A T-shaped cyanidometal-bridged tetranuclear Fe3Ru complex with oxidation-driven intramolecular charge transfer between metal centres
Wang, Hao; Liu, Xiao-Lin; Liu, Han; Wu, Xin-Tao; Sheng, Tian-Lu; New Journal of Chemistry 49 (2025) 6595–6602; doi:10.1039/D5NJ00751H

data_7063697
_publ_section_title
;
 A T-shaped cyanidometal-bridged tetranuclear Fe3Ru complex with
 oxidation-driven intramolecular charge transfer between metal centres
;
_journal_issue                   16
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              6595
_journal_page_last               6602
_journal_paper_doi               10.1039/D5NJ00751H
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'C108 H103 Cl Fe3 N7 P6 Ru, 2(F6 P), C H2 Cl2'
_chemical_formula_sum            'C109 H105 Cl3 F12 Fe3 N7 P8 Ru'
_chemical_formula_weight         2363.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-03-13
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-03-13 deposited with the CCDC.	2025-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.2150(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5721(3)
_cell_length_b                   17.3121(2)
_cell_length_c                   35.2530(5)
_cell_measurement_reflns_used    30524
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      67.0240
_cell_measurement_theta_min      2.5430
_cell_volume                     10554.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.127a 64-bit (release 16-06-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.90 (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -66.00 -27.00   0.50    0.19    --  -97.00  61.00-180.00   78
  2  \w    -53.00 -26.00   0.50    0.19    --  -97.00  45.00-180.00   54
  3  \w    -72.00 -24.00   0.50    0.19    --  -97.00  61.00 -60.00   96
  4  \w    -53.00 -27.00   0.50    0.19    --  -97.00  45.00   0.00   52
  5  \w    -66.00 -28.00   0.50    0.19    --  -97.00  61.00  30.00   76
  6  \w    -54.00 -25.00   0.50    0.19    --  -97.00  45.00  90.00   58
  7  \w    -54.00 -25.00   0.50    0.19    --  -97.00  45.00 120.00   58
  8  \w    -54.00 -26.00   0.50    0.19    --  -97.00  45.00  60.00   56
  9  \w    -57.00  13.00   0.50    0.05    --  -46.22  86.00 -32.00  140
 10  \w   -116.00 -30.00   0.50    0.05    --  -46.22 -57.00 150.00  172
 11  \w    -70.00 -44.00   0.50    0.19    --  -97.00  86.00 -32.00   52
 12  \w    128.00 153.00   0.50    0.19    --  106.84  61.00 -90.00   50
 13  \w     91.00 116.00   0.50    0.19    --  106.84  61.00 -90.00   50
 14  \w     96.00 175.00   0.50    0.19    --  106.84  86.00 -32.00  158
 15  \w     37.00  67.00   0.50    0.19    --  106.84 -61.00  30.00   60
 16  \w     36.00  63.00   0.50    0.19    --  106.84 -61.00   0.00   54
 17  \w     34.00  66.00   0.50    0.19    --  106.84 -61.00-150.00   64
 18  \w     43.00  68.00   0.50    0.19    --  106.84 -61.00-180.00   50
 19  \w    -16.00  55.00   0.50    0.05    --   46.22 -86.00-149.00  142
 20  \w     63.00 135.00   0.50    0.19    --  106.84 -86.00-149.00  144
 21  \w    -44.00  28.00   0.50    0.05    --  -46.22  38.00  90.00  144
 22  \w   -138.00-112.00   0.50    0.19    --  -97.00 -30.00 -90.00   52
 23  \w   -108.00 -83.00   0.50    0.19    --  -97.00 -30.00 -90.00   50
 24  \w   -108.00 -83.00   0.50    0.19    --  -97.00 -45.00 -90.00   50
 25  \w   -166.00 -91.00   0.50    0.19    --  -97.00 -30.00-120.00  150
 26  \w   -157.00-117.00   0.50    0.19    --  -97.00 -45.00 -90.00   80
 27  \w   -152.00-126.00   0.50    0.19    --  -97.00 -86.00-149.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            74182
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.076
_diffrn_reflns_theta_max         67.076
_diffrn_reflns_theta_min         2.547
_exptl_absorpt_coefficient_mu    6.834
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20017
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.90 (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       block
_exptl_crystal_F_000             4836
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.882
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1461
_refine_ls_number_reflns         18785
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0798P)^2^+18.8261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1414
_refine_ls_wR_factor_ref         0.1477
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15866
_reflns_number_total             18785
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj00751h2.cif
_cod_data_source_block           wh-2
_cod_depositor_comments          'Adding full bibliography for 7063697.cif.'
