Dinitrogen-bridged diruthenium complexes bearing 2,6-pyridinedicarboxylate in the mixed-valence state.
Uehara, Kazunari; Kim, Nayoung; Benzaki, Aya; Otsuka, Midori; Misawa-Suzuki, Tomoyo; Nagao, Hirotaka; Dalton transactions (Cambridge, England : 2003) 54 (2025) 16328–16332; doi:10.1039/d5dt02337h

data_7719787
_publ_section_title
;
 Dinitrogen-bridged diruthenium complexes bearing
 2,6-pyridinedicarboxylate in the mixed-valence state.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16328
_journal_page_last               16332
_journal_paper_doi               10.1039/d5dt02337h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C14 H22 N9 O9 Ru2, H2 O, 1[CH3OH]'
_chemical_formula_sum            'C15 H28 N9 O11 Ru2'
_chemical_formula_weight         712.60
_chemical_name_common            'Dinitrogen-bridged diruthenium'
_chemical_name_systematic
;
pentaamminehydroxidodinitrogenbis(2,6-pyridinedicarboxylato)diruthenium
;
_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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2025-06-09
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2025-06-20 deposited with the CCDC.	2025-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                69.891(2)
_cell_angle_beta                 70.037(2)
_cell_angle_gamma                81.608(2)
_cell_formula_units_Z            2
_cell_length_a                   10.3571(2)
_cell_length_b                   11.2191(2)
_cell_length_c                   12.4382(3)
_cell_measurement_reflns_used    10084
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      75.5520
_cell_measurement_theta_min      4.1920
_cell_volume                     1274.96(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.131a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.131a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.131a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.42
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.943
_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     36.00  93.00   0.50    0.30    --   49.15-125.00-180.00  114
  2  \w     45.00  84.00   0.50    1.00    --  108.66-125.00 -90.00   78
  3  \w     43.00 103.00   0.50    1.00    --  108.66 -99.00 -90.00  120
  4  \w     60.00 102.00   0.50    1.00    --  108.66 -99.00-180.00   84
  5  \w     49.00  94.00   0.50    1.00    --  108.66 -99.00 -30.00   90
  6  \w     78.00 103.00   0.50    1.00    --  108.66 -99.00  30.00   50
  7  \w     41.00  67.00   0.50    1.00    --  108.66 -99.00  30.00   52
  8  \w     42.00  70.00   0.50    1.00    --  108.66 -99.00  60.00   56
  9  \w     75.00 102.00   0.50    1.00    --  108.66 -99.00   0.00   54
 10  \w     72.00  97.00   0.50    1.00    --  108.66 -99.00-120.00   50
 11  \w     74.00 103.00   0.50    1.00    --  108.66 -99.00  60.00   58
 12  \w     77.00 102.00   0.50    1.00    --  108.66 -99.00  90.00   50
 13  \w     56.00  98.00   0.50    1.00    --  108.66 -99.00 150.00   84
 14  \w     40.00  71.00   0.50    1.00    --  108.66 -99.00  90.00   62
 15  \w     39.00  65.00   0.50    1.00    --  108.66 -99.00   0.00   52
 16  \w    -20.00  22.00   0.50    0.30    --   49.15 -72.00  79.00   84
 17  \w    -25.00  32.00   0.50    0.30    --   49.15 -19.00  90.00  114
 18  \w     36.00  90.00   0.50    1.00    --  108.66 -72.00  79.00  108
 19  \w     36.00  61.00   0.50    1.00    --  108.66 -57.00 -90.00   50
 20  \w     41.00  66.00   0.50    1.00    --  108.66 -57.00-120.00   50
 21  \w    104.00 178.00   0.50    1.00    --  108.66  37.00 -30.00  148
 22  \w     88.00 164.00   0.50    1.00    --  108.66  72.00-150.00  152
 23  \w     84.00 111.00   0.50    0.30    --   49.15  72.00-150.00   54
 24  \w     53.00  81.00   0.50    0.30    --   49.15  72.00-150.00   56
 25  \w    -68.00 -21.00   0.50    0.30    --  -49.15  72.00-150.00   94
 26  \w    -54.00 -28.00   0.50    1.00    --  -91.75  72.00-150.00   52
 27  \w    -16.00  10.00   0.50    0.30    --  -49.15  72.00-150.00   52
