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_7710988
_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         'C88 H82 Fe2 N6 P4 Ru, 2(F6 P), 1.32(O)'
_chemical_formula_sum            'C88 H82 F12 Fe2 N6 O1.33 P6 Ru'
_chemical_formula_weight         1871.46
_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     iterative
_audit_creation_date             2022-04-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-04-28 deposited with the CCDC.	2022-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                95.91(3)
_cell_angle_beta                 99.87(2)
_cell_angle_gamma                108.389(17)
_cell_formula_units_Z            2
_cell_length_a                   11.874(4)
_cell_length_b                   15.236(5)
_cell_length_c                   31.642(12)
_cell_measurement_reflns_used    20311
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.3573
_cell_measurement_theta_min      1.6730
_cell_volume                     5276(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            52540
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         1.826
_exptl_absorpt_coefficient_mu    0.566
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'Dark red'
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_description       Flaky
_exptl_crystal_F_000             1913
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.238
_exptl_crystal_size_min          0.112
_refine_diff_density_max         2.610
_refine_diff_density_min         -1.204
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.918
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1023
_refine_ls_number_reflns         17179
_refine_ls_number_restraints     171
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.1235
_refine_ls_R_factor_gt           0.1114
_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^)+(0.2000P)^2^+20.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2891
_refine_ls_wR_factor_ref         0.3061
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14239
_reflns_number_total             17179
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01313d2.cif
_cod_data_source_block           a_pl_sq
_cod_database_code               7710988
_shelx_shelxl_version_number     2014/7
_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
 O2-C37
 2 with sigma of 0.01
 O1-C69
 2 with sigma of 0.01
 C67-O1
 2.2 with sigma of 0.01
 C69-O1
 2.2 with sigma of 0.01
 O1-C68
 2.2 with sigma of 0.01
 O2-C38
 2.2 with sigma of 0.01
3. Rigid bond restraints
 C40, C41
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C41, C42
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 P6, F7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C38) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C41)
\\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C44) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.04
Uanis(C41) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C75) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.04
Uanis(F7) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F12)
\\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F6) \\sim Ueq,
Uanis(F4) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(O1) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C37) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C39) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C42)
\\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C40) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C64) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C65)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C57) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Secondary CH2 refined with riding coordinates:
 C88(H88A,H88B), C87(H87A,H87B), C56(H56A,H56B), C57(H57A,H57B)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C24(H24), C78(H78), C67(H67), C66(H66), C65(H65), C64(H64),
 C69(H69), C84(H84), C83(H83), C10(H10), C9(H9), C5(H5), C3(H3), C17(H17),
 C15(H15), C49(H49), C86(H86), C19(H19), C22(H22), C54(H54), C53(H53), C52(H52),
  C37(H37), C35(H35), C34(H34), C33(H33), C38(H38), C7(H7), C29(H29), C76(H76),
 C45(H45), C62(H62), C63(H63), C50(H50), C47(H47), C21(H21), C55(H55), C58(H58),
  C31(H31), C32(H32), C27(H27), C51(H51), C59(H59), C28(H28), C72(H72),
 C71(H71), C70(H70), C75(H75), C85(H85), C82(H82), C80(H80), C60(H60), C77(H77),
  C74(H74), C81(H81), C41(H41), C43(H43), C44(H44), C39(H39), C40(H40), C46(H46)
5.c Fitted hexagon refined as free rotating group:
 C67(C68,C66,C65,C64,C69), C37(C36,C35,C34,C33,C38), C41(C42,C43,C44,C39,C40)
5.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C8(H8A,H8B,H8C), C20(H20A,H20B,H20C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              31450
_shelx_fab_checksum              95372
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'