Different delocalized range in mixed valence cyanidometal-bridged Fe-Ru-Fe complexes controlled by terminal ligand substitution modification
Chen, Zeng; xu, qingdou; Liu, Xiao-Lin; Hu, Shengmin; Wu, Xintao; Sheng, Tianlu; Dalton Transactions  (2023) –; doi:10.1039/D3DT02208K

data_7714281
_publ_section_title
;
 Different delocalized range in mixed valence cyanidometal-bridged
 Fe-Ru-Fe complexes controlled by terminal ligand substitution
 modification
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02208K
_journal_year                    2023
_chemical_formula_moiety         'C88 H86 Fe2 N6 O4 P4 Ru, 2(F6 P)'
_chemical_formula_sum            'C88 H84 F12 Fe2 N6 O4 P6 Ru'
_chemical_formula_weight         1916.20
_chemical_name_systematic        {[CpFe(dppe)CN]2Ru(MeO-py)4}[PF6]2
_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
_audit_creation_date             2023-03-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-06-29 deposited with the CCDC.	2023-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                89.65(3)
_cell_angle_beta                 71.93(2)
_cell_angle_gamma                67.437(16)
_cell_formula_units_Z            1
_cell_length_a                   11.366(4)
_cell_length_b                   13.418(6)
_cell_length_c                   15.982(6)
_cell_measurement_reflns_used    9041
_cell_measurement_temperature    293.1500
_cell_measurement_theta_max      36.1729
_cell_measurement_theta_min      1.6573
_cell_volume                     2122.1(15)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.991
_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  0.0422
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18534
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.189
_exptl_absorpt_coefficient_mu    0.707
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear brownish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       block
_exptl_crystal_F_000             980
_exptl_crystal_preparation       null
_exptl_crystal_recrystallization_method CH2Cl2-Et2O
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         7420
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0771
_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^)+(0.0259P)^2^+7.9125P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1544
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6203
_reflns_number_total             7420
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02208k2.cif
_cod_data_source_block           a
_cod_database_code               7714281
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.871
_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.a Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C31(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C21(H21), C5(H5), C9(H9), C30(H30), C20(H20), C6(H6),
 C22(H22), C24(H24), C23(H23), C18(H18), C15(H15), C36(H36), C11(H11), C14(H14),
  C44(H44), C16(H16), C27(H27), C17(H17), C38(H38), C29(H29), C26(H26),
 C42(H42), C28(H28), C41(H41), C40(H40), C43(H43), C37(H37), C34(H34), C35(H35)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              49166
_olex2_submission_special_instructions 'No special instructions were received'