_cod_database_code               7063697
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.548
_shelx_estimated_absorpt_t_min   0.548
_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. Rigid bond restraints
 C5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C6) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C03S) \\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C22) \\sim Ueq, Uanis(C03S) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C52) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl7) \\sim Ueq, Uanis(Cl3) \\sim Ueq, Uanis(Cl6) \\sim Ueq, Uanis(Cl5)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C035) \\sim Ueq, Uanis(C03T) \\sim Ueq, Uanis(C03J) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C040)=Sof(C7)=Sof(H7)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=Sof(C8)=Sof(H8)=
 Sof(C9)=Sof(H9)=Sof(P6A)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C54)=Sof(H54A)=
 Sof(H54B)=1-FVAR(1)
 Sof(P6B)=Sof(C03R)=Sof(H03G)=Sof(H03M)=Sof(C03W)=Sof(H03N)=Sof(H03R)=
 Sof(C03Z)=Sof(C03X)=Sof(H03X)=Sof(C042)=Sof(H042)=Sof(C046)=Sof(H046)=
 Sof(C041)=Sof(H041)=Sof(C03Y)=Sof(H03Y)=FVAR(1)
 Fixed Sof: C03K(0.5) H03K(0.5) C03P(0.5) H03P(0.5) C03Q(0.5) H03Q(0.5)
 C03U(0.5) H03U(0.5) C03V(0.5) H03V(0.5) Cl4(0.5) Cl2(0.5) C11(0.5) H11A(0.5)
 H11B(0.5) C12(0.5) H12(0.5) C15(0.5) H15(0.5) C19(0.5) H19(0.5) C27(0.5)
 H27(0.5) C79(0.5) H79(0.5) Cl5(0.25) Cl6(0.25) Cl7(0.25) Cl3(0.25) C44(0.25)
 H44A(0.25) H44B(0.25) C52(0.25) H52A(0.25) H52B(0.25)
6.a Ternary CH refined with riding coordinates:
 C03K(H03K), C03P(H03P)
6.b Secondary CH2 refined with riding coordinates:
 C01S(H01J,H01M), C01V(H01N,H01O), C023(H02A,H02B), C02P(H02H,H02I), C03R(H03G,
 H03M), C03W(H03N,H03R), C4(H4A,H4B), C11(H11A,H11B), C54(H54A,H54B), C44(H44A,
 H44B), C52(H52A,H52B)
6.c Aromatic/amide H refined with riding coordinates:
 C00S(H00S), C00U(H00U), C00X(H00X), C00Y(H00Y), C010(H010), C011(H011),
 C016(H016), C017(H017), C01A(H01A), C01C(H01C), C01D(H01D), C01E(H01E),
 C01G(H01H), C01I(H01I), C01K(H01K), C01L(H01L), C02V(H02V), C03C(H03C),
 C039(H039), C03S(H03S), C01Q(H01Q), C01R(H01R), C01T(H01T), C01U(H01U),
 C01W(H01W), C01X(H01X), C01Z(H01Z), C020(H020), C021(H021), C022(H022),
 C024(H024), C025(H025), C027(H027), C028(H028), C029(H029), C02B(H02C),
 C02D(H02D), C02E(H02E), C02F(H02F), C02G(H02G), C02J(H02J), C02K(H02K),
 C02L(H02L), C02N(H02N), C02O(H02O), C02Q(H02Q), C02S(H02S), C02X(H02Z),
 C02Z(H02), C030(H030), C032(H032), C033(H033), C034(H034), C035(H035),
 C036(H036), C037(H037), C038(H038), C03A(H03A), C03B(H03B), C03D(H03D),
 C03E(H03E), C03F(H03F), C03H(H03H), C03I(H03I), C03J(H03J), C03L(H03L),
 C03O(H03O), C03Q(H03Q), C03T(H03T), C03U(H03U), C03V(H03V), C03X(H03X),
 C042(H042), C046(H046), C041(H041), C03Y(H03Y), C7(H7), C5(H5), C6(H6), C8(H8),
  C9(H9), C12(H12), C15(H15), C19(H19), C27(H27), C79(H79), C22(H22)
6.d Fitted hexagon refined as free rotating group:
 C040(C7,C5,C6,C8,C9)
6.e Idealised Me refined as rotating group:
 C01F(H01B,H01F,H01G), C02T(H02M,H02P,H02R), C02U(H02T,H02U,H02W), C02W(H02X,
 H02Y,H)
;
_shelx_res_checksum              13254
_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
;