Role of intramolecular hydrogen bonding in the redox chemistry of hydroxybenzoate-bridged paddlewheel diruthenium(II,II) complexes.
Kosaka, Wataru; Watanabe, Yudai; Aliyah, Kinanti Hantiyana; Miyasaka, Hitoshi; Dalton transactions (Cambridge, England : 2003) 51 (2021) 85–94; doi:10.1039/d1dt03791a

data_7708937
_publ_section_title
;
 Role of intramolecular hydrogen bonding in the redox chemistry of
 hydroxybenzoate-bridged paddlewheel diruthenium(II,II) complexes.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              85
_journal_page_last               94
_journal_paper_doi               10.1039/d1dt03791a
_journal_volume                  51
_journal_year                    2021
_chemical_formula_moiety         'C40 H32 F12 O14 Ru2'
_chemical_formula_sum            'C40 H32 F12 O14 Ru2'
_chemical_formula_weight         1166.79
_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             2020-07-03
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2021-11-09 deposited with the CCDC.	2021-11-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.954(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.5640(3)
_cell_length_b                   21.2804(5)
_cell_length_c                   9.1600(2)
_cell_measurement_reflns_used    16957
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.1410
_cell_measurement_theta_min      2.0270
_cell_volume                     2205.27(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.626
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_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   -110.00  70.00   0.50    8.00    --  -20.00  45.00   0.00  360
  2  \w   -110.00  70.00   0.50    8.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device       'AFC10: Fixed Chi 2 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0412397000
_diffrn_orient_matrix_UB_12      -0.0087484000
_diffrn_orient_matrix_UB_13      0.0655165000
_diffrn_orient_matrix_UB_21      -0.0467239000
_diffrn_orient_matrix_UB_22      -0.0120909000
_diffrn_orient_matrix_UB_23      0.0310952000
_diffrn_orient_matrix_UB_31      0.0069492000
_diffrn_orient_matrix_UB_32      -0.0297901000
_diffrn_orient_matrix_UB_33      -0.0317556000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0160
_diffrn_reflns_av_unetI/netI     0.0118
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            17129
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.628
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.801
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.757
_exptl_crystal_description       plate
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.213
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.056
_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     328
_refine_ls_number_reflns         5018
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0222
_refine_ls_R_factor_gt           0.0210
_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^)+(0.0266P)^2^+1.3844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0534
_refine_ls_wR_factor_ref         0.0541
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4782
_reflns_number_total             5018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03791a2.cif
_cod_data_source_block           hetero_23-oh
_cod_depositor_comments
'Adding full bibliography for 7708935--7708941.cif.'
_cod_database_code               7708937
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         Ru2C40O14F12H32
_reflns_odcompleteness_completeness 91.17
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.00
_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
 C20-C19 \\sim C20-C19A
 with sigma of 0.02
 C17-C19 \\sim C17-C19A
 with sigma of 0.04
 C17-C18 \\sim C17-C18A
 with sigma of 0.02
 C18-C19 \\sim C18A-C19A
 with sigma of 0.02
 C20-C18 \\sim C20-C18A
 with sigma of 0.04
3. Others
 Sof(H20C)=Sof(H20D)=Sof(H17C)=Sof(H17D)=Sof(C19A)=Sof(H19C)=Sof(H19D)=
 Sof(C18A)=Sof(H18C)=Sof(H18D)=1-FVAR(1)
 Sof(H20A)=Sof(H20B)=Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(C19)=
 Sof(H19A)=Sof(H19B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C20(H20C,H20D), C17(H17A,H17B), C17(H17C,H17D), C18(H18A,
 H18B), C19(H19A,H19B), C19A(H19C,H19D), C18A(H18C,H18D)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C14(H14), C16(H16), C6(H6A), C15(H15), C5(H5A)
4.c Idealised tetrahedral OH refined as rotating group:
 O5(H5), O6(H6)
;
_shelx_res_checksum              84556
_shelx_hkl_checksum              57586
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.757
_oxdiff_exptl_absorpt_empirical_full_min 0.635