The investigation on electron transfer properties between metal centers in binuclear and trinuclear cyanido-bridged mixed valence complexes with cis/trans-configuration
xu, qingdou; Chen, Zeng; Su, Shaodong; He, Yong; Liu, Yang; Hu, Shengmin; Wu, Xintao; Sheng, Tianlu; Dalton Transactions  (2022) –; doi:10.1039/D2DT01313D

data_7710986
_publ_section_title
;
 The investigation on electron transfer properties between metal centers
 in binuclear and trinuclear cyanido-bridged mixed valence complexes with
 cis/trans-configuration
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01313D
_journal_year                    2022
_chemical_formula_moiety         'C57 H53 Fe N6 P2 Ru, 2(F6 P), C4 H10 O'
_chemical_formula_sum            'C61 H63 F12 Fe N6 O P4 Ru'
_chemical_formula_weight         1404.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-04-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-04-24 deposited with the CCDC.	2022-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.0130(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.86160(10)
_cell_length_b                   41.2452(3)
_cell_length_c                   15.29680(10)
_cell_measurement_reflns_used    55094
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      60.3100
_cell_measurement_theta_min      1.9160
_cell_volume                     5916.92(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.967
_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     38.00  67.64   0.38    0.05    --   72.14 -46.00 -47.00   78
  2  \w      2.00  45.32   0.38    0.05    --   72.14 -38.00-150.00  114
  3  \w     58.00 141.22   0.38    0.05    --   72.14  46.00 102.00  219
  4  \w     85.00 142.00   0.38    0.05    --   72.14 125.00 120.00  150
  5  \w     27.00 111.36   0.38    0.05    --   72.14-125.00-180.00  222
  6  \w     61.00 108.50   0.38    0.05    --   72.14-125.00 -60.00  125
  7  \w     21.00  98.14   0.38    0.05    --   72.14-125.00 -30.00  203
  8  \w     14.00  88.86   0.38    0.05    --   72.14 -99.00 -30.00  197
  9  \w     68.00 109.80   0.38    0.05    --   72.14-125.00  90.00  110
 10  \w    -90.00  -5.64   0.38    0.05    --  -74.95  57.00 120.00  222
 11  \w    -78.00  -9.98   0.38    0.05    --  -74.95  46.00 102.00  179
 12  \w     -2.00  69.06   0.38    0.04    --   -1.41  46.00 102.00  187
 13  \w     -3.00  52.10   0.38    0.04    --   -1.41  38.00-120.00  145
 14  \w    -87.00 -58.88   0.38    0.05    --  -74.95  57.00 -90.00   74
 15  \w    -45.00 -11.94   0.38    0.05    --  -74.95  57.00 -90.00   87
 16  \w    -52.00  -2.98   0.38    0.05    --  -74.95  38.00 -90.00  129
 17  \w   -131.00 -65.26   0.38    0.05    --  -74.95 -46.00 -47.00  173
 18  \w   -147.00 -89.24   0.38    0.05    --  -74.95 -99.00-120.00  152
 19  \w   -145.00 -79.26   0.38    0.05    --  -74.95-125.00  60.00  173
 20  \w    -72.00 -11.96   0.38    0.04    --   -1.41 -46.00 -47.00  158
 21  \w    -72.00 -24.88   0.38    0.05    --  -74.95 125.00 120.00  124
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0928159000
_diffrn_orient_matrix_UB_12      -0.0163600000
_diffrn_orient_matrix_UB_13      -0.0683154000
_diffrn_orient_matrix_UB_21      -0.0731857000
_diffrn_orient_matrix_UB_22      -0.0085514000
_diffrn_orient_matrix_UB_23      0.0570218000
_diffrn_orient_matrix_UB_31      -0.0801260000
_diffrn_orient_matrix_UB_32      0.0267061000
_diffrn_orient_matrix_UB_33      -0.0236162000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            75045
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.405
_diffrn_reflns_theta_min         2.800
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    3.917
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32475
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'Dark brown'
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_description       Blocky
_exptl_crystal_F_000             2868
_exptl_crystal_size_max          0.384
_exptl_crystal_size_mid          0.367
_exptl_crystal_size_min          0.346
_refine_diff_density_max         1.641
_refine_diff_density_min         -1.683
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     781
_refine_ls_number_reflns         13076
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0597P)^2^+10.8484P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12622
_reflns_number_total             13076
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 68.1396\% 
around [0.07 -0.98 -0.20] (reciprocal) or [0.28 -0.56 -0.78] (direct)
;
_cod_data_source_file            d2dt01313d2.cif
_cod_data_source_block           xqd-1_twin1_hklf4
_cod_database_code               7710986
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N P F Cl Ru Fe'
_chemical_oxdiff_usercomment     'C H O N P F Cl Ru Fe'
_diffrn_oxdiff_digest_frames
;
01456881e2c59e18b28ce64db31771a2a303221b132
;
_diffrn_oxdiff_digest_hkl
;
0104f864e9f54b76795ed04338dcb9eb42f7cd
;
_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
 C51, C52
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C55) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C59) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C51) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C54)
\\sim Ueq, Uanis(C53) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C56(H56a,H56b), C57(H57a,H57b), C59(H59a,H59b), C60(H60a,H60b)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C12(H12), C32(H32), C24(H24), C31(H31), C41(H41), C29(H29), C17(H17),
 C47(H47), C49(H49), C55(H55), C37(H37), C19(H19), C7(H7), C54(H54), C43(H43),
 C51(H51), C52(H52), C50(H50), C10(H10), C15(H15), C53(H53), C3(H3), C27(H27),
 C21(H21), C45(H45), C28(H28), C9(H9), C40(H40), C46(H46), C38(H38), C22(H22),
 C44(H44), C33(H33), C35(H35), C39(H39), C34(H34)
4.c Idealised Me refined as rotating group:
 C26(H26a,H26b,H26c), C20(H20a,H20b,H20c), C8(H8a,H8b,H8c), C14(H14a,H14b,
 H14c), C61(H61a,H61b,H61c), C58(H58a,H58b,H58c)
;
_shelx_res_checksum              83445
_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 2.472
_oxdiff_exptl_absorpt_empirical_full_min 0.460
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2