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_7714992
_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
'C70 H65 N7 O2 P2 Ru3, F6 P, C H Cl2, C1 H2 Cl2, C H Cl'
_chemical_formula_sum            'C73 H69 Cl5 F6 N7 O2 P3 Ru3'
_chemical_formula_weight         1763.72
_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   mixed
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc2gg188
_audit_creation_date             2023-03-05
_audit_creation_method
;
Olex2 1.5
(compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725)
;
_audit_update_record
;
2023-06-28 deposited with the CCDC.	2024-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                82.5338(14)
_cell_angle_beta                 80.6957(13)
_cell_angle_gamma                89.2357(13)
_cell_formula_units_Z            2
_cell_length_a                   10.88399(16)
_cell_length_b                   17.8080(3)
_cell_length_c                   19.4153(3)
_cell_measurement_reflns_used    21588
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      60.4780
_cell_measurement_theta_min      2.0410
_cell_volume                     3682.01(10)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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     -1.00  43.00   0.50    0.70    --   72.31 -77.00 120.00   88
  2  \w     57.00  84.00   0.50    0.70    --   72.31 -77.00 120.00   54
  3  \w     17.00  66.00   0.50    0.70    --   72.31 -75.00 -88.00   98
  4  \w     30.00  56.00   0.50    0.70    --   72.31 -38.00 -60.00   52
  5  \w      1.00  63.00   0.50    0.70    --   72.31 -38.00 -90.00  124
  6  \w     49.00 145.00   0.50    0.70    --   72.31  75.00  39.00  192
  7  \w     80.00 106.00   0.50    0.70    --   72.31 125.00 -30.00   52
  8  \w    -91.00  -2.00   0.50    0.70    --  -74.81  57.00  30.00  178
  9  \w    -47.00 -21.00   0.50    0.70    --  -74.81  75.00  39.00   52
 10  \w    -85.00 -58.00   0.50    0.70    --  -74.81  75.00  39.00   54
 11  \w    -13.00  59.00   0.50    0.40    --   -1.25  75.00  39.00  144
 12  \w     24.00 110.00   0.50    0.70    --   72.31-125.00 -90.00  172
 13  \w     78.00 105.00   0.50    0.70    --   72.31-125.00-180.00   54
 14  \w      1.00  27.00   0.50    0.70    --   72.31 -99.00 -30.00   52
 15  \w     63.00  89.00   0.50    0.70    --   72.31 -99.00 -30.00   52
 16  \w      3.00  90.00   0.50    0.70    --   72.31 -99.00 120.00  174
 17  \w    -62.00  -1.00   0.50    0.40    --   -1.25 -38.00 120.00  122
 18  \w   -111.00 -20.00   0.50    0.70    --  -74.81 125.00 150.00  182
 19  \w   -110.00 -24.00   0.50    0.70    --  -74.81 125.00  30.00  172
 20  \w    -65.00  19.00   0.50    0.40    --   -1.25 -75.00 -88.00  168
 21  \w   -148.00 -52.00   0.50    0.70    --  -74.81 -75.00 -88.00  192
 22  \w   -141.00 -88.00   0.50    0.70    --  -74.81 -99.00  30.00  106
 23  \w   -145.00 -80.00   0.50    0.70    --  -74.81-125.00  30.00  130
 24  \w   -143.00-100.00   0.50    0.70    --  -74.81 -99.00-180.00   86
;
_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      -0.0225379000
_diffrn_orient_matrix_UB_12      0.0516138000
_diffrn_orient_matrix_UB_13      -0.0529944000
_diffrn_orient_matrix_UB_21      -0.1223251000
_diffrn_orient_matrix_UB_22      -0.0061908000
_diffrn_orient_matrix_UB_23      0.0241763000
_diffrn_orient_matrix_UB_31      0.0086925000
_diffrn_orient_matrix_UB_32      0.0552317000
_diffrn_orient_matrix_UB_33      0.0396973000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ga K\a'
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_unetI/netI     0.0099
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19940
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        52.927
_diffrn_reflns_theta_max         52.927
_diffrn_reflns_theta_min         2.022
_diffrn_source                   'micro-focus metaljet'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.213
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91172
_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            'metallic dark brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_description       plate
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.058
_refine_diff_density_min         -1.604
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     958
_refine_ls_number_reflns         19940
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0558
_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^)+(0.1357P)^2^+2.0242P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1541
_refine_ls_wR_factor_ref         0.1563
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18896
_reflns_number_total             19940
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9716\% 
around [0.00 1.00 0.00] (reciprocal) or [0.01 0.99 -0.12] (direct)
;
_cod_data_source_file            d3dt01861j2.cif
_cod_data_source_block           1_twin1_hklf5
_cod_depositor_comments
'Adding full bibliography for 7714990--7714997.cif.'
_cod_database_code               7714992
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C N O H P F Ru Cl'
_shelx_estimated_absorpt_t_max   0.422
_shelx_estimated_absorpt_t_min   0.180
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H59A,H59B} of C59, {H10C,H10D} of C10A, {H10A,H10B} of
  C10, {H64A,H64B} of C64, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H13A,H13B} of C13
2. Uiso/Uaniso restraints and constraints
Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(Cl2A)=1-FVAR(1)
 Sof(Cl2)=FVAR(1)
 Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(Cl4A)=Sof(Cl)=1-FVAR(2)
 Sof(Cl10)=Sof(Cl4)=Sof(C10)=Sof(H10A)=Sof(H10B)=FVAR(2)
 Fixed Sof: Cl1(0.5) H3AA(0.25) H3AB(0.25) H3BC(0.25) H3BD(0.25) Cl3(0.5)
 H13A(0.5) H13B(0.5) Cl5(0.5) Cl6(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C59(H59A,H59B), C64(H64A,H64B), C3(H3AA,H3AB), C3(H3BC,H3BD), C10(H10A,H10B),
 C10A(H10C,H10D)
4.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C31(H31),
 C32(H32), C33(H33), C35(H35), C37(H37), C38(H38), C40(H40), C47(H47), C48(H48),
  C51(H51), C53(H53), C55(H55), C56(H56), C57(H57), C58(H58), C60(H60),
 C63(H63), C66(H66), C69(H69), C70(H70), C71(H71), C72(H72), C73(H73), C74(H74),
  C75(H75), C76(H76), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84),
 C85(H85), C86(H86), C87(H87), C88(H88), C89(H89), C90(H90), C91(H91), C7(H7),
 C8(H8), C11(H11), C2(H2), C9(H9)
4.c Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C), C12(H12A,H12B,H12C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              83862
_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 1.845
_oxdiff_exptl_absorpt_empirical_full_min 0.493
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2