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_7717930
_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         'C40 H30 Cl2 F12 O12 Ru2'
_chemical_formula_sum            'C40 H30 Cl2 F12 O12 Ru2'
_chemical_formula_weight         1203.68
_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             2024-12-06
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-12-09 deposited with the CCDC.	2024-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.382(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.9776(5)
_cell_length_b                   14.0906(5)
_cell_length_c                   14.7802(7)
_cell_measurement_reflns_used    10833
_cell_measurement_temperature    102
_cell_measurement_theta_max      28.7680
_cell_measurement_theta_min      2.0230
_cell_volume                     2181.81(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
_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 0.821
_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    -64.00   5.00   0.50    1.86    --   14.53 -57.00 -60.00  138
  2  \w     10.00  45.00   0.50    1.86    --   14.53 -57.00 -60.00   70
  3  \w    -41.00  53.00   0.50    1.86    --   14.53 -79.00 153.00  188
  4  \w     55.00  96.00   0.50    1.86    --   14.53 179.00 120.00   82
  5  \w    -51.00 -25.00   0.50    1.86    --  -14.06  79.00 -81.00   52
  6  \w   -100.00 -74.00   0.50    1.86    --  -14.06 179.00 -30.00   52
  7  \w      7.00  33.00   0.50    1.86    --  -14.06  79.00 -81.00   52
  8  \w    -11.00  31.00   0.50    1.86    --  -14.06 -99.00   0.00   84
;
_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      -0.0488749000
_diffrn_orient_matrix_UB_12      -0.0347628000
_diffrn_orient_matrix_UB_13      -0.0121440000
_diffrn_orient_matrix_UB_21      0.0339587000
_diffrn_orient_matrix_UB_22      -0.0249329000
_diffrn_orient_matrix_UB_23      -0.0265051000
_diffrn_orient_matrix_UB_31      0.0321770000
_diffrn_orient_matrix_UB_32      -0.0265087000
_diffrn_orient_matrix_UB_33      0.0410079000
_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  0.0351
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.821
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15083
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.821
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.740
_diffrn_reflns_theta_min         2.043
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              micromax007
_exptl_absorpt_coefficient_mu    0.928
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86501
_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 brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_description       block
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.262
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.116
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         4637
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0296
_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^)+(0.0328P)^2^+1.8704P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0732
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4104
_reflns_number_total             4637
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03020f2.cif
_cod_data_source_block           c-179_hete-ru2(2-oh-4-cl)_auto
_cod_database_code               7717930
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ru C H O F Cl'
_shelx_estimated_absorpt_t_max   0.900
_shelx_estimated_absorpt_t_min   0.793
_reflns_odcompleteness_completeness 99.95
_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. Restrained distances
 F1-C4 \\sim F1A-C4
 with sigma of 0.02
 F2-C4 \\sim F2A-C4
 with sigma of 0.005
 F3-C4 \\sim F3A-C4
 with sigma of 0.005
 F4-C9 \\sim F4A-C9
 with sigma of 0.02
 F5-C9 \\sim F5A-C9
 with sigma of 0.005
 F6-C9 \\sim F6A-C9
 with sigma of 0.005
 C12-O5A \\sim C16-O5B
 with sigma of 0.02
3. Rigid bond restraints
 F1, F1A, F2, F2A, F3, F3A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F4, F4A, F5, F5A, F6, F6A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
F1 \\sim F1A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
F2 \\sim F2A: within 1.7A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 1.7A
F3 \\sim F3A: within 1.7A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 1.7A
F4 \\sim F4A: within 1.7A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 1.7A
F5 \\sim F5A \\sim F6 \\sim F6A: within 1.7A with sigma of 0.002 and sigma for
terminal atoms of 0.004 within 1.7A
Uanis(F2A) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
5. Others
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(2)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(2)
 Sof(O5B)=Sof(H5B)=Sof(H12)=1-FVAR(3)
 Sof(O5A)=Sof(H5A)=Sof(H16)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C12(H12), C13(H13), C15(H15), C16(H16)
6.c Tetrahedral OH refined with riding coordinates:
 O5B(H5B)
6.d Idealised tetrahedral OH refined as rotating group:
 O5A(H5A)
;
_shelx_res_checksum              19815
_shelx_hkl_checksum              86019
_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 3.228
_oxdiff_exptl_absorpt_empirical_full_min 0.413