A Class III asymmetric binuclear cyanido-bridged mixed-valence complex
Liu, Xiao-Lin; Li, Yi; Xu, Qing-Dou; Wei, Zi-Qin; Wu, Xin-Tao; Sheng, Tian-Lu; New Journal of Chemistry 46 (2022) 7922–7927; doi:10.1039/D2NJ00311B

data_7061411
_publ_section_title
;
 A Class III asymmetric binuclear cyanido-bridged mixed-valence complex
;
_journal_issue                   17
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7922
_journal_page_last               7927
_journal_paper_doi               10.1039/D2NJ00311B
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C57 H55 Cl N5 P2 Ru2, C H2 Cl2, 2(B F4)'
_chemical_formula_sum            'C58 H57 B2 Cl3 F8 N5 P2 Ru2'
_chemical_formula_weight         1368.13
_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             2022-03-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-03-23 deposited with the CCDC.	2022-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                86.830(3)
_cell_angle_beta                 78.341(3)
_cell_angle_gamma                62.157(4)
_cell_formula_units_Z            2
_cell_length_a                   12.2255(4)
_cell_length_b                   13.0636(5)
_cell_length_c                   21.7690(7)
_cell_measurement_reflns_used    27595
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      60.1750
_cell_measurement_theta_min      3.3180
_cell_volume                     3007.7(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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_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     59.00  85.00   0.50    0.05    --   72.28  57.00  90.00   52
  2  \w    101.00 144.00   0.50    0.05    --   72.28  57.00  90.00   86
  3  \w     93.00 118.00   0.50    0.05    --   72.28  57.00  60.00   50
  4  \w    116.00 142.00   0.50    0.05    --   72.28  57.00-150.00   52
  5  \w     73.00 110.00   0.50    0.05    --   72.28  57.00-150.00   74
  6  \w     88.00 113.00   0.50    0.05    --   72.28 122.00  84.00   50
  7  \w    110.00 141.00   0.50    0.05    --   72.28 150.00-113.00   62
  8  \w     70.00 106.00   0.50    0.05    --   72.28 150.00-113.00   72
  9  \w     83.00 142.00   0.50    0.05    --   72.28 125.00-150.00  118
 10  \w      0.00  25.00   0.50    0.05    --   72.28 -57.00-150.00   50
 11  \w     -1.00  35.00   0.50    0.05    --   72.28 -57.00-180.00   72
 12  \w     59.00  88.00   0.50    0.05    --   72.28 -57.00-150.00   58
 13  \w     77.00 103.00   0.50    0.05    --   72.28-150.00-158.00   52
 14  \w     75.00 107.00   0.50    0.05    --   72.28-125.00-120.00   64
 15  \w     20.00  93.00   0.50    0.05    --   72.28-122.00   3.00  146
 16  \w      2.00 105.00   0.50    0.05    --   72.28 -99.00  30.00  206
 17  \w    -16.00  47.00   0.50    0.05    --   -1.25  57.00  90.00  126
 18  \w    -87.00  -8.00   0.50    0.05    --  -74.78  57.00 -90.00  158
 19  \w    -98.00  -7.00   0.50    0.05    --  -74.78  77.00 -90.00  182
 20  \w   -127.00 -58.00   0.50    0.05    --  -74.78 150.00-113.00  138
 21  \w   -104.00 -42.00   0.50    0.05    --  -74.78 122.00  84.00  124
 22  \w    -77.00   2.00   0.50    0.05    --   -1.25 -19.00 -60.00  158
 23  \w    -54.00   6.00   0.50    0.05    --   -1.25 -57.00-120.00  120
 24  \w   -147.00 -53.00   0.50    0.05    --  -74.78 -77.00  30.00  188
 25  \w   -148.00 -60.00   0.50    0.05    --  -74.78 -57.00 150.00  176
 26  \w   -125.00 -98.00   0.50    0.05    --  -74.78-122.00   3.00   54
 27  \w   -147.00 -86.00   0.50    0.05    --  -74.78-125.00 -30.00  122
 28  \w   -105.00 -76.00   0.50    0.05    --  -74.78-150.00-158.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Synergy Custom(Liquid MetalJet D2+)'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0429276000
_diffrn_orient_matrix_UB_12      0.0269699000
_diffrn_orient_matrix_UB_13      0.0453231000
_diffrn_orient_matrix_UB_21      -0.0683990000
_diffrn_orient_matrix_UB_22      -0.0354712000
_diffrn_orient_matrix_UB_23      0.0431748000
_diffrn_orient_matrix_UB_31      0.0972793000
_diffrn_orient_matrix_UB_32      -0.1071591000
_diffrn_orient_matrix_UB_33      -0.0059592000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ga K\a'
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0967
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            39451
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         54.820
_diffrn_reflns_theta_min         3.609
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    4.271
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13851
_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 red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_description       block
_exptl_crystal_F_000             1382
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.129
_refine_diff_density_min         -1.321
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         11388
_refine_ls_number_restraints     1037
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0792
_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^)+(0.1694P)^2^+2.3884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2320
_refine_ls_wR_factor_ref         0.2379
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9675
_reflns_number_total             11388
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj00311b2.cif
_cod_data_source_block           sh-o
_cod_depositor_comments
'Adding full bibliography for 7061410--7061412.cif.'
