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_7717722
_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), 0.75(O)'
_chemical_formula_sum            'C28 H34 Cl2 N6 O14.75 Ru2 S'
_chemical_formula_weight         995.71
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-12-19
_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                 106.8070(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.3390(2)
_cell_length_b                   10.77610(10)
_cell_length_c                   31.4769(2)
_cell_measurement_reflns_used    37688
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      77.1010
_cell_measurement_theta_min      2.7710
_cell_volume                     7578.39(11)
_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 0.997
_diffrn_measured_fraction_theta_max 0.943
_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     39.00  65.00   0.50    1.70    --  108.69 -57.00 120.00   52
  2  \w     36.00  69.00   0.50    1.70    --  108.69 -57.00  90.00   66
  3  \w     36.00  61.00   0.50    1.70    --  108.69 -57.00   0.00   50
  4  \w     36.00  69.00   0.50    1.70    --  108.69 -57.00 -90.00   66
  5  \w     97.00 178.00   0.50    1.70    --  108.69  37.00   0.00  162
  6  \w    106.00 157.00   0.50    1.70    --  108.69 110.00  28.00  102
  7  \w     51.00 103.00   0.50    1.70    --  108.69 -99.00   0.00  104
  8  \w     63.00 104.00   0.50    1.70    --  108.69-110.00 -66.00   82
  9  \w     40.00 107.00   0.50    1.70    --  108.69-125.00   0.00  134
 10  \w     57.00 104.00   0.50    1.70    --  108.69-125.00  60.00   94
 11  \w     32.00  57.00   0.50    0.40    --   49.12-110.00 -66.00   50
 12  \w    -39.00  23.00   0.50    0.40    --  -49.12  37.00-180.00  124
 13  \w    -20.00  19.00   0.50    0.40    --  -49.12  19.00-180.00   78
 14  \w     -4.00  26.00   0.50    0.40    --  -49.12  19.00-150.00   60
 15  \w    -26.00  25.00   0.50    0.40    --  -49.12  19.00 -60.00  102
 16  \w    -25.00  26.00   0.50    0.40    --  -49.12  19.00 150.00  102
 17  \w    -75.00 -50.00   0.50    1.70    --  -91.75 110.00  28.00   50
 18  \w    -52.00 -26.00   0.50    1.70    --  -91.75 125.00  90.00   52
 19  \w    -82.00 -22.00   0.50    1.70    --  -91.75 125.00   0.00  120
 20  \w    -78.00 -14.00   0.50    0.40    --  -49.12 110.00  28.00  128
 21  \w    -62.00 -22.00   0.50    1.70    --  -91.75  57.00 -60.00   80
 22  \w    -62.00 -19.00   0.50    1.70    --  -91.75  57.00-120.00   86
 23  \w    -56.00 -19.00   0.50    1.70    --  -91.75  57.00-150.00   74
 24  \w    -51.00 -26.00   0.50    1.70    --  -91.75  57.00-180.00   50
 25  \w    -62.00 -37.00   0.50    1.70    --  -91.75  57.00 -30.00   50
 26  \w    -47.00 -21.00   0.50    1.70    --  -91.75  57.00 120.00   52
 27  \w   -148.00 -84.00   0.50    1.70    --  -91.75-110.00 -66.00  128
;
_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      0.0101611000
_diffrn_orient_matrix_UB_12      0.1323554000
_diffrn_orient_matrix_UB_13      0.0192347000
_diffrn_orient_matrix_UB_21      -0.0146735000
_diffrn_orient_matrix_UB_22      -0.0448630000
_diffrn_orient_matrix_UB_23      0.0421277000
_diffrn_orient_matrix_UB_31      0.0666076000
_diffrn_orient_matrix_UB_32      -0.0301062000
_diffrn_orient_matrix_UB_33      0.0216676000
_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  0.0374
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            59999
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.300
_diffrn_reflns_theta_min         3.957
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.921
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52095
_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    1.745
_exptl_crystal_description       plate
_exptl_crystal_F_000             4000
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.037
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1077
_refine_ls_number_reflns         15179
_refine_ls_number_restraints     1852
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0675P)^2^+7.4832P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1149
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12957
_reflns_number_total             15179
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02833c2.cif
_cod_data_source_block           exp_631_auto
_cod_depositor_comments
'Adding full bibliography for 7717718--7717722.cif.'
