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_7719785
_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         'C7 H5 Cl2 N O5 Ru, C8 H20 N'
_chemical_formula_sum            'C15 H25 Cl2 N2 O5 Ru'
_chemical_formula_weight         485.34
_chemical_name_common            Aquadichloridoruthenium
_chemical_name_systematic
;
tetraethylammonium aquadichlorido(2,6-pyridinedicarboxylato)ruthenate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-17
_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                90
_cell_angle_beta                 113.611(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.697(4)
_cell_length_b                   7.6027(7)
_cell_length_c                   14.077(3)
_cell_measurement_reflns_used    3203
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.0585
_cell_volume                     1931.6(6)
_computing_cell_refinement       'CrystalClear (Rigaku Corp, 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp, 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp, 2000)'
_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      113
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 14.6306
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       dtintegrate.ref
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0144
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7293
_diffrn_reflns_point_group_measured_fraction_full 0.859
_diffrn_reflns_point_group_measured_fraction_max 0.835
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         3.059
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    1.115
_exptl_absorpt_correction_T_max  0.9673
_exptl_absorpt_correction_T_min  0.8078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Empirical absorption correction was applied 
using Lorentz and polarization effects.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   1.0000
_exptl_transmission_factor_min   0.8919
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 1465 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     233
_refine_ls_number_reflns         3706
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0153
_refine_ls_R_factor_gt           0.0151
_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^)+(0.0170P)^2^+0.7776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0364
_refine_ls_wR_factor_ref         0.0366
_reflns_Friedel_coverage         0.673
_reflns_Friedel_fraction_full    0.721
_reflns_Friedel_fraction_max     0.673
_reflns_number_gt                3677
_reflns_number_total             3706
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02337h2.cif
_cod_data_source_block           RuCl2OH2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_geom_angle_publ_flag' value 'No' was changed to 'no' 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 (77 times).

data item '_geom_bond_publ_flag' value 'No' was changed to 'no' 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 (33 times).

data item '_geom_torsion_publ_flag' value 'No' was changed to 'no' 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 (38 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        1931.5(6)
_cod_database_code               7719785
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.808
_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,H) groups
2. Restrained distances
 Ru1-H1 \\sim Ru1-H2
 with sigma of 0.02
3.a Free rotating group:
 O1(H1,H2)
3.b Secondary CH2 refined with riding coordinates:
 C11(H12,H13), C10(H11,H10), C8(H6,H7), C9(H8,H9)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H3), C4(H5), C3(H4)
3.d Idealised Me refined as rotating group:
 C14(H20,H22,H21), C12(H16,H14,H15), C15(H24,H25,H23), C13(H18,H19,H17)
;
_olex2_submission_special_instructions 'No special instructions were received'