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_7708938
_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, 2(C4 H8 O)'
_chemical_formula_sum            'C48 H48 F12 O16 Ru2'
_chemical_formula_weight         1311.00
_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             2020-12-02
_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                 100.872(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.7407(5)
_cell_length_b                   8.5407(3)
_cell_length_c                   22.0232(8)
_cell_measurement_reflns_used    11987
_cell_measurement_temperature    98.15
_cell_measurement_theta_max      31.1550
_cell_measurement_theta_min      1.8870
_cell_volume                     2538.15(16)
_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      98.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_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    -73.00  -5.00   0.50    7.80    --   -3.68 -44.00 132.00  136
  2  \w      0.00  68.00   0.50    7.80    --   -3.68  44.00 -76.00  136
  3  \w    -11.00  35.00   0.50    7.80    --    4.46 -99.00-180.00   92
  4  \w    -10.00  32.00   0.50    7.80    --    4.46 -99.00 -60.00   84
  5  \w     11.00  37.00   0.50    7.80    --    4.46 -99.00  30.00   52
  6  \w      6.00  36.00   0.50    7.80    --    4.46 -99.00  60.00   60
;
_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      -0.0421816000
_diffrn_orient_matrix_UB_12      -0.0291414000
_diffrn_orient_matrix_UB_13      0.0106029000
_diffrn_orient_matrix_UB_21      0.0269809000
_diffrn_orient_matrix_UB_22      -0.0680116000
_diffrn_orient_matrix_UB_23      0.0115193000
_diffrn_orient_matrix_UB_31      0.0159731000
_diffrn_orient_matrix_UB_32      0.0377848000
_diffrn_orient_matrix_UB_33      0.0288011000
_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  0.0258
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            22890
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.495
_diffrn_reflns_theta_min         2.564
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.709
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75781
_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    1.715
_exptl_crystal_description       plate
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.147
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         5673
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0284
_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^)+(0.0315P)^2^+3.3880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0697
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5057
_reflns_number_total             5673
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03791a2.cif
_cod_data_source_block           ru-hetero-24-oh2
_cod_depositor_comments
'Adding full bibliography for 7708935--7708941.cif.'
_cod_database_code               7708938
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Ru2C40H32O14F12
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.903
_reflns_odcompleteness_completeness 98.92
_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), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,
 H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C13(H13), C15(H15), C16(H16)
2.c Idealised tetrahedral OH refined as rotating group:
 O5(H5A), O6(H6A)
;
_shelx_res_checksum              36952
_shelx_hkl_checksum              73571
_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 1.451
_oxdiff_exptl_absorpt_empirical_full_min 0.677