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_7717721
_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, Cl O4, 3.5(O)'
_chemical_formula_sum            'C28 H34 Cl N6 O13.5 Ru2 S'
_chemical_formula_weight         940.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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                 98.1500(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.7382(2)
_cell_length_b                   19.1628(2)
_cell_length_c                   20.5985(2)
_cell_measurement_reflns_used    38522
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      77.0340
_cell_measurement_theta_min      2.8940
_cell_volume                     7712.47(14)
_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_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.946
_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  99.00   0.50    2.10    --  108.69 -75.00 -91.00   98
  2  \w     36.00  65.00   0.50    2.10    --  108.69 -57.00 -90.00   58
  3  \w     36.00  69.00   0.50    2.10    --  108.69 -57.00 -60.00   66
  4  \w     38.00  68.00   0.50    2.10    --  108.69 -57.00   0.00   60
  5  \w     39.00  64.00   0.50    2.10    --  108.69 -57.00  30.00   50
  6  \w     36.00  69.00   0.50    2.10    --  108.69 -57.00  90.00   66
  7  \w     44.00  69.00   0.50    2.10    --  108.69 -57.00  60.00   50
  8  \w     47.00  85.00   0.50    2.10    --  108.69 -99.00-120.00   76
  9  \w     39.00  79.00   0.50    2.10    --  108.69 -99.00  90.00   80
 10  \w    -24.00  26.00   0.50    0.60    --  -49.12  19.00-180.00  100
 11  \w    -66.00  24.00   0.50    0.60    --  -49.12  75.00  35.00  180
 12  \w    -39.00   3.00   0.50    0.60    --  -49.12  37.00 150.00   84
 13  \w    103.00 178.00   0.50    2.10    --  108.69  75.00  35.00  150
 14  \w     94.00 168.00   0.50    2.10    --  108.69  57.00 150.00  148
 15  \w      2.00  28.00   0.50    0.60    --   49.12 -75.00 -91.00   52
 16  \w    -50.00 -23.00   0.50    2.10    --  -91.75  57.00-120.00   54
 17  \w    -62.00 -37.00   0.50    2.10    --  -91.75  57.00-150.00   50
 18  \w    -90.00 -31.00   0.50    2.10    --  -91.75  75.00  35.00  118
 19  \w   -162.00-100.00   0.50    2.10    --  -91.75 -19.00 120.00  124
 20  \w   -162.00 -84.00   0.50    2.10    --  -91.75 -37.00 -30.00  156
 21  \w    -93.00 -36.00   0.50    0.60    --  -49.12 -57.00-150.00  114
 22  \w   -142.00-116.00   0.50    2.10    --  -91.75 -75.00 -91.00   52
 23  \w   -117.00 -91.00   0.50    2.10    --  -91.75 -99.00-180.00   52
 24  \w   -158.00-133.00   0.50    2.10    --  -91.75 -99.00-180.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            57132
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.303
_diffrn_reflns_theta_min         2.902
_exptl_absorpt_coefficient_mu    8.080
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60008
_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 orange'
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_description       plate
_exptl_crystal_F_000             3784
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.513
_refine_diff_density_min         -1.287
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1013
_refine_ls_number_reflns         15476
_refine_ls_number_restraints     699
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0754P)^2^+7.4742P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1244
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13423
_reflns_number_total             15476
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02833c2.cif
_cod_data_source_block           exp_652_auto
_cod_depositor_comments
'Adding full bibliography for 7717718--7717722.cif.'
_cod_original_formula_sum        'C28 H34 Cl N6 O13.50 Ru2 S'
_cod_database_code               7717721
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.794
_shelx_estimated_absorpt_t_min   0.499
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All H(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All H(H,H) groups, All C(H,H,H) groups
2. Restrained distances
 Cl1-O13 = Cl1-O15 = Cl1-O19 = Cl1-O17
 1.43 with sigma of 0.02
 Cl1-O14 = Cl1-O20 = Cl1-O18 = Cl1-O16
 1.43 with sigma of 0.02
 O21-Cl2
 1.41 with sigma of 0.02
 O22-Cl2
 1.41 with sigma of 0.02
 Cl2-O27
 1.41 with sigma of 0.02
 Cl2-O23
 1.41 with sigma of 0.02
 Cl2-O24
 1.41 with sigma of 0.02
 Cl2-O25
 1.41 with sigma of 0.02
 Cl2-O28
 1.41 with sigma of 0.02
 Cl2-O26
 1.41 with sigma of 0.02
 Cl1-O17
 1.41 with sigma of 0.02
 Cl1-O15
 1.41 with sigma of 0.02
 Cl1-O16
 1.41 with sigma of 0.02
 Cl1-O19
 1.41 with sigma of 0.02
 O20-Cl1
 1.41 with sigma of 0.02
 Cl1-O18
 1.41 with sigma of 0.02
 O13-O15 = O13-O19 = O13-O17 = O15-O19 = O15-O17 = O19-O17
 2.37 with sigma of 0.04
 O14-O20 = O14-O18 = O14-O16 = O20-O18 = O20-O16 = O18-O16
 2.37 with sigma of 0.04
3. 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(O15) \\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(O23) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O13) = Uanis(O14)
Uanis(O20) = Uanis(O19)
Uanis(O21) = Uanis(O22)
Uanis(O25) = Uanis(O26)
Uanis(O28) = Uanis(O27)
4. Rigid body (RIGU) restrains
 O34, O33
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O13, O15, O19, O17
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 O14, O20, O18, O16
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 O15, O16, Cl1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O15, O16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O23, O27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O23, O25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O27, O23, Cl2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O21, O22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O14)=Sof(O20)=Sof(O18)=Sof(O16)=1-FVAR(1)
 Sof(O13)=Sof(O15)=Sof(O19)=Sof(O17)=FVAR(1)
 Fixed Sof: O36(0.5) O37(0.5) O32(0.5) O31(0.5) O29(0.5) O21(0.5) O27(0.5)
 O25(0.5) O23(0.5) O24(0.5) O26(0.5) O22(0.5) O28(0.5) O38(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B), C4(H4A,H4B), C45(H45A,H45B), C18(H18A,H18B), C32(H32A,H32B),
 C17(H17A,H17B), C15(H15A,H15B), C31(H31A,H31B), C3(H3A,H3B), C43(H43A,H43B),
 C1(H1A,H1B), C29(H29A,H29B)
6.b Aromatic/amide H refined with riding coordinates:
 C42(H42), C28(H28), C56(H56), C14(H14), C37(H37), C13(H13), C48(H48), C9(H9),
 C53(H53), C39(H39), C41(H41), C27(H27), C23(H23), C51(H51), C55(H55), C50(H50),
  C54(H54), C8(H8), C49(H49), C36(H36), C12(H12), C11(H11), C34(H34), C35(H35),
 C6(H6), C21(H21), C40(H40), C7(H7), C26(H26), C22(H22), C25(H25), C20(H20)
6.c Idealised Me refined with riding coordinates:
 C16(H16A,H16B,H16C), C2(H2A,H2B,H2C)
6.d Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C30(H30A,H30B,H30C)
;
_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
;