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_7714997
_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         'C75 H75 N7 O2 P2 Ru3, 2(F6 P)'
_chemical_formula_sum            'C75 H75 F12 N7 O2 P4 Ru3'
_chemical_formula_weight         1761.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2c3993
_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                90
_cell_angle_beta                 99.9850(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   61.4094(4)
_cell_length_b                   11.13090(10)
_cell_length_c                   26.7856(2)
_cell_measurement_reflns_used    40731
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      60.3400
_cell_measurement_theta_min      2.1140
_cell_volume                     18031.8(2)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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     50.00 137.00   0.25    0.40    --   72.28  77.00  30.00  348
  2  \w     41.00  74.00   0.25    0.40    --   72.28 -23.00 136.00  132
  3  \w     -3.00  25.00   0.25    0.40    --   72.28 -23.00 136.00  112
  4  \w     80.00 132.00   0.25    0.40    --   72.28  23.00 -58.00  208
  5  \w    103.00 139.00   0.25    0.40    --   72.28 125.00-180.00  144
  6  \w     43.00  75.00   0.25    0.10    --   -1.25  23.00 -58.00  128
  7  \w    -27.00  -2.00   0.25    0.40    --  -74.78  57.00   0.00  100
  8  \w    -88.00 -41.00   0.25    0.40    --  -74.78  57.00   0.00  188
  9  \w    -17.00  34.00   0.25    0.10    --   -1.25  57.00 -90.00  204
 10  \w    -75.00 -24.00   0.25    0.40    --  -74.78  23.00 -58.00  204
 11  \w    -84.00 -40.00   0.25    0.40    --  -74.78  57.00  30.00  176
 12  \w    -98.00  -2.00   0.25    0.40    --  -74.78  77.00  60.00  384
 13  \w    -32.00  -6.00   0.25    0.40    --  -74.78  57.00  30.00  104
 14  \w    -73.00 -14.00   0.25    0.10    --   -1.25 -23.00 136.00  236
 15  \w   -148.00 -60.00   0.25    0.40    --  -74.78 -23.00 136.00  352
 16  \w   -137.00-112.00   0.25    0.40    --  -74.78 -99.00-150.00  100
;
_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      -0.0177719000
_diffrn_orient_matrix_UB_12      0.0278492000
_diffrn_orient_matrix_UB_13      0.0204208000
_diffrn_orient_matrix_UB_21      0.0131016000
_diffrn_orient_matrix_UB_22      0.0231846000
_diffrn_orient_matrix_UB_23      0.0443366000
_diffrn_orient_matrix_UB_31      0.0016719000
_diffrn_orient_matrix_UB_32      0.1147483000
_diffrn_orient_matrix_UB_33      -0.0139140000
_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  0.0259
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       73
_diffrn_reflns_limit_h_min       -73
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            61911
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         53.854
_diffrn_reflns_theta_min         2.969
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    3.482
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61625
_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_density_diffrn    1.298
_exptl_crystal_F_000             7120
_refine_diff_density_max         1.121
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     797
_refine_ls_number_reflns         16473
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0577
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1046P)^2^+36.2977P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1768
_refine_ls_wR_factor_ref         0.1805
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14448
_reflns_number_total             16473
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01861j2.cif
_cod_data_source_block           a_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7714990--7714997.cif.'
_cod_database_code               7714997
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C N O P F Ru H'
_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 planarity
 C6, C1AA, C2, C3, C4, C5
 with sigma of 0.1
 C023, C12, C17, C9, C0AA, C02J
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Uanis(C6) = Uanis(C5) = Uanis(C4) = Uanis(C3) = Uanis(C2) = Uanis(C1AA)
Uanis(C023) = Uanis(C12) = Uanis(C17) = Uanis(C9) = Uanis(C0AA) = Uanis(C02J)
Uanis(C01S) = Uanis(C026) = Uanis(C02I) = Uanis(C02B) = Uanis(C02E)
Uanis(C027) = Uanis(C02G) = Uanis(C8) = Uanis(C24) = Uanis(C10)
4.a :
 C02B(C02I,C01S,C026,C02E)
4.b Secondary CH2 refined with riding coordinates:
 C021(H02A,H02B), C02M(H02L,H02M)
4.c Aromatic/amide H refined with riding coordinates:
 C00M(H00M), C00O(H00O), C00Q(H00Q), C00S(H00S), C00U(H00U), C00W(H00W),
 C00Y(H00Y), C00Z(H00Z), C011(H011), C012(H012), C013(H013), C014(H014),
 C015(H015), C016(H016), C017(H017), C01A(H01D), C01C(H01E), C01E(H01F),
 C01G(H01J), C01J(H01N), C01M(H01O), C01N(H01P), C01O(H01Q), C01T(H01U),
 C01U(H01V), C01X(H01X), C01Y(H01Y), C020(H020), C022(H022), C12(H12), C17(H17),
  C9(H9), C0AA(H0AA), C02J(H02J), C024(H024), C028(H028), C029(H029),
 C02A(H02F), C02D(H02G), C1AA(H1AA), C2(H2), C3(H3), C4(H4), C5(H5)
4.d Fitted hexagon refined as free rotating group:
 C023(C12,C17,C9,C0AA,C02J), C6(C1AA,C2,C3,C4,C5)
4.e Idealised Me refined as rotating group:
 C019(H01A,H01B,H01C), C01F(H01G,H01H,H01I), C01H(H01K,H01L,H01M), C01R(H01R,
 H01S,H01T), C027(H02C,H02D,H02E), C02G(H02H,H02I,H02K), C8(H8A,H8B,H8C),
 C10(H10A,H10B,H10C), C24(H24A,H24B,H24C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              61703
_shelx_fab_checksum              55656
_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 1.951
_oxdiff_exptl_absorpt_empirical_full_min 0.647