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_7717720
_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), 1.5(O)'
_chemical_formula_sum            'C28 H34 Cl2 N6 O15.5 Ru2 S'
_chemical_formula_weight         1007.71
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.8895(3)
_cell_length_b                   13.7436(2)
_cell_length_c                   23.2881(3)
_cell_measurement_reflns_used    17436
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.5520
_cell_measurement_theta_min      3.6880
_cell_volume                     7646.13(18)
_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 0.998
_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    -70.00 -41.00   0.50    9.80    --  -91.75 105.00 140.00   58
  2  \w   -164.00 -90.00   0.50    9.80    --  -91.75 -26.00 147.00  148
  3  \w   -122.00 -96.00   0.50    9.80    --  -91.75-109.00 -51.00   52
  4  \w     44.00 104.00   0.50    9.80    --  108.69-105.00  39.00  120
  5  \w     -9.00  22.00   0.50    2.50    --  -49.12  19.00 150.00   62
  6  \w    -40.00   5.00   0.50    2.50    --  -49.12  37.00  90.00   90
  7  \w    -26.00  -1.00   0.50    2.50    --  -49.12  19.00  30.00   50
  8  \w    -82.00 -52.00   0.50    2.50    --  -49.12 125.00-180.00   60
  9  \w   -116.00 -56.00   0.50    2.50    --  -49.12 -37.00 -30.00  120
 10  \w    -56.00 -30.00   0.50    9.80    --  -91.75  57.00   0.00   52
 11  \w    -53.00 -27.00   0.50    9.80    --  -91.75  57.00 -60.00   52
 12  \w     43.00  68.00   0.50    9.80    --  108.69 -57.00-150.00   50
 13  \w     36.00  69.00   0.50    9.80    --  108.69 -57.00  30.00   66
 14  \w     37.00  67.00   0.50    9.80    --  108.69 -57.00  60.00   60
 15  \w     49.00  94.00   0.50    9.80    --  108.69 -99.00-120.00   90
 16  \w     44.00  69.00   0.50    9.80    --  108.69 -57.00  90.00   50
;
_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      0.0629710000
_diffrn_orient_matrix_UB_12      -0.0242404000
_diffrn_orient_matrix_UB_13      -0.0006567000
_diffrn_orient_matrix_UB_21      -0.0032313000
_diffrn_orient_matrix_UB_22      -0.0303851000
_diffrn_orient_matrix_UB_23      0.0635878000
_diffrn_orient_matrix_UB_31      -0.0136134000
_diffrn_orient_matrix_UB_32      -0.1050935000
_diffrn_orient_matrix_UB_33      -0.0182445000
_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  0.0321
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            30978
_diffrn_reflns_point_group_measured_fraction_full 0.879
_diffrn_reflns_point_group_measured_fraction_max 0.806
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.267
_diffrn_reflns_theta_min         3.700
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.866
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90002
_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 red'
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_description       plate
_exptl_crystal_F_000             4048
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 4440 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.027(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1121
_refine_ls_number_reflns         13073
_refine_ls_number_restraints     857
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0671P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.0989
_reflns_Friedel_coverage         0.676
_reflns_Friedel_fraction_full    0.754
_reflns_Friedel_fraction_max     0.667
_reflns_number_gt                11883
_reflns_number_total             13073
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02833c2.cif
_cod_data_source_block           exp_653_auto
_cod_depositor_comments
'Adding full bibliography for 7717718--7717722.cif.'