_cod_database_code               7061411
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNPFRuCl
_chemical_oxdiff_usercomment     CHNPFRuCl
_shelx_estimated_absorpt_t_max   0.628
_shelx_estimated_absorpt_t_min   0.440
_reflns_odcompleteness_completeness 99.86
_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. Restrained distances
 F7-F5
 2.13 with sigma of 0.01
 F11-F10
 2.13 with sigma of 0.01
 B3-F12
 1.33 with sigma of 0.01
 F7-F8
 2.13 with sigma of 0.01
 F11-B3
 1.33 with sigma of 0.01
 F7-F6
 2.13 with sigma of 0.01
 F12-F10
 2.13 with sigma of 0.01
 F6-F5
 2.13 with sigma of 0.01
 F10-B3
 1.33 with sigma of 0.01
 F8-F6
 2.13 with sigma of 0.01
 F9-B3
 1.33 with sigma of 0.01
 B2-F8
 1.33 with sigma of 0.01
 F11-F12
 2.13 with sigma of 0.01
 B2-F7
 1.33 with sigma of 0.01
 F10-F9
 2.13 with sigma of 0.01
 B2-F5
 1.33 with sigma of 0.01
 B2-F6
 1.33 with sigma of 0.01
 F11-F9
 2.13 with sigma of 0.01
 F1-F2
 2.13 with sigma of 0.01
 F4-F3
 2.13 with sigma of 0.01
 F3-F4
 2.13 with sigma of 0.01
 F3-F1
 2.13 with sigma of 0.01
 F3-F2
 2.13 with sigma of 0.01
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 F10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
Uanis(B3) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F11)
\\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(B2) \\sim Ueq,
Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq: with sigma of 0.00001 and sigma for
terminal atoms of 0.00002
Uanis(F6) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F5) \\sim
Ueq, Uanis(B2) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(B3) \\sim Ueq, Uanis(F12)
\\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F9) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F9) \\sim
Ueq, Uanis(F10) \\sim Ueq, Uanis(B3) \\sim Ueq, Uanis(F12) \\sim Ueq,
Uanis(F11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F10) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
6. Others
 Fixed Sof: F5(0.5) B2(0.5) F7(0.5) F8(0.5) F10(0.5) F11(0.5) F12(0.5) F9(0.5)
 B3(0.5) F6(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C00M(H00A,H00B), C00N(H00C,H00D), C022(H02A,H02B)
7.b Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00T(H00T), C00X(H00X), C00Y(H00Y), C010(H010), C011(H011),
 C012(H012), C013(H013), C014(H014), C016(H016), C017(H017), C019(H019),
 C01A(H01G), C01B(H01H), C01C(H01I), C01D(H01J), C01E(H01K), C01F(H01L),
 C01G(H01M), C01H(H01N), C01I(H01O), C01J(H01P), C01K(H01Q), C01L(H01R),
 C01M(H01S), C01O(H01T), C01P(H01U), C01Q(H01V), C01R(H01W), C01S(H01X),
 C01T(H01Y), C01V(H01Z), C01W(H01), C01X(H1), C01Y(H2), C024(H024)
7.c Idealised Me refined as rotating group:
 C00Q(H00E,H00F,H00G), C00V(H00H,H00J,H00K), C00W(H00L,H00M,H00N), C015(H01A,
 H01B,H01C), C018(H01D,H01E,H01F)
;
_shelx_res_checksum              20644
_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 3.994
_oxdiff_exptl_absorpt_empirical_full_min 0.395