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_7714380
_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 H68 Fe2 N8 O7, 2(Cl O4), 2(C3 H8 O)'
_chemical_formula_sum            'C50 H84 Cl2 Fe2 N8 O17'
_chemical_formula_weight         1251.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-01-12
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2023-08-17 deposited with the CCDC.	2023-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.7610(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.2522(9)
_cell_length_b                   15.5311(5)
_cell_length_c                   16.9805(5)
_cell_measurement_reflns_used    9071
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.216
_cell_measurement_theta_min      3.477
_cell_volume                     5838.1(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX3 v2016.5-0 (Bruker AXS, 2016)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/1 (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 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.0324
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            51018
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.346
_diffrn_reflns_theta_min         3.476
_diffrn_source                   'I\mS Incoatec Microfocus Source'
_diffrn_source_current           1.0
_diffrn_source_power             0.04971
_diffrn_source_type              'Bruker KAPPA APEX Duo'
_diffrn_source_voltage           49.71
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.453
_exptl_absorpt_correction_T_max  0.7532
_exptl_absorpt_correction_T_min  0.5347
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0716 before and 0.0470 after correction.
The Ratio of minimum to maximum transmission is 0.7099.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       column
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         5427
_refine_ls_number_restraints     305
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+6.2987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0806
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5297
_reflns_number_total             5427
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02734a2.cif
_cod_data_source_block           g2725
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_database_code               7714380
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.538
_shelx_estimated_absorpt_t_min   0.283
_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 O(H) groups
2. Restrained distances
 Cl1-O14 \\sim Cl1A-O13A \\sim Cl1-O13 \\sim Cl1A-O11A \\sim Cl1-O11 \\sim
Cl1-O12 \\sim Cl1A-O12 ~
 Cl1A-O14A \\sim Cl1B-O14B \\sim Cl1B-O11B \\sim Cl1B-O12B \\sim Cl1B-O13B
 with sigma of 0.02
 O11B-O14B \\sim O13B-O12B \\sim O11B-O12B \\sim O11B-O13B \\sim O14B-O12B
\\sim O14B-O13B
 with sigma of 0.02
 O1SB-C2SB \\sim O1S-C2S
 with sigma of 0.02
 C2SB-C3SB \\sim C3S-C2S
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1A \\sim Cl1 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O11A \\sim O13A
\\sim O14A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
Cl1B \\sim O14B \\sim O11B \\sim O12B \\sim O13B: within 2A with sigma of 0.02
and sigma for terminal atoms of 0.04 within 2A
Uanis(O12B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O1S) = Uanis(O1SB)
Uanis(C2SB) = Uanis(C2S)
Uanis(C1SB) = Uanis(C1S)
Uanis(C3S) = Uanis(C3SB)
4. Rigid body (RIGU) restrains
 Cl1B, O14B, O11B, O12B, O13B, Cl1, O11, O12, O13, O14, Cl1A, O11A, O13A, O14A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O1SB)=Sof(H1SB)=Sof(C1SB)=Sof(H1SA)=Sof(H1SC)=Sof(H1SD)=Sof(C2SB)=
 Sof(H2SB)=Sof(C3SB)=Sof(H3SA)=Sof(H3SB)=Sof(H3SC)=1-FVAR(1)
 Sof(O1S)=Sof(H1S)=Sof(C1S)=Sof(H1SE)=Sof(H1SF)=Sof(H1SG)=Sof(C2S)=Sof(H2S)=
 Sof(C3S)=Sof(H3SD)=Sof(H3SE)=Sof(H3SF)=FVAR(1)
 Fixed Sof: Cl1(0.65) O11(0.65) O12(0.95) O13(0.65) O14(0.65) Cl1A(0.3)
 O11A(0.3) O13A(0.3) O14A(0.3) Cl1B(0.05) O14B(0.05) O11B(0.05) O12B(0.05)
 O13B(0.05)
6.a Ternary CH refined with riding coordinates:
 C2SB(H2SB), C2S(H2S)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C25(H25A,H25B)
6.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C30(H30)
6.d 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),
 C1SB(H1SA,H1SC,H1SD), C3SB(H3SA,H3SB,H3SC), C1S(H1SE,H1SF,H1SG), C3S(H3SD,H3SE,
 H3SF)
6.e Idealised tetrahedral OH refined with riding coordinates:
 O1SB(H1SB)
6.f Idealised tetrahedral OH refined as rotating group:
 O1S(H1S)
;
_shelx_res_checksum              63793
_olex2_submission_special_instructions 'No special instructions were received'