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_7717928
_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         'C42 H36 F12 O14 Ru2'
_chemical_formula_sum            'C42 H36 F12 O14 Ru2'
_chemical_formula_weight         1194.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-29
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-10-28 deposited with the CCDC.	2024-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 126.003(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.8874(17)
_cell_length_b                   9.9299(4)
_cell_length_c                   23.6731(19)
_cell_measurement_reflns_used    9025
_cell_measurement_temperature    102
_cell_measurement_theta_max      29.2710
_cell_measurement_theta_min      2.1050
_cell_volume                     4542.7(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 1.5 (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 1.000
_diffrn_measured_fraction_theta_max 0.844
_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    -53.00  93.00   0.50    3.81    --   16.03  -2.00 -96.00  292
  2  \w     65.00  90.00   0.50    3.81    --   16.03 179.00-150.00   50
  3  \w     -6.00  64.00   0.50    3.81    --   16.03  57.00 -60.00  140
  4  \w     15.00  65.00   0.50    3.81    --   16.03 -99.00-120.00  100
;
_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      -0.0142641000
_diffrn_orient_matrix_UB_12      0.0022371000
_diffrn_orient_matrix_UB_13      0.0191388000
_diffrn_orient_matrix_UB_21      -0.0338403000
_diffrn_orient_matrix_UB_22      -0.0005905000
_diffrn_orient_matrix_UB_23      -0.0316929000
_diffrn_orient_matrix_UB_31      -0.0001774000
_diffrn_orient_matrix_UB_32      -0.0713585000
_diffrn_orient_matrix_UB_33      0.0008310000
_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  0.0713
_diffrn_reflns_av_unetI/netI     0.0843
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.844
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13914
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.844
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.618
_diffrn_reflns_theta_min         1.922
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_exptl_absorpt_coefficient_mu    0.780
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36834
_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            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_description       block
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.314
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.086
_refine_diff_density_max         1.542
_refine_diff_density_min         -1.675
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         5390
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0560
_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^)+(0.0672P)^2^+13.0726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1363
_refine_ls_wR_factor_ref         0.1457
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4258
_reflns_number_total             5390
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03020f2.cif
_cod_data_source_block           tk249_hete-ru2(2-oh-4-ome)_auto
_cod_original_cell_volume        4542.7(7)
_cod_database_code               7717928
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ru C H O F'
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.792
_reflns_odcompleteness_completeness 99.96
_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 C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5A), C6(H6), C7(H7), C13(H13), C16(H16), C17(H17)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C)
2.d Idealised tetrahedral OH refined as rotating group:
 O5(H5)
;
_shelx_res_checksum              77238
_shelx_hkl_checksum              67079
_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 2.177
_oxdiff_exptl_absorpt_empirical_full_min 0.185