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_7717937
_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 F4 O14 Ru2'
_chemical_formula_sum            'C36 H32 F4 O14 Ru2'
_chemical_formula_weight         966.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                 103.587(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.4838(5)
_cell_length_b                   19.1954(10)
_cell_length_c                   10.1612(5)
_cell_measurement_reflns_used    8105
_cell_measurement_temperature    102.15
_cell_measurement_theta_max      31.0840
_cell_measurement_theta_min      2.3940
_cell_volume                     1798.03(17)
_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      102.15
_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 0.999
_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  74.00   0.50    2.58    --    4.46  57.00  30.00  166
  2  \w     -1.00  73.00   0.50    2.58    --    4.46  57.00 120.00  148
  3  \w    -11.00  15.00   0.50    2.58    --    4.46 -99.00 -60.00   52
;
_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      0.0733280000
_diffrn_orient_matrix_UB_12      0.0057217000
_diffrn_orient_matrix_UB_13      0.0340328000
_diffrn_orient_matrix_UB_21      -0.0146856000
_diffrn_orient_matrix_UB_22      0.0359585000
_diffrn_orient_matrix_UB_23      0.0061125000
_diffrn_orient_matrix_UB_31      -0.0177691000
_diffrn_orient_matrix_UB_32      -0.0064741000
_diffrn_orient_matrix_UB_33      0.0629192000
_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  0.0269
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11341
_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         27.498
_diffrn_reflns_theta_min         2.850
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_exptl_absorpt_coefficient_mu    0.932
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24574
_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    1.786
_exptl_crystal_description       plate
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         4040
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+1.1768P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0599
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3608
_reflns_number_total             4040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03020f2.cif
_cod_data_source_block           ru2_4f2oh_thf_auto
_cod_database_code               7717937
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ru2 C36 H32 O14 F4'
_chemical_oxdiff_usercomment     -180degree(display)
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.850
_reflns_odcompleteness_completeness 99.89
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O7-C15 \\sim O7-C15A
 with sigma of 0.02
 C16-C15 \\sim C16-C15A
 with sigma of 0.02
3. Rigid bond restraints
 O7, C15, C15A, C16, C17, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O7 \\sim C15 \\sim C15A \\sim C16 \\sim C17 \\sim C18: within 1.7A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
5. Others
 Sof(C15A)=Sof(H15C)=Sof(H15D)=Sof(H16C)=Sof(H16D)=1-FVAR(1)
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H16A)=Sof(H16B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C15A(H15C,H15D), C16(H16A,H16B), C16(H16C,H16D), C17(H17A,
 H17B), C18(H18A,H18B)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6A), C7(H7), C11(H11), C13(H13), C14(H14)
6.c Idealised tetrahedral OH refined as rotating group:
 O3(H3), O6(H6)
;
_shelx_res_checksum              97557
_shelx_hkl_checksum              27984
_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 5.203
_oxdiff_exptl_absorpt_empirical_full_min 0.403