Direct and Remote Control on Electronic Structures and Redox Potentials in μ-Oxo Diferric Complexes
Finke, Sebastian; Stammler, Anja; Oldengott, Jan; Walleck, Stephan; Glaser, Thorsten; Dalton Transactions  (2023) –; doi:10.1039/D3DT02734A

data_7714379
_publ_section_title
;
 Direct and Remote Control on Electronic Structures and Redox Potentials
 in \m-Oxo Diferric Complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02734A
_journal_year                    2023
_chemical_formula_moiety         'C44 H66 Cl2 Fe2 N8 O5, 2(Cl O4)'
_chemical_formula_sum            'C44 H66 Cl4 Fe2 N8 O13'
_chemical_formula_weight         1168.54
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-09-22
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.06.10 svn.r3fa896fb for OlexSys, GUI svn.r6535)
;
_audit_update_record
;
2023-08-17 deposited with the CCDC.	2023-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                106.420(2)
_cell_angle_beta                 110.555(2)
_cell_angle_gamma                110.926(2)
_cell_formula_units_Z            2
_cell_length_a                   14.7196(5)
_cell_length_b                   14.9845(5)
_cell_length_c                   15.0801(5)
_cell_measurement_reflns_used    9065
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.285
_cell_measurement_theta_min      3.539
_cell_volume                     2572.90(18)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'APEX3 v2016.5-0 (Bruker AXS, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II area detector'
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker KAPPA APEX Duo'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'QuazarTM Montel multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            39569
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.763
_diffrn_reflns_theta_min         3.539
_diffrn_source                   'I\mS Incoatec microfocus source'
_diffrn_source_current           1.0
_diffrn_source_power             0.04968
_diffrn_source_type              'Bruker KAPPA APEX Duo'
_diffrn_source_voltage           49.68
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.019
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1068 before and 0.0664 after correction.
The Ratio of minimum to maximum transmission is 0.7286.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       plate
_exptl_crystal_F_000             1220
_exptl_crystal_preparation
'Crystal selected from oil dispersion and mounted via cryoloop.'
_exptl_crystal_recrystallization_method
'A solution of the complex in ... was filtered. Single-crystals were obtained by slow vapour diffusion of .... into this solution.'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     737
_refine_ls_number_reflns         9173
_refine_ls_number_restraints     176
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0319P)^2^+2.1133P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1038
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7387
_reflns_number_total             9173
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02734a2.cif
_cod_data_source_block           g2578
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_original_cell_volume        2572.90(16)
_cod_database_code               7714379
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.767
_shelx_estimated_absorpt_t_min   0.440
_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
 O31-O32 \\sim O31-O33 \\sim O31-O34 \\sim O32-O33 \\sim O32-O34 \\sim O33-O34
 with sigma of 0.04
 Cl4-O41 \\sim Cl4-O42 \\sim Cl4-O43 \\sim Cl4-O44 \\sim Cl4A-O41A \\sim
Cl4A-O42A \\sim Cl4A-O43A ~
 Cl4A-O44A
 with sigma of 0.02
 O41-O42 \\sim O41-O43 \\sim O41-O44 \\sim O42-O43 \\sim O42-O44 \\sim O43-O44
\\sim O41A-O42A \\sim O41A-
 O43A \\sim O41A-O44A \\sim O42A-O43A \\sim O42A-O44A \\sim O43A-O44A
 with sigma of 0.04
 Cl3-O31 \\sim Cl3-O32 \\sim Cl3-O33 \\sim Cl3-O34 \\sim Cl3A-O31A \\sim
Cl3A-O32A \\sim Cl3A-O33A ~
 Cl3A-O34
 with sigma of 0.02
 O31A-O32A \\sim O31A-O33A \\sim O31A-O34 \\sim O32A-O33A \\sim O32A-O34 \\sim
O33A-O34
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O31 \\sim O31A \\sim O44A \\sim O44 \\sim O42 \\sim O42A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Others
 Sof(Cl4A)=Sof(O41A)=Sof(O42A)=Sof(O43A)=Sof(O44A)=1-FVAR(1)
 Sof(Cl4)=Sof(O41)=Sof(O42)=Sof(O43)=Sof(O44)=FVAR(1)
 Sof(Cl3A)=Sof(O31A)=Sof(O32A)=Sof(O33A)=1-FVAR(2)
 Sof(Cl3)=Sof(O31)=Sof(O32)=Sof(O33)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C25(H25A,H25B), C41(H41A,
 H41B), C42(H42A,H42B), C43(H43A,H43B), C45(H45A,H45B), C65(H65A,H65B)
5.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C30(H30), C50(H50), C70(H70)
5.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,
 H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C),
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              86618
_olex2_submission_special_instructions 'No special instructions were received'