Syntheses, crystal structures and MMCT properties of diruthenium-based cyanido-bridged RuV/VI2-NC-Ru<sup>II</sup> complexes.
Li, Ting-Ya; Su, Shao-Dong; He, Yong; Wu, Xin-Tao; Sheng, Tian-Lu; Dalton transactions (Cambridge, England : 2003) 53 (2024) 5010–5019; doi:10.1039/d3dt01861j

data_7714990
_publ_section_title
;
 Syntheses, crystal structures and MMCT properties of diruthenium-based
 cyanido-bridged RuV/VI2-NC-Ru<sup>II</sup> complexes.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5010
_journal_page_last               5019
_journal_paper_doi               10.1039/d3dt01861j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C71 H67 N7 O2 P2 Ru3, F6 P'
_chemical_formula_sum            'C71 H67 F6 N7 O2 P3 Ru3'
_chemical_formula_weight         1560.43
_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
_audit_block_doi                 10.5517/ccdc.csd.cc2c39jb
_audit_creation_date             2022-06-08
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-06-08 deposited with the CCDC.	2024-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                75.6150(19)
_cell_angle_beta                 81.7459(19)
_cell_angle_gamma                86.5897(19)
_cell_formula_units_Z            2
_cell_length_a                   10.9565(3)
_cell_length_b                   15.0440(3)
_cell_length_c                   22.5663(4)
_cell_measurement_reflns_used    26911
_cell_measurement_temperature    300.01(14)
_cell_measurement_theta_max      60.2700
_cell_measurement_theta_min      2.6330
_cell_volume                     3564.55(14)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      300.01(14)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.944
_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     81.00 144.00   0.50    0.20    --   72.28  84.00 -26.00  126
  2  \w     56.00 121.00   0.50    0.20    --   72.28  57.00 -90.00  130
  3  \w     86.00 114.00   0.50    0.20    --   72.28  57.00-120.00   56
  4  \w     -1.00  68.00   0.50    0.20    --   72.28 -38.00  60.00  138
  5  \w     -1.00  71.00   0.50    0.20    --   72.28 -38.00  30.00  144
  6  \w      2.00  71.00   0.50    0.20    --   72.28 -38.00 -90.00  138
  7  \w     35.00  84.00   0.50    0.20    --   72.28 -57.00 -90.00   98
  8  \w     24.00  65.00   0.50    0.20    --   72.28 -84.00-146.00   82
  9  \w     66.00  92.00   0.50    0.20    --   72.28-125.00-180.00   52
 10  \w     21.00  51.00   0.50    0.20    --   72.28-125.00-180.00   60
 11  \w     24.00 107.00   0.50    0.20    --   72.28-125.00   0.00  166
 12  \w     85.00 111.00   0.50    0.20    --   72.28-125.00  60.00   52
 13  \w      0.00 106.00   0.50    0.20    --   72.28 -99.00  60.00  212
 14  \w    -30.00  -5.00   0.50    0.10    --   -1.25 -84.00-146.00   50
 15  \w    -74.00   8.00   0.50    0.10    --   -1.25 -38.00-150.00  164
 16  \w   -148.00 -86.00   0.50    0.20    --  -74.78-125.00  30.00  124
 17  \w   -148.00 -79.00   0.50    0.20    --  -74.78-125.00  90.00  138
 18  \w   -136.00-101.00   0.50    0.20    --  -74.78 -99.00 120.00   70
 19  \w    -58.00  13.00   0.50    0.10    --   -1.25 -57.00 150.00  142
 20  \w   -142.00-108.00   0.50    0.20    --  -74.78 -99.00   0.00   68
 21  \w   -146.00 -81.00   0.50    0.20    --  -74.78 -84.00-146.00  130
 22  \w    -83.00 -35.00   0.50    0.20    --  -74.78  77.00 -90.00   96
 23  \w    -80.00 -27.00   0.50    0.20    --  -74.78 125.00 -30.00  106
 24  \w    -68.00 -42.00   0.50    0.20    --  -74.78  84.00 -26.00   52
 25  \w   -108.00 -21.00   0.50    0.20    --  -74.78 125.00 120.00  174
 26  \w    -26.00  38.00   0.50    0.10    --   -1.25  84.00 -26.00  128
;
_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      0.0349832000
_diffrn_orient_matrix_UB_12      -0.0853096000
