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_4345653
_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 H48 Br3 Fe N7 O'
_chemical_formula_sum            'C36 H48 Br3 Fe N7 O'
_chemical_formula_weight         890.39
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-10-06
_audit_creation_method
; 
Olex2 1.2 
(compiled 2016.08.31 svn.r3340 for OlexSys, GUI svn.r5227) 
;
_cell_angle_alpha                76.5460(10)
_cell_angle_beta                 83.8770(10)
_cell_angle_gamma                70.8190(10)
_cell_formula_units_Z            2
_cell_length_a                   11.7935(3)
_cell_length_b                   13.1513(3)
_cell_length_c                   14.3733(4)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      25.27
_cell_measurement_theta_min      2.27
_cell_volume                     2046.65(9)
_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      100.15
_diffrn_detector                 'Bruker APEXII CCD area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  cm58r
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            36902
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.460
_diffrn_reflns_theta_max         25.460
_diffrn_reflns_theta_min         1.457
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.333
_exptl_absorpt_correction_T_max  0.8605
_exptl_absorpt_correction_T_min  0.6488
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
; 
SADABS-2014/4 (Bruker,2014) was used for absorption correction. 
wR2(int) was 0.0578 before and 0.0524 after correction. 
The Ratio of minimum to maximum transmission is 0.7540. 
The \l/2 correction factor is Not present. 
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       tablet
_exptl_crystal_F_000             904
_exptl_crystal_id                cm58r
_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          0.198
_exptl_crystal_size_mid          0.151
_exptl_crystal_size_min          0.054
_refine_diff_density_max         1.077
_refine_diff_density_min         -2.188
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         7568
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0905P)^2^+7.5202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1482
_refine_ls_wR_factor_ref         0.1562
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6452
_reflns_number_total             7568
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b03071_si_001.cif
_cod_data_source_block           cm58rsa
_cod_depositor_comments
'Adding full bibliography for 4345651--4345656.cif.'
_cod_database_code               4345653
_shelx_estimated_absorpt_t_max   0.841
_shelx_estimated_absorpt_t_min   0.558
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups, {H1A,H1B} of C1, {H36A,H36B} of C36, {H35A,H35B} of C35, 
  {H9A,H9B} of C9, {H24A,H24B} of C24, {H21A,H21B} of C21, {H10A,H10B} of C10, 
  {H11A,H11B} of C11, {H25A,H25B} of C25, {H8A,H8B} of C8, {H20A,H20B} of C20, 
  {H12A,H12B} of C12, {H23A,H23B} of C23, {H13A,H13B} of C13, {H33A,H33B} of 
  C33, {H32A,H32B} of C32, {H22A,H22B} of C22, {H34A,H34B} of C34 
 At 1.5 times of: 
  All N(H) groups, {H1,H5} of C12 
2. Restrained distances 
 N6-H6 
 0.88 with sigma of 0.02 
 N5-H5 
 0.88 with sigma of 0.02 
 O1-H1 
 0.84 with sigma of 0.02 
3.a Ternary CH refined with riding coordinates: 
 C7(H7), C19(H19), C31(H31) 
3.b Secondary CH2 refined with riding coordinates: 
 C1(H1A,H1B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), 
 C12(H12A,H12B), C13(H13A,H13B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), 
  C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C32(H32A,H32B), C33(H33A, 
 H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B) 
3.c Aromatic/amide H refined with riding coordinates: 
 C4(H4), C6(H6A), C16(H16), C18(H18), C28(H28), C30(H30) 
;
_shelx_fab_checksum              94161
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'