H2), C3(H3), C4(H4), C21(H21), C22(H22), C24(H24), C31(H31), 
 C32(H32), C34(H34), C41(H41), C42(H42), C43(H43), C44(H44), C51(H51), C52(H52), 
  C53(H53) 
3.d Idealised Me refined as rotating group: 
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C) 
;
_olex2_submission_special_instructions 'No special instructions were received'