_cod_original_cell_volume        7578.38(11)
_cod_database_code               7717722
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C28H35N7O13Ru2Cl2
_chemical_oxdiff_usercomment     '298 K'
_reflns_odcompleteness_completeness 99.78
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O21-Cl3
 1.41 with sigma of 0.02
 O22-Cl3
 1.41 with sigma of 0.02
 O27-Cl3
 1.41 with sigma of 0.02
 O28-Cl3
 1.41 with sigma of 0.02
 O24-Cl3
 1.41 with sigma of 0.02
 O23-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
 O35-Cl4
 1.41 with sigma of 0.02
 O36-Cl5
 1.41 with sigma of 0.02
 O29-Cl5
 1.41 with sigma of 0.02
 O30-Cl5
 1.41 with sigma of 0.02
 O32-Cl5
 1.41 with sigma of 0.02
 O31-Cl4
 1.41 with sigma of 0.02
 Cl5-O33
 1.41 with sigma of 0.02
 O34-Cl5
 1.41 with sigma of 0.02
 Cl5-O36
 1.41 with sigma of 0.02
 Cl5-O35
 1.41 with sigma of 0.02
 O29-Cl4
 1.41 with sigma of 0.02
 O35-O29
 2.2 with sigma of 0.04
 O29-O31
 2.2 with sigma of 0.04
 O33-O31
 2.2 with sigma of 0.04
 O33-O29
 2.2 with sigma of 0.04
 O32-O34
 2.2 with sigma of 0.04
 O32-O30
 2.2 with sigma of 0.04
 O36-O30
 2.2 with sigma of 0.04
 O30-O34
 2.2 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(O28) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O25) \\sim Ueq, Uanis(O26) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(Cl4) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(Cl3) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O37) \\sim Ueq, Uanis(O38) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(Cl5) \\sim Ueq, Uanis(Cl4) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O22(0.5) O24(0.5) O28(0.5) H29A(0.6) H29B(0.6) H29C(0.4) H29D(0.4)
 C30(0.6) H30A(0.6) H30B(0.6) H30C(0.6) C31(0.4) H31A(0.4) H31B(0.4) H31C(0.4)
 O25(0.5) O37(0.5) O38(0.5) O26(0.5) O39(0.5) Cl4(0.4) O27(0.5) O23(0.5)
 O21(0.5) O35(0.4) O31(0.4) O29(0.4) O33(0.4) Cl5(0.6) O32(0.6) O34(0.6)
 O36(0.6) O30(0.6)
6.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C47(H47A,H47B), C17(H17A,H17B), C1(H1A,H1B), C18(H18A,H18B),
 C4(H4A,H4B), C33(H33A,H33B), C32(H32A,H32B), C3(H3A,H3B), C46(H46A,H46B),
 C44(H44A,H44B), C29(H29A,H29B), C29(H29C,H29D)
6.b Aromatic/amide H refined with riding coordinates:
 C43(H43), C28(H28), C27(H27), C38(H38), C14(H14), C57(H57), C52(H52),
 C23(H23), C9(H9), C42(H42), C13(H13), C6(H6), C11(H11), C26(H26), C56(H56),
 C25(H25), C37(H37), C8(H8), C7(H7), C35(H35), C22(H22), C49(H49), C54(H54),
 C36(H36), C51(H51), C12(H12), C20(H20), C40(H40), C21(H21), C41(H41), C55(H55),
  C50(H50)
6.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C2(H2A,H2B,H2C), C45(H45A,H45B,H45C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C)
;
_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 1.692
_oxdiff_exptl_absorpt_empirical_full_min 0.768