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_7717719
_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         'C29 H35 N6 O5 Ru2, 3(Cl O4), 0.25(O)'
_chemical_formula_sum            'C29 H35 Cl3 N6 O17.25 Ru2'
_chemical_formula_weight         1052.12
_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             2024-12-18
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-12-19 deposited with the CCDC.	2024-12-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.5280(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.22590(10)
_cell_length_b                   15.87400(10)
_cell_length_c                   19.5308(2)
_cell_measurement_reflns_used    21186
_cell_measurement_temperature    566.15
_cell_measurement_theta_max      77.1290
_cell_measurement_theta_min      3.5230
_cell_volume                     3887.92(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.116a (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    'SHELXD  (Sheldrick, 2008)'
_diffrn_ambient_temperature      566.15
_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 0.961
_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     96.00 121.00   0.50    0.25    --  108.68  37.00  60.00   50
  2  \w    126.00 172.00   0.50    0.25    --  108.68  37.00  60.00   92
  3  \w    114.00 139.00   0.50    0.25    --  108.68 124.00 138.00   50
  4  \w     98.00 166.00   0.50    0.25    --  108.68 125.00   0.00  136
  5  \w    101.00 126.00   0.50    0.25    --  108.68 146.00 -55.00   50
  6  \w    -27.00  27.00   0.50    0.06    --  -48.88  19.00   0.00  108
  7  \w    -27.00  26.00   0.50    0.06    --  -48.88  19.00  60.00  106
  8  \w     -2.00  27.00   0.50    0.06    --  -48.88  19.00  90.00   58
  9  \w    -62.00 -21.00   0.50    0.25    --  -91.75  57.00   0.00   82
 10  \w    -57.00 -32.00   0.50    0.25    --  -91.75  57.00 -60.00   50
 11  \w    -86.00 -61.00   0.50    0.25    --  -91.75 146.00 -55.00   50
 12  \w    -81.00 -25.00   0.50    0.06    --  -48.88 124.00 138.00  112
 13  \w   -155.00-123.00   0.50    0.25    --  -91.75 -57.00 150.00   64
 14  \w   -120.00 -94.00   0.50    0.25    --  -91.75 -57.00 150.00   52
 15  \w   -136.00-103.00   0.50    0.25    --  -91.75-124.00  59.00   66
 16  \w    -99.00 -61.00   0.50    0.06    --  -48.88-146.00-106.00   76
 17  \w   -105.00 -61.00   0.50    0.25    --  -91.75-146.00-106.00   88
 18  \w   -162.00 -75.00   0.50    0.25    --  -91.75-125.00  30.00  174
 19  \w   -111.00 -75.00   0.50    0.06    --  -48.88-125.00 120.00   72
 20  \w     72.00 103.00   0.50    0.25    --  108.68 -99.00 120.00   62
 21  \w     76.00 102.00   0.50    0.25    --  108.68 -99.00 150.00   52
 22  \w     68.00 102.00   0.50    0.25    --  108.68-124.00  59.00   68
 23  \w     38.00 103.00   0.50    0.25    --  108.68 -99.00  90.00  130
 24  \w     38.00  67.00   0.50    0.25    --  108.68 -99.00 120.00   58
 25  \w     49.00 101.00   0.50    0.25    --  108.68 -99.00  60.00  104
 26  \w     55.00  80.00   0.50    0.06    --   48.88-124.00  59.00   50
 27  \w     54.00  79.00   0.50    0.06    --   48.88-146.00-106.00   50
 28  \w     83.00 111.00   0.50    0.25    --  108.68-146.00-106.00   56
 29  \w     38.00  67.00   0.50    0.25    --  108.68 -57.00 -90.00   58
 30  \w     36.00  67.00   0.50    0.25    --  108.68 -57.00-120.00   62
 31  \w     36.00  61.00   0.50    0.25    --  108.68 -57.00-180.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1113307000
_diffrn_orient_matrix_UB_12      0.0152795000
_diffrn_orient_matrix_UB_13      0.0070188000
_diffrn_orient_matrix_UB_21      -0.0137630000
_diffrn_orient_matrix_UB_22      -0.0954857000
_diffrn_orient_matrix_UB_23      0.0078658000
_diffrn_orient_matrix_UB_31      0.0501088000
_diffrn_orient_matrix_UB_32      0.0078239000
_diffrn_orient_matrix_UB_33      0.0825326000
_diffrn_radiation_collimation    0.3
_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  0.0525
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31590
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.114
_diffrn_reflns_theta_min         3.524
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    8.913
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.116a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_description       plate
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.519
_refine_diff_density_min         -1.307
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         7902
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0700P)^2^+7.5536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1233
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7281
_reflns_number_total             7902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02833c2.cif
_cod_data_source_block           exp_495_auto
_cod_depositor_comments
'Adding full bibliography for 7717718--7717722.cif.'
_cod_database_code               7717719
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C29H37N6O17Cl3Ru2
_chemical_oxdiff_usercomment     298K
_shelx_estimated_absorpt_t_max   0.776
_shelx_estimated_absorpt_t_min   0.175
_reflns_odcompleteness_completeness 99.97
_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, All O(H) groups
2. Restrained distances
 O13-Cl2
 1.41 with sigma of 0.02
 Cl2-O12
 1.41 with sigma of 0.02
 O11-Cl2
 1.41 with sigma of 0.02
 O6-Cl2
 1.41 with sigma of 0.02
 O7-Cl1
 1.41 with sigma of 0.02
 O10-Cl1
 1.41 with sigma of 0.02
 Cl3-O16
 1.41 with sigma of 0.02
 Cl3-O20
 1.41 with sigma of 0.02
 Cl4-O15
 1.41 with sigma of 0.02
 Cl4-O21
 1.41 with sigma of 0.02
 O19-Cl4
 1.41 with sigma of 0.02
 Cl4-O17
 1.41 with sigma of 0.02
 O21-O15
 2.2 with sigma of 0.04
 O20-O18
 2.2 with sigma of 0.04
 O18-O20
 2.2 with sigma of 0.04
 O18-O16
 2.2 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O16 \\sim O17: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
O18 \\sim O19: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
O15 \\sim O14: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
Uanis(O22) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O10) \\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(Cl4) \\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(O16) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(O18) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 O7, Cl1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O9, O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O13, O11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O11, Cl2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Cl3(0.4) O22(0.25) O18(0.4) O14(0.4) O16(0.4) O15(0.6) O17(0.6)
 O19(0.6) Cl4(0.6) O20(0.4) O21(0.6)
6.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C3(H3A,H3B), C15(H15A,H15B), C1(H1A,H1B),
 C4(H4A,H4B)
6.b Aromatic/amide H refined with riding coordinates:
 C28(H28), C23(H23), C27(H27), C9(H9), C25(H25), C6(H6), C26(H26), C14(H14),
 C20(H20), C22(H22), C8(H8), C11(H11), C21(H21), C13(H13), C12(H12), C7(H7)
6.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C16(H16A,H16B,H16C)
6.d Idealised tetrahedral OH refined as rotating group:
 O5(H5)
;
_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 1.842
_oxdiff_exptl_absorpt_empirical_full_min 0.563