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_7708940
_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, 4(C4 H8 O)'
_chemical_formula_sum            'C56 H64 F12 O18 Ru2'
_chemical_formula_weight         1455.21
_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             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                 111.700(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.1637(6)
_cell_length_b                   8.5969(3)
_cell_length_c                   20.5738(7)
_cell_measurement_reflns_used    15614
_cell_measurement_temperature    93
_cell_measurement_theta_max      31.0590
_cell_measurement_theta_min      1.8770
_cell_volume                     2984.96(19)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.626
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    7.00    --  -20.00  45.00   0.00  360
  2  \w   -110.00  70.00   0.50    7.00    --  -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      0.0247861000
_diffrn_orient_matrix_UB_12      -0.0591798000
_diffrn_orient_matrix_UB_13      0.0208932000
_diffrn_orient_matrix_UB_21      0.0262531000
_diffrn_orient_matrix_UB_22      0.0093472000
_diffrn_orient_matrix_UB_23      -0.0180559000
_diffrn_orient_matrix_UB_31      0.0215158000
_diffrn_orient_matrix_UB_32      0.0567273000
_diffrn_orient_matrix_UB_33      0.0247896000
_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  0.0396
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            23473
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.562
_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    0.614
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75292
_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    1.619
_exptl_crystal_description       plate
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.011
_refine_diff_density_max         1.853
_refine_diff_density_min         -1.062
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         6840
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0538
_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^)+(0.0583P)^2^+7.3022P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1375
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5751
_reflns_number_total             6840
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03791a2.cif
_cod_data_source_block           ru_34-oh_hetero
_cod_depositor_comments
'Adding full bibliography for 7708935--7708941.cif.'
_cod_database_code               7708940
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         Ru2C40O14F12H32
_reflns_odcompleteness_completeness 90.42
_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
 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), C25(H25A,
 H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C21(H21A,H21B),
 C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5A), C6(H6A), C7(H7), C12(H12), C13(H13), C16(H16)
2.c Idealised tetrahedral OH refined as rotating group:
 O5(H5), O6(H6)
;
_shelx_res_checksum              25048
_shelx_hkl_checksum              45596
_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 1.248
_oxdiff_exptl_absorpt_empirical_full_min 0.778