Ru(IV)-Ru(IV) complexes having the doubly oxido-bridged core with a bridging carbonato or hydrogencarbonato ligand.
Misawa-Suzuki, Tomoyo; Nagao, Hirotaka; Dalton transactions (Cambridge, England : 2003) 52 (2023) 2863–2871; doi:10.1039/d2dt04080h

data_7712445
_publ_section_title
;
 Ru(IV)-Ru(IV) complexes having the doubly oxido-bridged core with a
 bridging carbonato or hydrogencarbonato ligand.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2863
_journal_page_last               2871
_journal_paper_doi               10.1039/d2dt04080h
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C29 H35 N6 O5 Ru2, 4(Cl O4), O'
_chemical_formula_sum            'C29 H35 Cl4 N6 O22 Ru2'
_chemical_formula_weight         1163.57
_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             2021-08-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-10-13 deposited with the CCDC.	2023-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                79.7680(10)
_cell_angle_beta                 81.3400(10)
_cell_angle_gamma                82.2290(10)
_cell_formula_units_Z            2
_cell_length_a                   12.58570(10)
_cell_length_b                   13.65550(10)
_cell_length_c                   13.97300(10)
_cell_measurement_reflns_used    18046
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.5590
_cell_measurement_theta_min      3.2090
_cell_volume                     2321.76(3)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.960
_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     16.00 104.00   0.50    0.10    --   42.55  74.00-151.00  176
  2  \w    146.00 172.00   0.50    0.56    --  109.88  74.00-151.00   52
  3  \w     93.00 123.00   0.50    0.56    --  109.88  74.00-151.00   60
  4  \w    113.00 177.00   0.50    0.56    --  109.88  45.00 -60.00  128
  5  \w     92.00 166.00   0.50    0.56    --  109.88  45.00 -30.00  148
  6  \w     88.00 175.00   0.50    0.56    --  109.88  45.00 -90.00  174
  7  \w     88.00 177.00   0.50    0.56    --  109.88  45.00-120.00  178
  8  \w    129.00 177.00   0.50    0.56    --  109.88  15.00-180.00   96
  9  \w     71.00 126.00   0.50    0.56    --  109.88  15.00-180.00  110
 10  \w     73.00 102.00   0.50    0.56    --  109.88 -94.00   0.00   58
 11  \w     76.00 104.00   0.50    0.56    --  109.88 -94.00 120.00   56
 12  \w     65.00 122.00   0.50    0.10    --   42.55-178.00 120.00  114
 13  \w     75.00 104.00   0.50    0.56    --  109.88 -94.00  60.00   58
 14  \w     36.00  69.00   0.50    0.56    --  109.88 -94.00   0.00   66
 15  \w     78.00 104.00   0.50    0.56    --  109.88 -94.00 -60.00   52
 16  \w     37.00 101.00   0.50    0.56    --  109.88 -94.00 -90.00  128
 17  \w     37.00 103.00   0.50    0.56    --  109.88 -94.00-180.00  132
 18  \w     77.00 105.00   0.50    0.56    --  109.88-107.00-114.41   56
 19  \w     38.00  92.00   0.50    0.56    --  109.88 -77.00   0.00  108
 20  \w     50.00  96.00   0.50    0.56    --  109.88 -74.00  80.00   92
 21  \w     40.00 100.00   0.50    0.56    --  109.88 -77.00  30.00  120
 22  \w     37.00  73.00   0.50    0.56    --  109.88 -61.00  90.00   72
 23  \w     -3.00  23.00   0.50    0.10    --   42.55 -74.00  80.00   52
 24  \w     45.00  71.00   0.50    0.56    --  109.88 -77.00 -90.00   52
 25  \w     73.00  99.00   0.50    0.56    --  109.88 -77.00 -90.00   52
 26  \w     37.00  98.00   0.50    0.56    --  109.88 -77.00-180.00  122
 27  \w    -69.00  19.00   0.50    0.10    --  -42.55  74.00-151.00  176
 28  \w    -23.00  32.00   0.50    0.10    --  -42.55  57.00 -30.00  110
 29  \w    -62.00 -33.00   0.50    0.10    --  -42.55  57.00 -30.00   58
 30  \w    -36.00  31.00   0.50    0.10    --  -42.55  37.00 150.00  134
 31  \w    -47.00 -14.00   0.50    0.56    --  -90.25  45.00  60.00   66
 32  \w    -40.00 -14.00   0.50    0.56    --  -90.25  45.00 120.00   52
 33  \w    -64.00 -30.00   0.50    0.56    --  -90.25  61.00   0.00   68
 34  \w    -45.00 -20.00   0.50    0.56    --  -90.25  45.00  30.00   50
 35  \w    -48.00 -16.00   0.50    0.56    --  -90.25  45.00 -30.00   64
 36  \w    -40.00 -14.00   0.50    0.56    --  -90.25  45.00-150.00   52
 37  \w    -77.00 -52.00   0.50    0.56    --  -90.25  74.00-151.00   50
 38  \w   -166.00-141.00   0.50    0.56    --  -90.25 -45.00-120.00   50
 39  \w   -121.00 -96.00   0.50    0.56    --  -90.25 -45.00-120.00   50
 40  \w   -109.00 -24.00   0.50    0.10    --  -42.55 -74.00  80.00  170
 41  \w   -158.00 -81.00   0.50    0.56    --  -90.25 -74.00  80.00  154
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27538
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.689
_diffrn_reflns_theta_min         3.241
_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    8.125
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1166
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.780
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         9278
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0719P)^2^+1.0137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1183
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8296
_reflns_number_total             9278
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04080h2.cif
_cod_data_source_block           exp_377
_cod_database_code               7712445
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_usercomment     '298 K'
_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 C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C1(H1A,H1B), C4(H4A,H4B), C17(H17A,H17B), C3(H3A,H3B),
 C15(H15A,H15B)
2.b Aromatic/amide H refined with riding coordinates:
 C28(H28), C14(H14), C22(H22), C23(H23), C6(H6), C27(H27), C7(H7), C21(H21),
 C20(H20), C11(H11), C9(H9), C25(H25), C8(H8), C26(H26), C13(H13), C12(H12)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C16(H16A,H16B,H16C)
2.d Idealised tetrahedral OH refined as rotating group:
 O5(H5)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              75174
_shelx_hkl_checksum              94629
_shelx_fab_checksum              43212
_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
;