Ru(IV)-Ru(IV), Ru(III)-Ru(IV), and Ru(III)-Ru(III) complexes having a sulfato bridging ligand on the doubly oxido-/hydroxido-bridged core, and their crystallographic and electronic structures.
Misawa-Suzuki, Tomoyo; Kataoka, Yusuke; Mafune, Sota; Niwa, Teresa; Nagao, Hirotaka; Dalton transactions (Cambridge, England : 2003) 54 (2025) 2937–2949; doi:10.1039/d4dt02833c

data_7717718
_publ_section_title
;
 Ru(IV)-Ru(IV), Ru(III)-Ru(IV), and Ru(III)-Ru(III) complexes having a
 sulfato bridging ligand on the doubly oxido-/hydroxido-bridged core, and
 their crystallographic and electronic structures.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2937
_journal_page_last               2949
_journal_paper_doi               10.1039/d4dt02833c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C28 H34 N6 O6 Ru2 S, 2(Cl O4), O'
_chemical_formula_sum            'C28 H34 Cl2 N6 O15 Ru2 S'
_chemical_formula_weight         999.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-11-12
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-11-29 deposited with the CCDC.	2024-12-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.9800(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.97110(10)
_cell_length_b                   10.53080(10)
_cell_length_c                   29.8099(2)
_cell_measurement_reflns_used    18526
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      77.1890
_cell_measurement_theta_min      2.9550
_cell_volume                     3755.75(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.61a (Rigaku OD, 2022)'
_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 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 0.999
_diffrn_measured_fraction_theta_max 0.938
_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    112.00 173.00   0.50    1.50    --  108.69 100.00  47.00  122
  2  \w     42.00  68.00   0.50    1.50    --  108.69 -57.00   0.00   52
  3  \w     48.00 104.00   0.50    1.50    --  108.69 -77.00 -30.00  112
  4  \w     36.00  61.00   0.50    1.50    --  108.69 -57.00 -90.00   50
  5  \w     39.00  64.00   0.50    1.50    --  108.69 -57.00-180.00   50
  6  \w     96.00 178.00   0.50    1.50    --  108.69  37.00  30.00  164
  7  \w     42.00  67.00   0.50    1.50    --  108.69 -57.00  90.00   50
  8  \w     38.00  99.00   0.50    1.50    --  108.69 -99.00 -30.00  122
  9  \w     70.00 104.00   0.50    1.50    --  108.69-100.00 -57.00   68
 10  \w     20.00  71.00   0.50    0.30    --   49.12-100.00 -57.00  102
 11  \w   -120.00 -34.00   0.50    0.30    --  -49.12 -57.00 -60.00  172
 12  \w    -78.00 -53.00   0.50    1.50    --  -91.75 100.00  47.00   50
 13  \w    -77.00  14.00   0.50    0.30    --  -49.12 100.00  47.00  182
 14  \w    -60.00 -24.00   0.50    0.30    --  -49.12  57.00 -90.00   72
 15  \w    -61.00 -20.00   0.50    1.50    --  -91.75  57.00  30.00   82
 16  \w    -54.00 -19.00   0.50    1.50    --  -91.75  57.00   0.00   70
 17  \w    -16.00  23.00   0.50    0.30    --  -49.12  57.00 -90.00   78
 18  \w    -62.00 -35.00   0.50    1.50    --  -91.75  57.00-120.00   54
 19  \w   -162.00-105.00   0.50    1.50    --  -91.75-100.00 -57.00  114
 20  \w   -106.00 -81.00   0.50    1.50    --  -91.75 -37.00-150.00   50
 21  \w   -164.00-134.00   0.50    1.50    --  -91.75 -37.00-150.00   60
 22  \w   -109.00 -81.00   0.50    1.50    --  -91.75 -19.00   0.00   56
 23  \w   -146.00-120.00   0.50    1.50    --  -91.75 -19.00   0.00   52
 24  \w   -165.00 -79.00   0.50    1.50    --  -91.75 -37.00 150.00  172
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0392666000
_diffrn_orient_matrix_UB_12      -0.1387484000
_diffrn_orient_matrix_UB_13      0.0038962000
_diffrn_orient_matrix_UB_21      0.0046679000
_diffrn_orient_matrix_UB_22      0.0114460000
_diffrn_orient_matrix_UB_23      0.0515505000
_diffrn_orient_matrix_UB_31      -0.1225518000
_diffrn_orient_matrix_UB_32      0.0449074000
_diffrn_orient_matrix_UB_33      -0.0011648000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            28212
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.297
_diffrn_reflns_theta_min         2.967
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.009
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71234
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.61a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_description       plate
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         7477
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+1.4586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0810
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6643
_reflns_number_total             7477
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02833c2.cif
_cod_data_source_block           exp_628_auto
_cod_depositor_comments
'Adding full bibliography for 7717718--7717722.cif.'
_cod_database_code               7717718
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C28H35N7O17Ru2Cl3
_chemical_oxdiff_usercomment     '298 K'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Others
 Fixed Sof: O15(0.5) O16(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b), C4(H4a,H4b), C18(H18a,H18b), C1(H1a,H1b), C17(H17a,H17b),
 C15(H15a,H15b)
3.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C9(H9), C13(H13), C11(H11), C6(H6), C23(H23), C8(H8), C28(H28),
 C22(H22), C7(H7), C27(H27), C12(H12), C20(H20), C21(H21), C25(H25), C26(H26)
3.c Idealised Me refined as rotating group:
 C2(H2a,H2b,H2c), C16(H16a,H16b,H16c)
;
_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 1.505
_oxdiff_exptl_absorpt_empirical_full_min 0.734