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_7714282
_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, C H2 Cl2, 4(B F4)'
_chemical_formula_sum            'C99 H108 B4 Cl2 F16 Fe2 N6 O4 P4 Ru'
_chemical_formula_weight         2200.70
_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             2023-03-30
_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                96.4022(9)
_cell_angle_beta                 101.3199(12)
_cell_angle_gamma                91.2395(12)
_cell_formula_units_Z            2
_cell_length_a                   12.8285(2)
_cell_length_b                   15.42782(19)
_cell_length_c                   28.5354(3)
_cell_measurement_reflns_used    30886
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      59.7830
_cell_measurement_theta_min      2.4950
_cell_volume                     5497.71(13)
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_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      99.9(3)
_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 0.999
_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    -75.00 -23.00   0.50    0.11    --   -1.41 -57.00 -43.00  104
  2  \w     -7.00  19.00   0.50    0.11    --   -1.41 -57.00 -43.00   52
  3  \w   -140.00 -57.00   0.50    0.44    --  -78.15 -57.00 -43.00  166
  4  \w   -111.00 -20.00   0.50    0.44    --  -78.15 125.00  90.00  182
  5  \w    -93.00 -36.00   0.50    0.44    --  -78.15 125.00 120.00  114
  6  \w    -44.00 -11.00   0.50    0.44    --  -78.15  77.00 150.00   66
  7  \w    -26.00  -1.00   0.50    0.44    --  -78.15  38.00 120.00   50
  8  \w    -55.00 -29.00   0.50    0.44    --  -78.15  38.00 120.00   52
  9  \w   -105.00 -56.00   0.50    0.44    --  -78.15  77.00 150.00   98
 10  \w    -88.00  -5.00   0.50    0.44    --  -78.15  57.00  97.00  166
 11  \w    -23.00  69.00   0.50    0.11    --   -1.41  57.00  97.00  184
 12  \w   -151.00 -89.00   0.50    0.44    --  -78.15 -99.00  90.00  124
 13  \w   -147.00-104.00   0.50    0.44    --  -78.15 -99.00 120.00   86
 14  \w   -131.00 -84.00   0.50    0.44    --  -78.15-125.00  90.00   94
 15  \w   -117.00 -88.00   0.50    0.44    --  -78.15 -99.00-120.00   58
 16  \w     -4.00  35.00   0.50    0.11    --   -1.41 -99.00 -30.00   78
 17  \w     -8.00  17.00   0.50    0.11    --   -1.41 -99.00-180.00   50
 18  \w     39.00  73.00   0.50    0.44    --   75.34 -77.00-180.00   68
 19  \w      1.00  29.00   0.50    0.44    --   75.34 -77.00-180.00   56
 20  \w     -2.00  71.00   0.50    0.44    --   75.34 -38.00 -30.00  146
 21  \w      4.00  30.00   0.50    0.44    --   75.34 -57.00 -43.00   52
 22  \w     21.00 102.00   0.50    0.44    --   75.34 -99.00 -60.00  162
 23  \w     61.00  99.00   0.50    0.44    --   75.34-125.00 -90.00   76
 24  \w     20.00 111.00   0.50    0.44    --   75.34-125.00 -60.00  182
 25  \w     57.00 110.00   0.50    0.44    --   75.34-125.00  90.00  106
 26  \w     69.00 148.00   0.50    0.44    --   75.34  57.00  97.00  158
 27  \w     80.00 146.00   0.50    0.44    --   75.34 125.00 120.00  132
 28  \w     83.00 108.00   0.50    0.44    --   75.34 125.00 -90.00   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      0.0274640000
_diffrn_orient_matrix_UB_12      0.0551356000
_diffrn_orient_matrix_UB_13      -0.0290440000
_diffrn_orient_matrix_UB_21      -0.1026860000
_diffrn_orient_matrix_UB_22      0.0156136000
_diffrn_orient_matrix_UB_23      -0.0151378000
_diffrn_orient_matrix_UB_31      0.0076499000
_diffrn_orient_matrix_UB_32      0.0660407000
_diffrn_orient_matrix_UB_33      0.0353621000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0928
_diffrn_reflns_av_unetI/netI     0.0809
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            62333
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        52.931
_diffrn_reflns_theta_max         52.931
_diffrn_reflns_theta_min         2.717
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    3.270
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_description       prism
_exptl_crystal_F_000             2260
_exptl_crystal_size_max          0.053
_exptl_crystal_size_mid          0.041
_exptl_crystal_size_min          0.027
_refine_diff_density_max         2.873
_refine_diff_density_min         -2.232
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1254
_refine_ls_number_reflns         19384
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1225
_refine_ls_R_factor_gt           0.1096
_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^)+(0.1758P)^2^+42.0636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2895
_refine_ls_wR_factor_ref         0.2998
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15902
_reflns_number_total             19384
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02208k2.cif
_cod_data_source_block           cp5iso-2o_auto
_cod_original_cell_volume        5497.70(13)
_cod_database_code               7714282
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         FeRuCHNOClPFB
_chemical_oxdiff_usercomment     FeRuCHNOClPFB
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.846
_diffrn_oxdiff_digest_frames
;
01e36da1e6845f7d469b00451af01506fe0291236f2
;
_diffrn_oxdiff_digest_hkl
;
019b729a5a007fb88864cc601d8026bdc0c6e4
;
_reflns_odcompleteness_completeness 99.92
_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. Uiso/Uaniso restraints and constraints
Uanis(B2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C42) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C13(H13A,H13B), C14(H14A,H14B), C50(H50A,H50B), C99(H99A,H99B)
3.b Me refined with riding coordinates:
 C48(H48A,H48B,H48C), C11(H11A,H11B,H11C), C92(H92A,H92B,H92C)
3.c Aromatic/amide H refined with riding coordinates:
 C58(H58), C87(H87), C88(H88), C81(H81), C91(H91), C82(H82), C90(H90),
 C56(H56), C97(H97), C25(H25), C22(H22), C94(H94), C93(H93), C28(H28), C96(H96),
  C76(H76), C75(H75), C68(H68), C78(H78), C59(H59), C84(H84), C74(H74),
 C85(H85), C29(H29), C31(H31), C24(H24), C23(H23), C16(H16), C55(H55), C73(H73),
  C62(H62), C26(H26), C79(H79), C20(H20), C38(H38), C54(H54), C52(H52),
 C67(H67), C32(H32), C70(H70), C19(H19), C72(H72), C60(H60), C66(H66), C61(H61),
  C64(H64), C53(H53), C37(H37), C17(H17), C18(H18), C30(H30), C71(H71),
 C35(H35), C65(H65), C34(H34), C36(H36)
3.d Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C98(H98A,H98B,H98C), C47(H47A,H47B,H47C), C10(H10A,H10B,
 H10C), C80(H80A,H80B,H80C), C46(H46A,H46B,H46C), C8(H8A,H8B,H8C), C9(H9A,H9B,
 H9C), C45(H45A,H45B,H45C), C86(H86A,H86B,H86C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              8837
_shelx_fab_checksum              48934
_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 2.452
_oxdiff_exptl_absorpt_empirical_full_min 0.464