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_4345652
_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 H30 Br3 Fe N7 O'
_chemical_formula_sum            'C36 H30 Br3 Fe N7 O'
_chemical_formula_weight         872.24
_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_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             2016-03-14
_audit_creation_method
; 
Olex2 1.2 
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155) 
;
_cell_angle_alpha                90
_cell_angle_beta                 92.915(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7341(7)
_cell_length_b                   16.2049(8)
_cell_length_c                   16.4602(8)
_cell_measurement_reflns_used    9387
_cell_measurement_temperature    100.01
_cell_measurement_theta_max      2.43
_cell_measurement_theta_min      28.30
_cell_volume                     3392.2(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      100.01
_diffrn_detector                 'Bruker Photon 100 area detector'
_diffrn_detector_type            'photon counter area detector'
_diffrn_measured_fraction_theta_full 0.9996
_diffrn_measured_fraction_theta_max 0.9960
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture/Photon 100'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  cd59z
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            91171
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         2.34
_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    4.020
_exptl_absorpt_correction_T_max  0.7875
_exptl_absorpt_correction_T_min  0.2674
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
; 
SADABS-2014/4 (Bruker,2014) was used for absorption correction. 
wR2(int) was 0.1640 before and 0.0638 after correction. 
The Ratio of minimum to maximum transmission is 0.3396. 
The \l/2 correction factor is 0.00150. 
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.7078
_exptl_crystal_description       column
_exptl_crystal_F_000             1734.7077
_exptl_crystal_id                cd59z
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (0,-1,-1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.438
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.096
_refine_diff_density_max         0.5934
_refine_diff_density_min         -0.8386
_refine_diff_density_rms         0.1163
_refine_ls_d_res_high            0.7481
_refine_ls_d_res_low             8.7023
_refine_ls_goodness_of_fit_ref   1.0834
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    54
_refine_ls_number_parameters     441
_refine_ls_number_reflns         8448
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0834
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0259P)^2^+4.8535P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0634
_refine_ls_wR_factor_ref         0.0691
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                7370
_reflns_number_total             8448
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ic6b03071_si_001.cif
_cod_data_source_block           cd59zsa
_cod_depositor_comments
'Adding full bibliography for 4345651--4345656.cif.'
_cod_database_code               4345652
_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 N(H) groups, All O(H) groups 
2.a Secondary CH2 refined with riding coordinates: 
 C1(H1a,H1b), C13(H13a,H13b), C25(H25a,H25b) 
2.b Aromatic/amide H refined with riding coordinates: 
 C4(H4), C6(H6a), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C16(H16), 
 C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C28(H28), 
 C30(H30),   C32(H32), C33(H33), C34(H34), C35(H35), C36(H36) 
;
_olex2_submission_special_instructions 'No special instructions were received'