_cod_original_formula_sum        'C28 H34 Cl2 N6 O15.50 Ru2 S'
_cod_database_code               7717720
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C28H34N6O10Cl1S1Ru2
_chemical_oxdiff_usercomment     '298 K'
_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
 O32-Cl3
 1.41 with sigma of 0.02
 O31-Cl3
 1.41 with sigma of 0.02
 O27-Cl3
 1.41 with sigma of 0.02
 O26-Cl3
 1.41 with sigma of 0.02
 O25-Cl3
 1.41 with sigma of 0.02
 O29-Cl3
 1.41 with sigma of 0.02
 O28-Cl3
 1.41 with sigma of 0.02
 O30-Cl3
 1.41 with sigma of 0.02
 O22-Cl2
 1.41 with sigma of 0.02
 O21-Cl2
 1.41 with sigma of 0.02
 O23-Cl2
 1.41 with sigma of 0.02
 O24-Cl2
 1.41 with sigma of 0.02
 O20-Cl2
 1.41 with sigma of 0.02
 O17-Cl2
 1.41 with sigma of 0.02
 O18-Cl2
 1.41 with sigma of 0.02
 O40-Cl4 = O40-O38
 1.41 with sigma of 0.02
 O38-Cl4
 1.41 with sigma of 0.02
 O35-Cl4
 1.41 with sigma of 0.02
 O36-Cl4
 1.41 with sigma of 0.02
 O39-Cl4
 1.41 with sigma of 0.02
 O34-Cl4
 1.41 with sigma of 0.02
 O40-Cl4
 1.41 with sigma of 0.02
 Cl4-O39
 1.41 with sigma of 0.02
 Cl4-O36
 1.41 with sigma of 0.02
 O37-Cl4
 1.41 with sigma of 0.02
 O33-Cl4
 1.41 with sigma of 0.02
 O21-O19
 2.2 with sigma of 0.04
 O21-O23
 2.2 with sigma of 0.04
 O32-O30
 2.2 with sigma of 0.04
 O26-O28
 2.2 with sigma of 0.04
 O33-O35
 2.2 with sigma of 0.04
 O37-O36
 2.2 with sigma of 0.04
 O36-O40
 2.2 with sigma of 0.04
 O33-O36
 2.2 with sigma of 0.04
 O33-O40
 2.2 with sigma of 0.04
 O35-O38
 2.2 with sigma of 0.04
 O30-O32
 2.2 with sigma of 0.04
 O18-O24
 2.2 with sigma of 0.04
 O21-O17
 2.2 with sigma of 0.04
 O40-O37
 2.2 with sigma of 0.04
3. Rigid bond restraints
 O37, Cl4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1.7A
Uanis(O18) \\sim Ueq, Uanis(O24) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(O24) \\sim Ueq, Uanis(O18) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(O18) \\sim Ueq, Uanis(Cl2) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(O22) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(Cl2) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O30) \\sim Ueq, Uanis(O28) \\sim Ueq, Uanis(O27) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(O19) \\sim Ueq, Uanis(O20) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
5. Others
 Fixed Sof: O31(0.6) O35(0.5) O22(0.5) O39(0.5) O24(0.5) O34(0.5) O29(0.6)
 O19(0.5) O37(0.5) O26(0.6) O18(0.5) O27(0.6) O44(0.5) O28(0.4) O38(0.5)
 O23(0.5) O43(0.5) O42(0.5) O45(0.25) O46(0.25) O25(0.4) O32(0.4) O30(0.4)
 O33(0.5) O40(0.5) O36(0.5) O20(0.5) O17(0.5) O21(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C46(H46A,H46B), C29(H29A,H29B), C32(H32A,H32B), C18(H18A,H18B),
 C1(H1A,H1B), C45(H45A,H45B), C3(H3A,H3B), C31(H31A,H31B), C43(H43A,H43B),
 C17(H17A,H17B), C15(H15A,H15B)
6.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C42(H42), C14(H14), C41(H41), C8(H8), C37(H37), C56(H56), C9(H9),
 C7(H7), C6(H6), C39(H39), C51(H51), C22(H22), C36(H36), C13(H13), C53(H53),
 C27(H27), C40(H40), C48(H48), C35(H35), C25(H25), C28(H28), C55(H55), C34(H34),
  C54(H54), C11(H11), C26(H26), C50(H50), C49(H49), C21(H21), C12(H12), C20(H20)
6.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C44(H44A,H44B,H44C), 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 1.174
_oxdiff_exptl_absorpt_empirical_full_min 0.801