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_7714285
_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, 4(B F4), 2(C2 H3 N)'
_chemical_formula_sum            'C92 H92 B4 F16 Fe2 N8 O4 P4 Ru'
_chemical_formula_weight         2057.62
_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     dual
_audit_creation_date             2022-06-23
_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                82.436(2)
_cell_angle_beta                 78.481(2)
_cell_angle_gamma                76.674(2)
_cell_formula_units_Z            2
_cell_length_a                   14.2053(3)
_cell_length_b                   15.3072(3)
_cell_length_c                   23.6959(6)
_cell_measurement_reflns_used    9230
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      58.9540
_cell_measurement_theta_min      2.8280
_cell_volume                     4892.96(19)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_Laue_measured_fraction_full 0.952
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            45646
_diffrn_reflns_point_group_measured_fraction_full 0.952
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        52.931
_diffrn_reflns_theta_max         52.931
_diffrn_reflns_theta_min         2.590
_exptl_absorpt_coefficient_mu    3.320
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       prism
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.745
_refine_diff_density_min         -0.929
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1174
_refine_ls_number_reflns         16470
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0692
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1130P)^2^+9.0617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1848
_refine_ls_wR_factor_ref         0.2045
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12514
_reflns_number_total             16470
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02208k2.cif
_cod_data_source_block           a_pl
_cod_original_cell_volume        4893.0(2)
_cod_database_code               7714285
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.733
_shelx_estimated_absorpt_t_min   0.733
_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-C76
 1.43 with sigma of 0.01
 B05T-F02S
 1.38 with sigma of 0.01
 B05T-F02P
 1.38 with sigma of 0.01
 B05T-F03Q
 1.38 with sigma of 0.01
 C76-C73
 2.26 with sigma of 0.01
 C73-C76
 2.25 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(F19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F02P) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F03Q) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F02S) \\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(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C73) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(B05T) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C73
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C39(H39A,H39B), C40(H40A,H40B)
5.b Aromatic/amide H refined with riding coordinates:
 C64(H64), C68(H68), C80(H80), C46(H46), C17(H17), C55(H55), C30(H30),
 C66(H66), C42(H42), C18(H18), C38(H38), C34(H34), C78(H78), C63(H63), C54(H54),
  C61(H61), C21(H21), C84(H84), C27(H27), C83(H83), C7(H7), C65(H65), C60(H60),
 C69(H69), C81(H81), C87(H87), C3(H3), C43(H43), C32(H32), C86(H86), C11(H11),
 C50(H50), C57(H57), C33(H33), C19(H19), C20(H20), C6(H6), C36(H36), C44(H44),
 C45(H45), C25(H25), C56(H56), C5(H5), C49(H49), C23(H23), C29(H29), C4(H4),
 C31(H31), C52(H52), C77(H77), C14(H14), C37(H37), C51(H51), C26(H26), C48(H48),
  C62(H62), C35(H35), C12(H12), C15(H15), C24(H24), C13(H13), C58(H58),
 C71(H71), C72(H72), C74(H74), C75(H75)
5.c Fitted hexagon refined as free rotating group:
 N4(C71,C72,C73,C74,C75)
5.d Idealised Me refined as rotating group:
 C82(H82A,H82B,H82C), C88(H88A,H88B,H88C), C70(H70A,H70B,H70C), C6AA(H6AA,H6AB,
 H6AC), C4AA(H4AA,H4AB,H4AC), C76(H76A,H76B,H76C)
;
_shelx_res_checksum              29105
_shelx_fab_checksum              51619
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'