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_7717927
_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'
_chemical_formula_sum            'C36 H32 Cl4 O14 Ru2'
_chemical_formula_weight         1032.55
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-22
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2024-10-28 deposited with the CCDC.	2024-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                70.742(4)
_cell_angle_beta                 88.958(4)
_cell_angle_gamma                81.456(4)
_cell_formula_units_Z            1
_cell_length_a                   8.8418(5)
_cell_length_b                   10.0803(3)
_cell_length_c                   11.1109(5)
_cell_measurement_reflns_used    8431
_cell_measurement_temperature    102.15
_cell_measurement_theta_max      31.1510
_cell_measurement_theta_min      1.9320
_cell_volume                     924.00(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      102.15
_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 0.980
_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     -9.00  77.00   0.50    0.88    --    4.46  57.00-120.00  172
  2  \w     10.00  46.00   0.50    0.88    --   -3.68  57.00 -30.00   72
  3  \w     -2.00  63.00   0.50    0.88    --    4.46  38.00   0.00  130
  4  \w      1.00  77.00   0.50    0.88    --    4.46  38.00 120.00  152
  5  \w     -6.00  37.00   0.50    0.88    --    4.46 -99.00 150.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0128582000
_diffrn_orient_matrix_UB_12      0.0723272000
_diffrn_orient_matrix_UB_13      -0.0034373000
_diffrn_orient_matrix_UB_21      -0.0064697000
_diffrn_orient_matrix_UB_22      -0.0212434000
_diffrn_orient_matrix_UB_23      0.0671915000
_diffrn_orient_matrix_UB_31      0.0798789000
_diffrn_orient_matrix_UB_32      -0.0016496000
_diffrn_orient_matrix_UB_33      0.0071574000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10205
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_min         2.932
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.178
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68012
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.89a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.856
_exptl_crystal_description       plate
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.033
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4164
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0237
_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^)+(0.0297P)^2^+0.4707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0610
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3829
_reflns_number_total             4164
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03020f2.cif
_cod_data_source_block           ru2_5cl2oh_2_auto
_cod_database_code               7717927
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Ru2C36H32O14Cl4
_chemical_oxdiff_usercomment     180d
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C15(H15A,H15B), C17(H17A,H17B), C18(H18A,H18B)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C11(H11), C12(H12), C7(H7), C5(H5), C4(H4)
2.c Idealised tetrahedral OH refined as rotating group:
 O6(H6), O3(H3)
;
_shelx_res_checksum              24817
_shelx_hkl_checksum              97289
_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 1.319
_oxdiff_exptl_absorpt_empirical_full_min 0.753