Synthesis and structural and spectroscopic properties of a cyanido-bridged mixed-valence compound [Fe–NC–Ru–CN–Fe]
Liu, Ming; Xiong, Yan; Xu, Weixiu; Wang, Yong; New Journal of Chemistry 47 (2023) 6796–6803; doi:10.1039/D3NJ00049D

data_7062348
_publ_section_title
;
 Synthesis and structural and spectroscopic properties of a
 cyanido-bridged mixed-valence compound [Fe--NC--Ru--CN--Fe]
;
_journal_issue                   14
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              6796
_journal_page_last               6803
_journal_paper_doi               10.1039/D3NJ00049D
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety
'C84 H78 Fe2 N6 P4 Ru, 4(F3 P0.5), 7[H2O], 0.625[], 0.5[], 0.25[], 0.375[]'
_chemical_formula_sum            'C84 H92 F12 Fe2 N6 O7 P6 Ru'
_chemical_formula_weight         1924.22
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-02-17
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2023.02.15 svn.rb8c1d4dc for OlexSys, GUI svn.r6444)
;
_audit_update_record
;
2023-02-20 deposited with the CCDC.	2023-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.879(4)
_cell_length_b                   30.879(4)
_cell_length_c                   20.440(4)
_cell_measurement_reflns_used    31104
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5828
_cell_measurement_theta_min      2.1146
_cell_volume                     19490(5)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXL-2016/4 (Sheldrick, 2016)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  Saturn724+
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1013
_diffrn_reflns_av_unetI/netI     0.0765
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            123917
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.200
_exptl_absorpt_coefficient_mu    0.618
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8570
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'RIGAKU/MSC(2004),CrystalClear Version 1.3.6'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       prism
_exptl_crystal_F_000             7904
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.036
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1225
_refine_ls_number_reflns         17137
_refine_ls_number_restraints     575
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1365
_refine_ls_R_factor_gt           0.0758
_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^)+(0.1143P)^2^+48.3706P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1921
_refine_ls_wR_factor_ref         0.2522
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9921
_reflns_number_total             17137
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj00049d2.cif
_cod_data_source_block           ccdc2233237
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' 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 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7062344--7062348.cif.
;
_cod_original_cell_volume        19490(6)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               7062348
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{P7, P7A}
3. Restrained distances
 P7-F7 = P7-F8 = P7-F9 = P7-F10 = P7-F11 = P7-F12
 1.58 with sigma of 0.01
 F10-F11 = F7-F12 = F9-F8
 3.16 with sigma of 0.02
 F7-F9 = F7-F11 = F7-F8 = F7-F10 = F9-F11 = F9-F12 = F9-F10
 2.23 with sigma of 0.02
 F11-F12 = F11-F8
 2.23 with sigma of 0.02
 P6-F5 = P6-F6
 1.58 with sigma of 0.01
 P8-F13 = P8-F14 = P8-F15 = P8-F16 = P8-F17 = P8-F18
 1.58 with sigma of 0.01
 F15-F18 = F14-F17 = F13-F16
 3.16 with sigma of 0.02
 F13-F14 = F13-F15 = F13-F17 = F13-F18 = F14-F15 = F14-F16 = F14-F18
 2.23 with sigma of 0.02
 F15-F16 = F15-F17
 2.23 with sigma of 0.02
 P8A-F13A = P8A-F14A = P8A-F15A = P8A-F16A = P8A-F17A = P8A-F18A
 1.58 with sigma of 0.01
 F15A-F17A = F14A-F16A = F13A-F18A
 3.16 with sigma of 0.02
 F13A-F16A = F13A-F17A = F13A-F14A = F13A-F15A = F16A-F17A = F16A-F18A
 2.23 with sigma of 0.02
 F16A-F15A = F17A-F18A = F17A-F14A
 2.23 with sigma of 0.02
 P7A-F7A = P7A-F8A = P7A-F9A = P7A-F10A = P7A-F11A = P7A-F12A
 1.58 with sigma of 0.01
 F8A-F12A = F9A-F7A = F11A-F10A
 3.16 with sigma of 0.02
 F7A-F11A = F7A-F8A = F7A-F10A = F7A-F12A = F11A-F8A = F11A-F9A
 2.23 with sigma of 0.02
 F11A-F12A = F8A-F9A = F8A-F10A
 2.23 with sigma of 0.02
 P6A-F4A = P6A-F5A = P6A-F4AA = P6A-F5AA = P6A-F5AC = P6A-F5AB
 1.58 with sigma of 0.01
 F4A-F5AA = F5A-F4AA = F5AC-F5AB
 3.16 with sigma of 0.02
 F4A-F5A = F4A-F5AC = F4A-F4AA = F4A-F5AB = F5A-F5AC = F5A-F5AA = F5A-F5AB
 2.23 with sigma of 0.02
 F5AC-F5AA = F5AC-F4AA
 2.23 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33)
\\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C45) \\sim Ueq,
Uanis(C44) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C74) \\sim Ueq, Uanis(P8) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F14)
\\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(F17) \\sim Ueq,
Uanis(P6) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C46) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(F5AB) \\sim Ueq, Uanis(P6A) \\sim Ueq, Uanis(F4A) \\sim Ueq, Uanis(F5A)
\\sim Ueq, Uanis(F4AA) \\sim Ueq, Uanis(F5AA) \\sim Ueq, Uanis(F5AC) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(P7) = Uanis(P7A)
5. Rigid body (RIGU) restrains
 F13A, P8A, F14A, F15A, F16A, F17A, F18A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F15, P8, F13, F14, F16, F17, F18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F4AA, P6A, F4A, F5A, F5AA, F5AB, F5AC
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F5, P6, F4, F6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F8A, P7A, F7A, F9A, F10A, F11A, F12A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F7, P7, F8, F9, F10, F11, F12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: P6(0.125) F4(0.5) F5(0.125) F6(0.125) P6A(0.125) F4A(0.125)
 F5A(0.125) F4AA(0.125) F5AA(0.125) F5AB(0.125) F5AC(0.125) P7(0.5) F7(0.5)
 F8(0.5) F9(0.5) F10(0.5) F11(0.5) F12(0.5) P7A(0.5) F7A(0.5) F8A(0.5) F9A(0.5)
 F10A(0.5) F11A(0.5) F12A(0.5) P8(0.125) F13(0.125) F14(0.125) F15(0.125)
 F16(0.125) F17(0.125) F18(0.125) P8A(0.125) F13A(0.125) F14A(0.125)
 F15A(0.125) F16A(0.125) F17A(0.125) F18A(0.125)
7.a Ternary CH refined with riding coordinates:
 C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C54(H54), C55(H55),
 C56(H56), C57(H57), C58(H58)
7.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C59(H59A,H59B), C60(H60A,H60B)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19),
  C20(H20), C21(H21), C22(H22), C31(H31), C32(H32), C33(H33), C34(H34),
 C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C43(H43), C44(H44),
  C45(H45), C46(H46), C47(H47), C49(H49), C50(H50), C51(H51), C52(H52),
 C53(H53), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C68(H68), C69(H69),
  C70(H70), C71(H71), C72(H72), C74(H74), C75(H75), C76(H76), C77(H77),
 C78(H78), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84)
;
_shelx_res_checksum              53135
_shelx_fab_checksum              26811
_platon_squeeze_special_details
;
A solvent mask was calculated and 552 electrons were 
found in a volume of 3877\%A^3^ in 5 voids per unit cell. 
This is consistent with the presence of 7[H2O] per Formula Unit 
which account for 560 electrons per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'