Introduction of substituents for tuning the redox properties of benzoate-bridged paddlewheel diruthenium(II,II) complexes: what does the OH group bring?
Kosaka, Wataru; Watanabe, Yudai; Kitayama, Taku; Itoh, Chisa; Miyasaka, Hitoshi; Dalton transactions (Cambridge, England : 2003) 54 (2025) 1838–1849; doi:10.1039/d4dt03020f

data_7717925
_publ_section_title
;
 Introduction of substituents for tuning the redox properties of
 benzoate-bridged paddlewheel diruthenium(II,II) complexes: what does the
 OH group bring?
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1838
_journal_page_last               1849
_journal_paper_doi               10.1039/d4dt03020f
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C36 H32 Cl4 O14 Ru2, 1.4[[C4H8O]]'
_chemical_formula_sum            'C41.6 H43.2 Cl4 O15.4 Ru2'
_chemical_formula_weight         1133.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-11-26
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-12-03 deposited with the CCDC.	2024-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.540(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.1252(6)
_cell_length_b                   21.4303(8)
_cell_length_c                   9.2625(5)
_cell_measurement_reflns_used    6099
_cell_measurement_temperature    102
_cell_measurement_theta_max      28.4670
_cell_measurement_theta_min      1.8960
_cell_volume                     2455.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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      102
_diffrn_detector                 'Rigaku HyPix-6000 area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.833
_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   -101.00 -49.00   0.50    5.65    --  -14.06 164.00 -68.00  104
  2  \w    -72.00 -45.00   0.50    5.65    --  -14.06 116.00 143.00   54
  3  \w     19.00  44.00   0.50    5.65    --   14.53-116.00  55.00   50
  4  \w     42.00  67.00   0.50    5.65    --   14.53-164.00 -92.00   50
  5  \w   -105.00 -48.00   0.50    5.65    --  -14.06-179.00-150.00  114
  6  \w     26.00  62.00   0.50    5.65    --  -14.06  57.00-180.00   72
  7  \w    -43.00 -18.00   0.50    5.65    --  -14.06  57.00-180.00   50
  8  \w     45.00  95.00   0.50    5.65    --   14.53 179.00  60.00  100
  9  \w    -48.00  42.00   0.50    5.65    --   14.53 -57.00-150.00  180
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-Custom'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0396284000
_diffrn_orient_matrix_UB_12      0.0056000000
_diffrn_orient_matrix_UB_13      -0.0726603000
_diffrn_orient_matrix_UB_21      -0.0130176000
_diffrn_orient_matrix_UB_22      -0.0322258000
_diffrn_orient_matrix_UB_23      -0.0068723000
_diffrn_orient_matrix_UB_31      -0.0393209000
_diffrn_orient_matrix_UB_32      0.0050689000
_diffrn_orient_matrix_UB_33      0.0358067000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.833
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            9160
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.833
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.650
_diffrn_reflns_theta_min         1.901
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_exptl_absorpt_coefficient_mu    0.896
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91189
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.259
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.086
_refine_diff_density_max         1.593
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         2702
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0601
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1426P)^2^+13.5264P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2040
_refine_ls_wR_factor_ref         0.2144
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2308
_reflns_number_total             2702
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03020f2.cif
_cod_data_source_block           231026_ru2(2-oh-4-cl)4_autored
_cod_original_formula_sum        'C41.60 H43.20 Cl4 O15.40 Ru2'
_cod_database_code               7717925
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ru C H O Cl'
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.801
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.07
_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 O(H) groups
2. Others
 Sof(H3)=Sof(O3B)=Sof(H3B)=1-FVAR(1)
 Sof(H7)=Sof(O3A)=Sof(H3A)=FVAR(1)
 Fixed Sof: H9A(0.5) H9B(0.5) C8(0.5) H8A(0.5) H8B(0.5) C10(0.5) H10A(0.5)
 H10B(0.5) C11(0.5) H11A(0.5) H11B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7)
3.c Idealised tetrahedral OH refined as rotating group:
 O3A(H3A), O3B(H3B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              60894
_shelx_hkl_checksum              93426
_shelx_fab_checksum              20121
_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 2.498
_oxdiff_exptl_absorpt_empirical_full_min 0.576