The investigation on electron transfer properties between metal centers in binuclear and trinuclear cyanido-bridged mixed valence complexes with cis/trans-configuration
xu, qingdou; Chen, Zeng; Su, Shaodong; He, Yong; Liu, Yang; Hu, Shengmin; Wu, Xintao; Sheng, Tianlu; Dalton Transactions  (2022) –; doi:10.1039/D2DT01313D

data_7710987
_publ_section_title
;
 The investigation on electron transfer properties between metal centers
 in binuclear and trinuclear cyanido-bridged mixed valence complexes with
 cis/trans-configuration
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01313D
_journal_year                    2022
_chemical_formula_moiety         'C88 H82 Fe2 N6 P4 Ru, 4(F6 P), C2 H3 N'
_chemical_formula_sum            'C90 H85 F24 Fe2 N7 P8 Ru'
_chemical_formula_weight         2181.17
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2022-04-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-04-24 deposited with the CCDC.	2022-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.1279(6)
_cell_length_b                   19.5282(4)
_cell_length_c                   36.8338(7)
_cell_measurement_reflns_used    22756
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      60.1180
_cell_measurement_theta_min      2.1180
_cell_volume                     20232.3(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.98a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.98a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.98a (Rigaku OD, 2021)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -41.00 -16.00   0.50    4.00    --   -1.25 -26.00  39.00   50
  2  \w    110.00 135.00   0.50   12.00    --   72.76 114.00  47.00   50
  3  \w   -147.00 -96.00   0.50   12.00    --  -75.26-102.00-141.00  102
  4  \w   -150.00 -72.00   0.50   12.00    --  -75.26 -26.00  39.00  156
  5  \w    -14.00  65.00   0.50    4.00    --   -1.25  57.00   0.00  158
  6  \w    -54.00  -2.00   0.50   12.00    --  -75.26  38.00 -30.00  104
  7  \w   -119.00 -94.00   0.50   12.00    --  -75.26 -99.00 -60.00   50
  8  \w   -113.00 -88.00   0.50   12.00    --  -75.26 -99.00-120.00   50
  9  \w   -104.00 -47.00   0.50   12.00    --  -75.26 125.00 -90.00  114
 10  \w    -51.00 -18.00   0.50   12.00    --  -75.26  38.00   0.00   66
;
_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      -0.0069900000
_diffrn_orient_matrix_UB_12      -0.0678583000
_diffrn_orient_matrix_UB_13      0.0003849000
_diffrn_orient_matrix_UB_21      0.0137388000
_diffrn_orient_matrix_UB_22      -0.0023006000
_diffrn_orient_matrix_UB_23      0.0348096000
_diffrn_orient_matrix_UB_31      -0.0450042000
_diffrn_orient_matrix_UB_32      0.0096412000
_diffrn_orient_matrix_UB_33      0.0105943000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0994
_diffrn_reflns_av_unetI/netI     0.0893
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            67536
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        48.134
_diffrn_reflns_theta_max         48.134
_diffrn_reflns_theta_min         2.086
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    3.604
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15326
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.98a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'Dark green'
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       Blocky
_exptl_crystal_F_000             8848
_exptl_crystal_size_max          0.367
_exptl_crystal_size_mid          0.356
_exptl_crystal_size_min          0.348
_refine_diff_density_max         2.016
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1194
_refine_ls_number_reflns         14530
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0622
_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^)+(0.0857P)^2^+28.0972P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1531
_refine_ls_wR_factor_ref         0.1715
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10075
_reflns_number_total             14530
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01313d2.cif
_cod_data_source_block           xqd-3
_cod_database_code               7710987
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N P F Cl Ru Fe'
_chemical_oxdiff_usercomment     'C H O N P F Cl Ru Fe'
_reflns_odcompleteness_completeness 99.90
_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(F14) \\sim Ueq, Uanis(F15) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F1)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C87(H87A,H87B), C88(H88A,H88B), C56(H56A,H56B), C57(H57A,H57B)
3.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C84(H84), C69(H69), C82(H82), C24(H24), C78(H78), C72(H72),
 C27(H27), C35(H35), C22(H22), C83(H83), C55(H55), C15(H15), C29(H29), C52(H52),
  C66(H66), C77(H77), C60(H60), C51(H51), C5(H5), C65(H65), C54(H54), C28(H28),
 C12(H12), C71(H71), C85(H85), C75(H75), C34(H34), C21(H21), C74(H74), C37(H37),
  C9(H9), C33(H33), C17(H17), C38(H38), C32(H32), C46(H46), C41(H41), C45(H45),
 C47(H47), C40(H40), C80(H80), C76(H76), C70(H70), C10(H10), C81(H81), C3(H3),
 C50(H50), C63(H63), C49(H49), C64(H64), C44(H44), C58(H58), C68(H68), C39(H39),
  C59(H59), C53(H53), C86(H86), C19(H19), C43(H43), C62(H62), C7(H7)
3.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C8(H8A,H8B,H8C), C26(H26A,H26B,H26C), C14(H14A,H14B,
 H14C), C89(H89A,H89B,H89C)
;
_shelx_res_checksum              83926
_shelx_fab_checksum              28115
_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 4.467
_oxdiff_exptl_absorpt_empirical_full_min 0.520