Metal-to-metal electron transfer in a cyanido-bridged {Fe<sub>2</sub>Co<sub>2</sub>} square complex followed by X-ray diffraction and absorption techniques.
Mathonière, Corine; Mitcov, Dmitri; Koumousi, Evangelia; Amorin-Rosario, Daniel; Dechambenoit, Pierre; Fatima Jafri, Sadaf; Sainctavit, Philippe; Cartier Dit Moulin, Christophe; Toupet, Loic; Trzop, Elzbieta; Collet, Eric; Arrio, Marie-Anne; Rogalev, Andrei; Wilhelm, Fabrice; Clérac, Rodolphe; Chemical communications (Cambridge, England) 58 (2022) 12098–12101; doi:10.1039/d2cc04246k

data_7130756
_publ_section_title
;
 Metal-to-metal electron transfer in a cyanido-bridged
 {Fe<sub>2</sub>Co<sub>2</sub>} square complex followed by X-ray
 diffraction and absorption techniques.
;
_journal_issue                   86
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12098
_journal_page_last               12101
_journal_paper_doi               10.1039/d2cc04246k
_journal_volume                  58
_journal_year                    2022
_chemical_formula_moiety
'C42 H46 B Co Fe N13, C F3 O3 S, C3 H7 N O, 0.5(H2 O)'
_chemical_formula_sum            'C46 H54 B Co F3 Fe N14 O4.5 S'
_chemical_formula_weight         1089.68
_chemical_melting_point          ?
_chemical_properties_physical    Light-sensitive,Photo-sensitive
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-06-29 deposited with the CCDC.	2022-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                69.516(6)
_cell_angle_beta                 89.648(6)
_cell_angle_gamma                73.040(6)
_cell_formula_units_Z            2
_cell_length_a                   13.5817(9)
_cell_length_b                   14.0463(8)
_cell_length_c                   14.9259(10)
_cell_measurement_reflns_used    1657
_cell_measurement_temperature    240.0
_cell_measurement_theta_max      20.4300
_cell_measurement_theta_min      2.9940
_cell_volume                     2536.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.95a (Rigaku OD, 2021)'
_computing_data_collection
'CrysAlisPro 1.171.33.5 (Oxford Diffraction Ltd., 2008)'
_computing_data_reduction        'CrysAlisPro 1.171.41.95a (Rigaku OD, 2021)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      240.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1852
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -104.00 -32.00   1.00   60.00    --  -21.92 179.00-180.00   72
  2  \w    -48.00  51.00   1.00   60.00    --  -21.92  38.00-150.00   99
  3  \w    -24.00  16.00   1.00   60.00    --  -21.92 -88.00 164.00   40
  4  \w    -87.00   9.00   1.00   60.00    --  -21.92 -38.00  30.00   96
  5  \w    -83.00  11.00   1.00   60.00    --  -21.92 -77.00 -30.00   94
  6  \w     78.00 103.00   1.00   60.00    --   23.80 179.00-180.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0170297000
_diffrn_orient_matrix_UB_12      0.0531199000
_diffrn_orient_matrix_UB_13      -0.0339469000
_diffrn_orient_matrix_UB_21      0.0358793000
_diffrn_orient_matrix_UB_22      -0.0151008000
_diffrn_orient_matrix_UB_23      -0.0310587000
_diffrn_orient_matrix_UB_31      -0.0379251000
_diffrn_orient_matrix_UB_32      -0.0127694000
_diffrn_orient_matrix_UB_33      -0.0220506000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1010
_diffrn_reflns_av_unetI/netI     0.2301
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17159
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.786
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.723
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.95a (Rigaku Oxford Diffraction, 2021)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1130
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.027
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     734
_refine_ls_number_reflns         8913
_refine_ls_number_restraints     232
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.2168
_refine_ls_R_factor_gt           0.0802
_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^)+(0.0195P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1605
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3474
_reflns_number_total             8913
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04246k2.cif
_cod_data_source_block           mebipy240K
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7130756--7130758.cif.
;
_cod_original_formula_sum        'C46 H54 B Co F3 Fe N14 O4.50 S'
_cod_database_code               7130756
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C46 H54 B Co F3 Fe N14 O4.50 S'
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.20
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 F2-C46
 1.38 with sigma of 0.002
 F3-C46
 1.38 with sigma of 0.002
 F1-C46
 1.38 with sigma of 0.002
 S1-C46
 1.74 with sigma of 0.01
 F1A-C46A = F3A-C46A = F2A-C46A
 1.38 with sigma of 0.002
 S1A-C46A
 1.74 with sigma of 0.01
 F2-F3
 2.17 with sigma of 0.01
 S1-F2
 2.6 with sigma of 0.01
 O2-O4 \\sim O2A-O4A
 with sigma of 0.04
 F2-F3 \\sim F2A-F3A
 with sigma of 0.04
 O2-O3 \\sim O2A-O3A
 with sigma of 0.04
 O3-O4 \\sim O3A-O4A
 with sigma of 0.04
 F2-C46 \\sim F2A-C46A
 with sigma of 0.02
 F3-C46 \\sim F3A-C46A
 with sigma of 0.02
 O2-C46 \\sim O2A-C46A
 with sigma of 0.04
 O4-C46 \\sim O4A-C46A
 with sigma of 0.04
 O3-C46 \\sim O3A-C46A
 with sigma of 0.04
 F1-F2 \\sim F1A-F2A
 with sigma of 0.04
 F1-F3 \\sim F1A-F3A
 with sigma of 0.04
 F1-C46 \\sim F1A-C46A
 with sigma of 0.02
 S1-O2 \\sim S1A-O2A
 with sigma of 0.02
 S1-O4 \\sim S1A-O4A
 with sigma of 0.02
 S1-F2 \\sim S1A-F2A
 with sigma of 0.04
 S1-F3 \\sim S1A-F3A
 with sigma of 0.04
 S1-O3 \\sim S1A-O3A
 with sigma of 0.02
 S1-F1 \\sim S1A-F1A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C46A \\sim C46: within 1.7A with sigma of 0.005 and sigma for terminal atoms of
0.01
F1A \\sim F2A \\sim F3A: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
S1 \\sim S1A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C5) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C44)
\\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq,
Uanis(C34) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C38)
\\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C35) \\sim Ueq,
Uanis(C31) \\sim Ueq, Uanis(C42) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O4) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(C46) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O2A)
\\sim Ueq, Uanis(O3A) \\sim Ueq, Uanis(S1) \\sim Ueq, Uanis(F1) \\sim Ueq: with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C46A) \\sim Ueq, Uanis(F1A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(F3A) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(O4A) \\sim Ueq, Uanis(S1A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(F2A)=Sof(S1A)=Sof(O2A)=Sof(O3A)=Sof(O4A)=Sof(C46A)=Sof(F1A)=Sof(F3A)=1-
 FVAR(1)
 Sof(S1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(O2)=Sof(O3)=Sof(O4)=Sof(C46)=FVAR(1)
 Fixed Sof: O5(0.5) H5D(0.5) H5E(0.5)
5.a Riding coordinates:
 O5(H5D,H5E)
5.b Ternary CH refined with riding coordinates:
 B1(H1)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C13(H13), C19(H19), C20(H20), C22(H22), C26(H26), C28(H28),
 C29(H29), C31(H31), C32(H32), C34(H34), C38(H38), C40(H40), C41(H41), C43(H43)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C24(H24A,H24B,H24C), C30(H30A,H30B,
 H30C), C36(H36A,H36B,H36C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C45(H45A,
 H45B,H45C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.054
_oxdiff_exptl_absorpt_empirical_full_min 0.941