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_7061410
_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         'C36 H39 N O P2 Ru, 2(B F4)'
_chemical_formula_sum            'C36 H39 B2 F8 N O P2 Ru'
_chemical_formula_weight         838.31
_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                84.1790(10)
_cell_angle_beta                 78.8260(10)
_cell_angle_gamma                73.611(2)
_cell_formula_units_Z            2
_cell_length_a                   8.87820(10)
_cell_length_b                   12.3726(2)
_cell_length_c                   18.0161(2)
_cell_measurement_reflns_used    19102
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      60.9650
_cell_measurement_theta_min      2.2370
_cell_volume                     1860.30(5)
_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 0.964
_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      2.00  70.00   0.50    0.10    --   74.23 -38.00 150.00  136
  2  \w    102.00 135.00   0.50    0.10    --   74.23 105.00 -88.00   66
  3  \w     70.00 135.00   0.50    0.10    --   74.23  19.00-120.00  130
  4  \w      9.00  62.00   0.50    0.10    --   74.23 -38.00-150.00  106
  5  \w      8.00  33.00   0.50    0.10    --   74.23 -57.00-150.00   50
  6  \w     41.00  89.00   0.50    0.10    --   74.23 -57.00-150.00   96
  7  \w    -73.00 -36.00   0.50    0.10    --  -74.85 105.00 -88.00   74
  8  \w   -110.00 -75.00   0.50    0.10    --  -74.85 125.00-150.00   70
  9  \w   -111.00 -85.00   0.50    0.10    --  -74.85 125.00  60.00   52
 10  \w    -68.00 -27.00   0.50    0.10    --  -74.85 125.00  60.00   82
 11  \w    -37.00 -11.00   0.50    0.10    --  -74.85  77.00 -60.00   52
 12  \w    -98.00 -18.00   0.50    0.10    --  -74.85  77.00  60.00  160
 13  \w    -87.00  -3.00   0.50    0.10    --  -74.85  57.00  60.00  168
 14  \w    -71.00  -6.00   0.50    0.10    --  -74.85  38.00  30.00  130
 15  \w    -41.00  -6.00   0.50    0.10    --  -74.85  19.00 120.00   70
 16  \w    -15.00  71.00   0.50    0.05    --   -0.31  57.00  90.00  172
 17  \w    -81.00 -55.00   0.50    0.10    --  -74.85  19.00 120.00   52
 18  \w    -96.00 -71.00   0.50    0.10    --  -74.85  77.00 -60.00   50
 19  \w      3.00  55.00   0.50    0.05    --   -0.31  38.00-180.00  104
 20  \w    -26.00  14.00   0.50    0.05    --   -0.31 -38.00 -60.00   80
 21  \w    -72.00 -31.00   0.50    0.05    --   -0.31 -38.00 -60.00   82
 22  \w   -143.00-118.00   0.50    0.10    --  -74.85 -99.00-120.00   50
 23  \w   -143.00 -89.00   0.50    0.10    --  -74.85 -99.00 -30.00  108
 24  \w   -141.00 -90.00   0.50    0.10    --  -74.85-105.00 170.00  102
 25  \w     45.00 107.00   0.50    0.10    --   74.23-105.00 170.00  124
 26  \w     49.00 104.00   0.50    0.10    --   74.23 -99.00 120.00  110
 27  \w      3.00  33.00   0.50    0.10    --   74.23 -99.00 120.00   60
 28  \w      1.00  84.00   0.50    0.10    --   74.23 -99.00-180.00  166
;
_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      0.1153606000
_diffrn_orient_matrix_UB_12      -0.0511045000
_diffrn_orient_matrix_UB_13      -0.0548226000
_diffrn_orient_matrix_UB_21      -0.1020297000
_diffrn_orient_matrix_UB_22      0.0294408000
_diffrn_orient_matrix_UB_23      -0.0490654000
_diffrn_orient_matrix_UB_31      0.0420268000
_diffrn_orient_matrix_UB_32      0.0963429000
_diffrn_orient_matrix_UB_33      -0.0185041000
_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  0.0367
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26128
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         61.136
_diffrn_reflns_theta_min         2.176
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    3.195
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64512
_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            'light orange'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_description       plate
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.713
_refine_diff_density_min         -0.980
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         8386
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0602
_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^)+(0.1137P)^2^+2.2430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1760
_refine_ls_wR_factor_ref         0.1826
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7560
_reflns_number_total             8386
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj00311b2.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 7061410--7061412.cif.'
_cod_database_code               7061410
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H B N P F Ru'
_chemical_oxdiff_usercomment     'C H B N P F Ru'
_shelx_estimated_absorpt_t_max   0.720
_shelx_estimated_absorpt_t_min   0.527
_reflns_odcompleteness_completeness 99.78
_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-B2
 1.33 with sigma of 0.01
 F4-F1
 2.13 with sigma of 0.01
 F1-F3
 2.13 with sigma of 0.01
 B2-F5
 1.33 with sigma of 0.01
 F2-F4
 2.13 with sigma of 0.01
 B1-F4
 1.33 with sigma of 0.01
 B2-F8
 1.33 with sigma of 0.01
 B2-F6
 1.33 with sigma of 0.01
 F2-F3
 2.13 with sigma of 0.01
 B1-F1
 1.33 with sigma of 0.01
 F3-F4
 2.13 with sigma of 0.01
 F8-F5
 2.13 with sigma of 0.01
 B1-F2
 1.33 with sigma of 0.01
 F8-F6
 2.13 with sigma of 0.01
 F2-F1
 2.13 with sigma of 0.01
 F8-F7
 2.13 with sigma of 0.01
 B1-F3
 1.33 with sigma of 0.01
 F5-F6
 2.13 with sigma of 0.01
 F5-F7
 2.13 with sigma of 0.01
3. Rigid bond restraints
 F1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 F8, B2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 B2, F6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 B2, F5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 B2, F7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(F1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F7) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F6) \\sim
Ueq, Uanis(F1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
5.a Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C35(H35A,H35B)
5.b Aromatic/amide H refined with riding coordinates:
 C28(H28), C33(H33), C26(H26), C27(H27), C24(H24), C31(H31), C13(H13),
 C25(H25), C16(H16), C29(H29), C32(H32), C15(H15), C11(H11), C18(H18), C20(H20),
  C34(H34), C14(H14), C22(H22), C19(H19), C21(H21)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C),
 C6(H6A,H6B,H6C)
;
_shelx_res_checksum              51011
_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 2.565
_oxdiff_exptl_absorpt_empirical_full_min 0.650