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_7714283
_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         'C98 H106 Fe2 N6 O4 P4 Ru, 2(F6 P), C H2 Cl2'
_chemical_formula_sum            'C99 H108 Cl2 F12 Fe2 N6 O4 P6 Ru'
_chemical_formula_weight         2143.40
_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     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                90
_cell_angle_beta                 100.979(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7860(2)
_cell_length_b                   32.4422(4)
_cell_length_c                   25.3027(4)
_cell_measurement_reflns_used    37040
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      60.3390
_cell_measurement_theta_min      1.9970
_cell_volume                     11109.5(3)
_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_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     20.00  90.00   0.50    0.21    --   72.28-125.00-150.00  140
  2  \w     36.00  61.00   0.50    0.21    --   72.28 -26.00 -93.00   50
  3  \w     58.00 124.00   0.50    0.21    --   72.28  26.00  69.00  132
  4  \w    -72.00 -41.00   0.50    0.05    --   -1.25 -26.00 -93.00   62
  5  \w   -145.00 -94.00   0.50    0.21    --  -74.78 -99.00-150.00  102
  6  \w   -136.00 -60.00   0.50    0.21    --  -74.78 -26.00 -93.00  152
  7  \w    -49.00  14.00   0.50    0.05    --   -1.25 -38.00 120.00  126
  8  \w   -111.00 -26.00   0.50    0.21    --  -74.78 125.00  90.00  170
  9  \w    -61.00 -13.00   0.50    0.21    --  -74.78  57.00 150.00   96
 10  \w    -71.00 -18.00   0.50    0.21    --  -74.78  38.00 -60.00  106
 11  \w    -38.00  -2.00   0.50    0.21    --  -74.78  38.00-150.00   72
 12  \w    -71.00  -1.00   0.50    0.21    --  -74.78  38.00-120.00  140
 13  \w    -55.00 -29.00   0.50    0.21    --  -74.78  38.00 -90.00   52
 14  \w    -26.00  -1.00   0.50    0.21    --  -74.78  38.00 -90.00   50
 15  \w     22.00  70.00   0.50    0.05    --   -1.25  26.00  69.00   96
 16  \w    -60.00 -35.00   0.50    0.21    --  -74.78  26.00  69.00   50
;
_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      -0.0893456000
_diffrn_orient_matrix_UB_12      -0.0140239000
_diffrn_orient_matrix_UB_13      -0.0232406000
_diffrn_orient_matrix_UB_21      -0.0294661000
_diffrn_orient_matrix_UB_22      0.0021367000
_diffrn_orient_matrix_UB_23      0.0474067000
_diffrn_orient_matrix_UB_31      -0.0306494000
_diffrn_orient_matrix_UB_32      0.0387514000
_diffrn_orient_matrix_UB_33      -0.0110376000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            79138
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        52.931
_diffrn_reflns_theta_max         52.931
_diffrn_reflns_theta_min         1.948
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    3.300
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17847
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       block
_exptl_crystal_F_000             4416
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.868
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1203
_refine_ls_number_reflns         19597
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0967P)^2^+5.5508P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.1624
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15666
_reflns_number_total             19597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02208k2.cif
_cod_data_source_block           a_CCDC1
_cod_database_code               7714283
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Fe Ru C H N O Cl P F'
_chemical_oxdiff_usercomment     'Fe Ru C H N O Cl P F'
_shelx_estimated_absorpt_t_max   0.558
_shelx_estimated_absorpt_t_min   0.558
_diffrn_oxdiff_digest_frames
;
015a7788cefb01147b7c78ab439e73b41501596cdb6
;
_diffrn_oxdiff_digest_hkl
;
013b1c9201164861a8eb7370842bb5e2c51cf9
;
_reflns_odcompleteness_completeness 99.83
_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:
 C14(H14A,H14B), C50(H50A,H50B), C13(H13A,H13B), C49(H49A,H49B), C99(H99A,H99B)
2.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C82(H82), C90(H90), C70(H70), C94(H94), C79(H79), C75(H75),
 C23(H23), C58(H58), C64(H64), C76(H76), C93(H93), C81(H81), C88(H88), C96(H96),
  C34(H34), C26(H26), C62(H62), C84(H84), C59(H59), C78(H78), C87(H87),
 C24(H24), C61(H61), C60(H60), C91(H91), C68(H68), C85(H85), C97(H97), C25(H25),
  C20(H20), C56(H56), C38(H38), C65(H65), C28(H28), C52(H52), C32(H32),
 C29(H29), C35(H35), C16(H16), C66(H66), C67(H67), C74(H74), C37(H37), C71(H71),
  C72(H72), C73(H73), C30(H30), C19(H19), C36(H36), C31(H31), C17(H17),
 C54(H54), C55(H55), C18(H18), C53(H53)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C12(H12A,H12B,H12C), C11(H11A,H11B,
 H11C), C8(H8A,H8B,H8C), C47(H47A,H47B,H47C), C45(H45A,H45B,H45C), C46(H46A,
 H46B,H46C), C48(H48A,H48B,H48C), C86(H86A,H86B,H86C), C44(H44A,H44B,H44C),
 C98(H98A,H98B,H98C), C80(H80A,H80B,H80C), C92(H92A,H92B,H92C)
;
_shelx_res_checksum              92594
_shelx_fab_checksum              27132
_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 1.706
_oxdiff_exptl_absorpt_empirical_full_min 0.551