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_7714284
_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, 3(B F4), 4(C2 H3 N)'
_chemical_formula_sum            'C96 H98 B3 F12 Fe2 N10 O4 P4 Ru'
_chemical_formula_weight         2052.92
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-05
_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                90
_cell_angle_beta                 108.3240(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4029(2)
_cell_length_b                   36.5766(4)
_cell_length_c                   17.9000(2)
_cell_measurement_reflns_used    36824
_cell_measurement_temperature    99.98(13)
_cell_measurement_theta_max      59.9250
_cell_measurement_theta_min      2.4840
_cell_volume                     9573.3(2)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_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     71.00 105.00   0.50    0.08    --   76.11-125.00 -30.00   68
  2  \w     37.00  63.00   0.50    0.08    --   76.11 -92.00 -95.00   52
  3  \w     -1.00  70.00   0.50    0.08    --   76.11 -38.00 -90.00  142
  4  \w     85.00 149.00   0.50    0.08    --   76.11  92.00  17.00  128
  5  \w     -6.00  21.00   0.50    0.05    --   -0.94  92.00  17.00   54
  6  \w    -33.00  -7.00   0.50    0.05    --   -0.94  92.00  17.00   52
  7  \w    -71.00  -2.00   0.50    0.08    --  -77.99  38.00-180.00  138
  8  \w   -104.00 -27.00   0.50    0.08    --  -77.99  92.00  17.00  154
  9  \w    -22.00  70.00   0.50    0.05    --   -0.94  57.00 120.00  184
 10  \w      7.00  32.00   0.50    0.05    --   -0.94 -99.00-180.00   50
 11  \w    -17.00  13.00   0.50    0.05    --   -0.94 -92.00 -95.00   60
 12  \w   -155.00 -61.00   0.50    0.08    --  -77.99 -38.00 -60.00  188
 13  \w   -152.00 -88.00   0.50    0.08    --  -77.99 -99.00-120.00  128
 14  \w   -124.00 -79.00   0.50    0.08    --  -77.99-125.00-120.00   90
 15  \w   -118.00 -84.00   0.50    0.08    --  -77.99 -92.00 -95.00   68
 16  \w   -139.00-114.00   0.50    0.08    --  -77.99 -99.00  30.00   50
 17  \w   -138.00-105.00   0.50    0.08    --  -77.99 -99.00  60.00   66
 18  \w   -148.00-103.00   0.50    0.08    --  -77.99-125.00 150.00   90
;
_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      -0.0635209000
_diffrn_orient_matrix_UB_12      0.0261368000
_diffrn_orient_matrix_UB_13      -0.0247187000
_diffrn_orient_matrix_UB_21      -0.0462269000
_diffrn_orient_matrix_UB_22      -0.0212433000
_diffrn_orient_matrix_UB_23      -0.0602294000
_diffrn_orient_matrix_UB_31      -0.0471338000
_diffrn_orient_matrix_UB_32      -0.0143735000
_diffrn_orient_matrix_UB_33      0.0443326000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0762
_diffrn_reflns_av_unetI/netI     0.0608
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            73200
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.160
_diffrn_reflns_theta_min         2.100
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    3.293
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18013
_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_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       prism
_exptl_crystal_F_000             4220
_exptl_crystal_size_max          0.084
_exptl_crystal_size_mid          0.037
_exptl_crystal_size_min          0.019
_refine_diff_density_max         1.242
_refine_diff_density_min         -1.501
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1197
_refine_ls_number_reflns         21201
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0642
_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^)+(0.1067P)^2^+12.7092P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1662
_refine_ls_wR_factor_ref         0.1731
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17663
_reflns_number_total             21201
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02208k2.cif
_cod_data_source_block           tr133b0622_auto
_cod_database_code               7714284
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         ' Ru C H N O P F B Fe'
_chemical_oxdiff_usercomment     ' Ru C H N O P F B Fe'
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.769
_diffrn_oxdiff_digest_frames
;
01cb96d9b270a64a8e478b788b463ad3da01762e17c
;
_diffrn_oxdiff_digest_hkl
;
01b22407d002f456b13907bb3556b4522596a4
;
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     56.82
_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:
 C9(H9A,H9B), C40(H40A,H40B), C8(H8A,H8B), C39(H39A,H39B)
2.b Aromatic/amide H refined with riding coordinates:
 C34(H34), C33(H33), C15(H15), C52(H52), C29(H29), C77(H77), C72(H72),
 C42(H42), C35(H35), C74(H74), C65(H65), C36(H36), C86(H86), C71(H71), C75(H75),
  C84(H84), C48(H48), C23(H23), C24(H24), C5(H5), C87(H87), C69(H69), C37(H37),
 C46(H46), C83(H83), C43(H43), C27(H27), C11(H11), C68(H68), C44(H44), C78(H78),
  C17(H17), C45(H45), C6(H6), C49(H49), C66(H66), C81(H81), C60(H60), C30(H30),
 C80(H80), C54(H54), C38(H38), C51(H51), C3(H3), C25(H25), C21(H21), C61(H61),
 C7(H7), C50(H50), C4(H4), C14(H14), C26(H26), C63(H63), C20(H20), C64(H64),
 C55(H55), C19(H19), C31(H31), C62(H62), C58(H58), C32(H32), C18(H18), C12(H12),
  C13(H13), C56(H56), C57(H57)
2.c Idealised Me refined as rotating group:
 C76(H76A,H76B,H76C), C88(H88A,H88B,H88C), C82(H82A,H82B,H82C), C70(H70A,H70B,
 H70C), C90(H90A,H90B,H90C), C96(H96A,H96B,H96C), C92(H92A,H92B,H92C), C94(H94A,
 H94B,H94C)
;
_shelx_res_checksum              52682
_shelx_fab_checksum              22507
_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 2.219
_oxdiff_exptl_absorpt_empirical_full_min 0.501