Tuning the Fe(II/III) Redox Potential in Nonheme Fe(II)-Hydroxo Complexes through Primary and Secondary Coordination Sphere Modifications.
Gordon, Zachary; Drummond, Michael J.; Matson, Ellen M.; Bogart, Justin A.; Schelter, Eric J.; Lord, Richard L.; Fout, Alison R.; Inorganic chemistry 56 (2017) 4852–4863; doi:10.1021/acs.inorgchem.6b03071

data_4345651
_publ_section_title
;
 Tuning the Fe(II/III) Redox Potential in Nonheme Fe(II)-Hydroxo Complexes
 through Primary and Secondary Coordination Sphere Modifications.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4852
_journal_page_last               4863
_journal_paper_doi               10.1021/acs.inorgchem.6b03071
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C36 H33 Fe N7 O'
_chemical_formula_sum            'C36 H33 Fe N7 O'
_chemical_formula_weight         635.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-03-19
_audit_creation_method
; 
Olex2 1.2 
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155) 
;
_cell_angle_alpha                90
_cell_angle_beta                 91.705(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8142(6)
_cell_length_b                   14.1429(9)
_cell_length_c                   24.2432(16)
_cell_measurement_reflns_used    9811
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.21
_cell_volume                     3020.8(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2013.10-0 (Bruker, 2013)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2013/3, SADABS V2012/1, TWINABS V2012/1 
(Bruker, 2012 & 2013) 
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELX-2013-4 (Sheldrick, 2013)'
_computing_structure_solution    'SHELX-2013-4 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker Photon 100 area detector'
_diffrn_detector_type            'photon counter area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  cd29s
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            66799
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.440
_diffrn_reflns_theta_min         2.213
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.542
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9010
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
; 
SADABS-2014/4 (Bruker,2014) was used for absorption correction. 
wR2(int) was 0.0646 before and 0.0546 after correction. 
The Ratio of minimum to maximum transmission is 0.9010. 
The \l/2 correction factor is Not present. 
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1328
_exptl_crystal_id                cd29s
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (1,2,-4) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.192
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         6187
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0387P)^2^+3.5813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1123
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5513
_reflns_number_total             6187
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b03071_si_001.cif
_cod_data_source_block           cd29ssa
_cod_depositor_comments
'Adding full bibliography for 4345651--4345656.cif.'
_cod_database_code               4345651
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.903
_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 
2. Restrained distances 
 O1-H1 
 0.84 with sigma of 0.02 
3.a Secondary CH2 refined with riding coordinates: 
 C1(H1A,H1B), C13(H13A,H13B), C25(H25A,H25B) 
3.b Aromatic/amide H refined with riding coordinates: 
 C3(H3), C4(H4), C6(H6A), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), 
 C15(H15), C16(H16), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), 
 C24(H24),  C27(H27), C28(H28), C30(H30), C32(H32), C33(H33), C34(H34), 
 C35(H35), C36(H36) 
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'