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_7714381
_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         'C46 H69 Fe2 N8 O7, 3(Cl O4) , 2(C2H3N)'
_chemical_formula_sum            'C50 H75 Cl3 Fe2 N10 O19'
_chemical_formula_weight         1338.25
_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
_audit_creation_date             2019-03-21
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2023-08-17 deposited with the CCDC.	2023-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                80.277(2)
_cell_angle_beta                 77.367(2)
_cell_angle_gamma                87.802(2)
_cell_formula_units_Z            2
_cell_length_a                   11.7251(4)
_cell_length_b                   13.1324(5)
_cell_length_c                   20.1201(7)
_cell_measurement_reflns_used    9859
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.33
_cell_measurement_theta_min      3.41
_cell_volume                     2979.64(19)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX3 v2016.5-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (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 0.996
_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  0.0347
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_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       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            47373
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.365
_diffrn_reflns_theta_min         2.281
_diffrn_source                   'I\mS Incoatec Microfocus Source '
_diffrn_source_type              'Bruker KAPPA APEX Duo'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.824
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5309
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.0806 before and 0.0479 after correction. The Ratio 
of minimum to maximum transmission is 0.7050. The \l/2 correction 
factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_description       plate
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.908
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         10879
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0744P)^2^+3.7801P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1324
_refine_ls_wR_factor_ref         0.1340
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10392
_reflns_number_total             10879
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02734a2.cif
_cod_data_source_block           g2617
_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               7714381
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.653
_shelx_estimated_absorpt_t_min   0.257
_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
 Cl3-O31 \\sim Cl3-O31A
 with sigma of 0.02
 Cl3-O34 \\sim Cl3-O34A
 with sigma of 0.02
 Cl1A-O11A \\sim Cl1-O11
 with sigma of 0.02
 Cl1-O14 \\sim Cl1A-O14A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O11A) = Uanis(O11)
4. Others
 Sof(O31A)=Sof(O34A)=1-FVAR(1)
 Sof(O31)=Sof(O34)=FVAR(1)
 Sof(Cl1A)=Sof(O14A)=Sof(O11A)=1-FVAR(2)
 Sof(Cl1)=Sof(O11)=Sof(O14)=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), C52(H52A,H52B,
 H52C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              54249
_shelx_fab_checksum              52355
_olex2_submission_special_instructions 'No special instructions were received'