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_7712444
_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 H34 N6 O5 Ru2, 2(Cl O4), 2(O)'
_chemical_formula_sum            'C29 H34 Cl2 N6 O15 Ru2'
_chemical_formula_weight         979.66
_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             2021-08-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-10-13 deposited with the CCDC.	2023-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                116.757(2)
_cell_angle_beta                 91.7440(10)
_cell_angle_gamma                98.8400(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1701(2)
_cell_length_b                   13.1905(2)
_cell_length_c                   13.4573(3)
_cell_measurement_reflns_used    11907
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.1200
_cell_measurement_theta_min      3.6660
_cell_volume                     1893.88(7)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.957
_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    -38.00  35.00   0.50    0.38    --  -42.55  37.00 -30.00  146
  2  \w    -31.00  25.00   0.50    0.38    --  -42.55  93.00-136.00  112
  3  \w    -30.00  35.00   0.50    0.38    --  -42.55  37.00-150.00  130
  4  \w    -24.00  35.00   0.50    0.38    --  -42.55  19.00 -60.00  118
  5  \w    -44.00 -18.00   0.50    3.00    --  -90.25  45.00  30.00   52
  6  \w    -47.00 -22.00   0.50    3.00    --  -90.25  45.00  90.00   50
  7  \w    -48.00 -23.00   0.50    3.00    --  -90.25  45.00 150.00   50
  8  \w    -48.00 -16.00   0.50    3.00    --  -90.25  45.00  60.00   64
  9  \w    -48.00 -14.00   0.50    3.00    --  -90.25  45.00 -60.00   68
 10  \w    -52.00 -26.00   0.50    3.00    --  -90.25  93.00-136.00   52
 11  \w    -76.00 -34.00   0.50    0.38    --  -42.55  93.00-136.00   84
 12  \w     68.00 104.00   0.50    0.38    --   42.55 178.00 -60.00   72
 13  \w    118.00 146.00   0.50    3.00    --  109.88  93.00-136.00   56
 14  \w    150.00 176.00   0.50    3.00    --  109.88  93.00-136.00   52
 15  \w    141.00 178.00   0.50    3.00    --  109.88  45.00 -90.00   74
 16  \w    128.00 174.00   0.50    3.00    --  109.88  45.00   0.00   92
 17  \w    120.00 178.00   0.50    3.00    --  109.88 125.00 -30.00  116
 18  \w     97.00 176.00   0.50    3.00    --  109.88 125.00  60.00  158
 19  \w    100.00 170.00   0.50    3.00    --  109.88  30.00  30.00  140
 20  \w     88.00 178.00   0.50    3.00    --  109.88  45.00 -60.00  180
 21  \w     99.00 133.00   0.50    3.00    --  109.88  45.00 -90.00   68
 22  \w     89.00 119.00   0.50    3.00    --  109.88  45.00   0.00   60
 23  \w     38.00  65.00   0.50    3.00    --  109.88 -61.00-150.00   54
 24  \w     76.00 102.00   0.50    3.00    --  109.88 -94.00-150.00   52
 25  \w     72.00  98.00   0.50    3.00    --  109.88 -77.00 -60.00   52
 26  \w     46.00 100.00   0.50    3.00    --  109.88 -94.00 -90.00  108
 27  \w     44.00  69.00   0.50    3.00    --  109.88 -94.00-150.00   50
 28  \w     36.00 104.00   0.50    3.00    --  109.88 -94.00 -30.00  136
 29  \w     77.00 104.00   0.50    3.00    --  109.88 -94.00  60.00   54
 30  \w     60.00 103.00   0.50    3.00    --  109.88 -93.00 111.00   86
 31  \w     76.00 104.00   0.50    3.00    --  109.88 -94.00 150.00   56
 32  \w     41.00  67.00   0.50    3.00    --  109.88 -94.00  60.00   52
 33  \w     44.00  89.00   0.50    3.00    --  109.88 -94.00  90.00   90
 34  \w     47.00  99.00   0.50    3.00    --  109.88 -94.00  30.00  104
 35  \w     42.00  68.00   0.50    3.00    --  109.88 -77.00  60.00   52
 36  \w     40.00  66.00   0.50    3.00    --  109.88 -61.00   0.00   52
 37  \w      9.00  68.00   0.50    0.38    --   42.55 -93.00 111.00  118
 38  \w     38.00  74.00   0.50    3.00    --  109.88 -77.00 150.00   72
 39  \w     37.00  62.00   0.50    3.00    --  109.88 -61.00 150.00   50
 40  \w     65.00 116.00   0.50    0.38    --   42.55 178.00-180.00  102
 41  \w   -136.00 -85.00   0.50    3.00    --  -90.25 -93.00 111.00  102
 42  \w   -164.00-122.00   0.50    3.00    --  -90.25 -94.00   0.00   84
 43  \w   -148.00 -90.00   0.50    3.00    --  -90.25 -94.00-150.00  116
;
_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_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1164612000
_diffrn_orient_matrix_UB_12      0.0701247000
_diffrn_orient_matrix_UB_13      0.0602147000
_diffrn_orient_matrix_UB_21      -0.0265260000
_diffrn_orient_matrix_UB_22      -0.0180269000
_diffrn_orient_matrix_UB_23      0.1027739000
_diffrn_orient_matrix_UB_31      0.0485453000
_diffrn_orient_matrix_UB_32      -0.1117562000
_diffrn_orient_matrix_UB_33      -0.0496042000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21288
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.669
_diffrn_reflns_theta_min         3.699
_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    8.417
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73503
_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 intense orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   intense
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.067
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.033
_refine_diff_density_max         1.274
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         7562
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.066
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0686P)^2^+1.2584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1198
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6545
_reflns_number_total             7562
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04080h2.cif
_cod_data_source_block           exp_389
_cod_database_code               7712444
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C29H34N6O17Cl3Ru2
_chemical_oxdiff_usercomment     '298 K'
_diffrn_oxdiff_digest_frames
;
017a7dbaab7d9d4e3a2385158df93d825a03636c68c
;
_diffrn_oxdiff_digest_hkl
;
01c7df0ba54970fbb09a0fcf714c189d6906c8
;
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
2.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C18(H18A,H18B), C15(H15A,H15B), C3(H3A,H3B), C1(H1A,H1B),
 C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C23(H23), C9(H9), C20(H20), C28(H28), C8(H8), C11(H11), C22(H22),
 C13(H13), C7(H7), C12(H12), C27(H27), C21(H21), C6(H6), C26(H26), C25(H25)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              16354
_shelx_hkl_checksum              29157
_shelx_fab_checksum              75140
_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 1.728
_oxdiff_exptl_absorpt_empirical_full_min 0.642