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_7717926
_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 Br4 O14 Ru2'
_chemical_formula_sum            'C36 H32 Br4 O14 Ru2'
_chemical_formula_weight         1210.39
_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                70.963(4)
_cell_angle_beta                 89.019(4)
_cell_angle_gamma                81.985(4)
_cell_formula_units_Z            1
_cell_length_a                   9.1173(5)
_cell_length_b                   10.0764(4)
_cell_length_c                   11.2003(5)
_cell_measurement_reflns_used    6708
_cell_measurement_temperature    102.15
_cell_measurement_theta_max      31.1900
_cell_measurement_theta_min      2.1500
_cell_volume                     962.75(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 0.975
_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  10.00   0.50    0.69    --   -3.60 -57.00  90.00  148
  2  \w    -74.00   3.00   0.50    0.69    --   -3.60 -19.00 150.00  154
  3  \w    -75.00   5.00   0.50    0.69    --   -3.60 -57.00 -30.00  160
  4  \w    -29.00  -4.00   0.50    0.69    --    4.30 -38.00-180.00   50
  5  \w      2.00  61.00   0.50    0.69    --   -3.60  77.00 -90.00  118
;
_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      0.0165897000
_diffrn_orient_matrix_UB_12      -0.0734075000
_diffrn_orient_matrix_UB_13      0.0343300000
_diffrn_orient_matrix_UB_21      -0.0195199000
_diffrn_orient_matrix_UB_22      0.0138898000
_diffrn_orient_matrix_UB_23      0.0567910000
_diffrn_orient_matrix_UB_31      -0.0743089000
_diffrn_orient_matrix_UB_32      -0.0087691000
_diffrn_orient_matrix_UB_33      -0.0094015000
_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  0.0222
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10840
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.895
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.003
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54946
_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    2.088
_exptl_crystal_description       plate
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.034
_refine_diff_density_max         1.406
_refine_diff_density_min         -0.953
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4318
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0268
_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^)+(0.0319P)^2^+1.5126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0642
_refine_ls_wR_factor_ref         0.0660
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3850
_reflns_number_total             4318
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03020f2.cif
_cod_data_source_block           ru2_5br2oh_auto
_cod_database_code               7717926
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Ru2C36H32O14Br2
_chemical_oxdiff_usercomment     180d
_reflns_odcompleteness_completeness 99.92
_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:
 C17(H17A,H17B), C16(H16A,H16B), C18(H18A,H18B), C15(H15A,H15B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C14(H14), C11(H11), C4(H4), C5(H5), C12(H12)
2.c Idealised tetrahedral OH refined as rotating group:
 O6(H6), O3(H3)
;
_shelx_res_checksum              64475
_shelx_hkl_checksum              8865
_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 1.673
_oxdiff_exptl_absorpt_empirical_full_min 0.754