Paddlewheel-type and half-paddlewheel-type diruthenium(II,II) complexes with 1,8-naphthyridine-2-carboxylate.
Kataoka, Yusuke; Tada, Nozomi; Masamori, Naoki; Yano, Natsumi; Moriyoshi, Chikako; Handa, Makoto; Dalton transactions (Cambridge, England : 2003) 54 (2025) 3047–3056; doi:10.1039/d4dt03321c

data_7717831
_publ_section_title
;
 Paddlewheel-type and half-paddlewheel-type diruthenium(II,II) complexes
 with 1,8-naphthyridine-2-carboxylate.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3047
_journal_page_last               3056
_journal_paper_doi               10.1039/d4dt03321c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C16 H10 N2 O4 Ru, C H Cl3'
_chemical_formula_sum            'C17 H11 Cl3 N2 O4 Ru'
_chemical_formula_weight         514.70
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-09
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-11-28 deposited with the CCDC.	2025-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            36
_cell_length_a                   20.7336(3)
_cell_length_b                   20.7336(3)
_cell_length_c                   45.9883(12)
_cell_measurement_reflns_used    30834
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      30.3720
_cell_measurement_theta_min      2.5460
_cell_volume                     17120.9(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'CCD plate'
_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     -7.00  21.00   0.25    1.84    --    5.00  21.00 -25.00  112
  2  \w    -48.00 -14.00   0.25    1.84    --  -15.00  21.00 -25.00  136
  3  \w    -40.00  10.00   0.25    1.84    --  -15.00  57.00  60.00  200
  4  \w    -52.00  71.00   0.25    1.84    --  -15.00  57.00-150.00  492
  5  \w    -26.00  -1.00   0.25    1.84    --  -15.00  57.00  30.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0393177000
_diffrn_orient_matrix_UB_12      -0.0186958000
_diffrn_orient_matrix_UB_13      0.0013794000
_diffrn_orient_matrix_UB_21      -0.0001047000
_diffrn_orient_matrix_UB_22      -0.0330096000
_diffrn_orient_matrix_UB_23      0.0040637000
_diffrn_orient_matrix_UB_31      0.0037245000
_diffrn_orient_matrix_UB_32      0.0108782000
_diffrn_orient_matrix_UB_33      0.0148350000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            33423
_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         27.481
_diffrn_reflns_theta_min         1.964
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.271
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             9144
_exptl_crystal_size_max          0.650
_exptl_crystal_size_mid          0.511
_exptl_crystal_size_min          0.496
_refine_diff_density_max         1.523
_refine_diff_density_min         -1.450
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4378
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0606P)^2^+224.6776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1325
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4060
_reflns_number_total             4378
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03321c2.cif
_cod_data_source_block           Ru2(NPC)2(O2CPh)2
_cod_depositor_comments
'Adding full bibliography for 7717829--7717831.cif.'
_cod_original_cell_volume        17120.9(7)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               7717831
_shelx_shelxl_version_number     2019/2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C17(H17)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C16(H16), C14(H14), C2(H2), C3(H3), C13(H13), C8(H8), C15(H15),
 C7(H7), C6(H6)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              18811
_shelx_fab_checksum              52764
_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 1.868
_oxdiff_exptl_absorpt_empirical_full_min 0.670