 28  \w    -53.00 -20.00   0.50    1.00    --  -91.75  57.00 -60.00   66
 29  \w    -23.00  22.00   0.50    0.30    --  -49.15  19.00   0.00   90
 30  \w    -52.00 -23.00   0.50    1.00    --  -91.75  57.00  60.00   58
 31  \w    -54.00 -26.00   0.50    1.00    --  -91.75  57.00  30.00   56
 32  \w    -56.00 -30.00   0.50    0.30    --  -49.15 125.00 -90.00   52
 33  \w   -122.00 -82.00   0.50    1.00    --  -91.75 -37.00 120.00   80
 34  \w   -128.00-102.00   0.50    1.00    --  -91.75 -72.00  79.00   52
 35  \w   -165.00-140.00   0.50    1.00    --  -91.75 -37.00 120.00   50
 36  \w   -164.00 -79.00   0.50    1.00    --  -91.75 -37.00 150.00  170
 37  \w    -54.00 -28.00   0.50    0.30    --  -49.15 -72.00  79.00   52
 38  \w   -118.00 -61.00   0.50    0.30    --  -49.15 -72.00  79.00  114
 39  \w   -104.00 -79.00   0.50    1.00    --  -91.75 -19.00  30.00   50
 40  \w   -165.00 -83.00   0.50    1.00    --  -91.75 -19.00-150.00  164
 41  \w   -162.00-137.00   0.50    1.00    --  -91.75 -19.00  30.00   50
 42  \w   -141.00 -88.00   0.50    1.00    --  -91.75 -99.00 150.00  106
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Hypix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1420710000
_diffrn_orient_matrix_UB_12      -0.0125468000
_diffrn_orient_matrix_UB_13      -0.0907258000
_diffrn_orient_matrix_UB_21      0.0037472000
_diffrn_orient_matrix_UB_22      -0.1440158000
_diffrn_orient_matrix_UB_23      0.0654035000
_diffrn_orient_matrix_UB_31      -0.0698016000
_diffrn_orient_matrix_UB_32      -0.0225295000
_diffrn_orient_matrix_UB_33      -0.0823687000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14969
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.188
_diffrn_reflns_theta_min         3.986
_diffrn_source                   'Advanced Light Source, station 11.3.1'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.238
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84124
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.131a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.856
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             714
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.260
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         5089
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0403P)^2^+1.4955P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0856
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4523
_reflns_number_total             5089
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02337h2.cif
_cod_data_source_block           RuN2Ru
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_geom_angle_publ_flag' value 'N' was changed to 'n' in
accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26 (64 times).

data item '_geom_angle_publ_flag' value 'Y' was changed to 'y' in
accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26 (50 times).

data item '_geom_bond_publ_flag' value 'N' was changed to 'n' in
accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26 (24 times).

data item '_geom_bond_publ_flag' value 'Y' was changed to 'y' in
accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26 (37 times).

data item '_geom_torsion_publ_flag' value 'N' was changed to 'n' in
accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26 (49 times).

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7719785--7719787.cif.
;
_cod_original_cell_volume        1274.97(5)
_cod_database_code               7719787
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C15H28N9O11Ru2
_olex2_refinement_description
;
1. Restrained distances
 O10-H23 = O10-H24
 0.84 with sigma of 0.02
 O1-H1
 0.82 with sigma of 0.02
 H23-H24
 1.33 with sigma of 0.04
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 34 electrons were 
found in a volume of 127\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
1[CH3OH] per Asymmetric Unit 
which account for 36 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.356
_oxdiff_exptl_absorpt_empirical_full_min 0.770