_diffrn_orient_matrix_UB_13      -0.0041355000
_diffrn_orient_matrix_UB_21      0.0433021000
_diffrn_orient_matrix_UB_22      -0.0154521000
_diffrn_orient_matrix_UB_23      0.0543104000
_diffrn_orient_matrix_UB_31      -0.1102942000
_diffrn_orient_matrix_UB_32      -0.0305666000
_diffrn_orient_matrix_UB_33      0.0292334000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'micro-focus metaljet'
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            51281
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         61.498
_diffrn_reflns_theta_min         2.637
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    4.211
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63040
_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_density_diffrn    1.454
_exptl_crystal_F_000             1578
_refine_diff_density_max         2.885
_refine_diff_density_min         -1.505
_refine_diff_density_rms         0.153
_refine_ls_extinction_coef       0.00099(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     805
_refine_ls_number_reflns         15887
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      Infinity
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0676
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1446P)^2^+7.1273P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2068
_refine_ls_wR_factor_ref         0.2248
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12932
_reflns_number_total             15887
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01861j2.cif
_cod_data_source_block           cp1ru-ru2_auto
_cod_depositor_comments
'Adding full bibliography for 7714990--7714997.cif.'
_cod_database_code               7714990
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C N O P F Ru H Cl'
_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
 F6-F2
 2.23 with sigma of 0.1
 F4-F6
 2.23 with sigma of 0.1
 F2-F4
 2.23 with sigma of 0.1
 F3-P3
 1.58 with sigma of 0.1
 F3-F2
 2.23 with sigma of 0.1
 F5-F4
 2.23 with sigma of 0.1
 F6-F4
 2.23 with sigma of 0.1
 F4-F5
 2.23 with sigma of 0.01
 F4-F2
 2.23 with sigma of 0.01
 F2-F3
 2.23 with sigma of 0.01
 F3-F5
 2.23 with sigma of 0.01
 F6-F3
 2.23 with sigma of 0.01
 F1-F3
 2.23 with sigma of 0.01
 P3-F2
 1.58 with sigma of 0.01
 P3-F4
 1.58 with sigma of 0
 P3-F3
 1.58 with sigma of 0.01
 P3-F1
 1.58 with sigma of 0.01
 P3-F4 = P3-F3
 1.58 with sigma of 0.01
 P3-F6
 1.58 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(F4) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F2) \\sim
Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(F4) = Uanis(F2) = Uanis(F1) = Uanis(F6)
Uanis(F1) = Uanis(F4) = Uanis(F5) = Uanis(F3) = Uanis(F2) = Uanis(F6)
Uanis(F4) = Uanis(F5) = Uanis(F6) = Uanis(F3) = Uanis(F2) = Uanis(F1)
Uanis(F6) = Uanis(F5) = Uanis(F4) = Uanis(F3) = Uanis(F2) = Uanis(F1)
4.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C11(H11A,H11B)
4.b Aromatic/amide H refined with riding coordinates:
 C45(H45), C74(H74), C44(H44), C57(H57), C86(H86), C60(H60), C58(H58),
 C42(H42), C30(H30), C67(H67), C81(H81), C53(H53), C71(H71), C29(H29), C28(H28),
  C24(H24), C26(H26), C77(H77), C88(H88), C9(H9), C89(H89), C87(H87), C72(H72),
 C63(H63), C66(H66), C18(H18), C20(H20), C49(H49), C15(H15), C5(H5), C79(H79),
 C23(H23), C52(H52), C80(H80), C7(H7), C22(H22), C8(H8), C27(H27), C65(H65),
 C50(H50), C51(H51), C78(H78), C6(H6), C17(H17), C16(H16), C21(H21), C64(H64),
 C(H)
4.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C54(H54A,H54B,H54C), C82(H82A,H82B,H82C), C68(H68A,H68B,
 H68C), C90(H90A,H90B,H90C)
;
_shelx_res_checksum              84323
_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 2.114
_oxdiff_exptl_absorpt_empirical_full_min 0.523