Spin dynamics in Ru<sup>III</sup>-oxalate complexes: synthesis, characterization, and a<i>b initio</i> insights.
Mesa, Federico; Pacheco, Carolina; González-Platas, Javier; Cruz, Carlos; Paredes-García, Verónica; Veiga, Nicolás; Martínez, Lorena; Chiozzone, Raúl; Dalton transactions (Cambridge, England : 2003)  (2026) –; doi:10.1039/d6dt00473c

data_7720871
_publ_section_title
;
 Spin dynamics in Ru<sup>III</sup>-oxalate complexes: synthesis,
 characterization, and a<i>b initio</i> insights.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5902
_journal_page_last               5907
_journal_paper_doi               10.1039/d6dt00473c
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C16 H30 Cl2 La N4 O13 Ru'
_chemical_formula_sum            'C16 H30 Cl2 La N4 O13 Ru'
_chemical_formula_weight         797.311
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     dual
_audit_creation_date             2025-09-24
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2026-02-23 deposited with the CCDC.	2026-04-08 downloaded from the CCDC.
;
_cell_angle_alpha                89.742(5)
_cell_angle_beta                 65.308(6)
_cell_angle_gamma                67.666(6)
_cell_formula_units_Z            2
_cell_length_a                   11.1623(7)
_cell_length_b                   12.4160(7)
_cell_length_c                   12.6227(8)
_cell_measurement_reflns_used    7361
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      30.0980
_cell_measurement_theta_min      2.1930
_cell_volume                     1445.24(19)
_computing_cell_refinement       'CrysAlisPro 1.171.43.121a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.120a 64-bit (release 16-04-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.121a (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  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1268
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.9992
_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     47.00  73.00   1.00    5.00    --   -0.78  37.00  90.00   26
  2  \w    -38.00 -12.00   1.00    5.00    --   -0.78  37.00  90.00   26
  3  \w     63.00 119.00   1.00   20.00    --   30.12 178.00-180.00   56
  4  \w     74.00 118.00   1.00   20.00    --   30.12 178.00 -60.00   44
  5  \w     69.00 121.00   1.00   20.00    --   30.12 178.00  90.00   52
  6  \w    -44.00  41.00   1.00   20.00    --  -31.68  57.00 -60.00   85
  7  \w    -81.00  31.00   1.00   20.00    --  -31.68  37.00-120.00  112
  8  \w   -112.00  43.00   1.00   20.00    --  -31.68  19.00 120.00  155
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0625199000
_diffrn_orient_matrix_UB_12      -0.0091666000
_diffrn_orient_matrix_UB_13      0.0364050000
_diffrn_orient_matrix_UB_21      0.0443959000
_diffrn_orient_matrix_UB_22      -0.0540349000
_diffrn_orient_matrix_UB_23      0.0091054000
_diffrn_orient_matrix_UB_31      -0.0060349000
_diffrn_orient_matrix_UB_32      0.0307177000
_diffrn_orient_matrix_UB_33      0.0504990000
_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  0.0208
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_Laue_measured_fraction_full 0.9998
_diffrn_reflns_Laue_measured_fraction_max 0.9992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13575
_diffrn_reflns_point_group_measured_fraction_full 0.9998
_diffrn_reflns_point_group_measured_fraction_max 0.9992
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         1.80
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.222
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.744
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.121a (Rigaku Oxford Diffraction, 2024)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_description       irregular
_exptl_crystal_F_000             784.510
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.0166
_refine_diff_density_min         -0.6362
_refine_diff_density_rms         0.1253
_refine_ls_d_res_high            0.7400
_refine_ls_d_res_low             11.2895
_refine_ls_goodness_of_fit_ref   1.0345
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    55
_refine_ls_number_parameters     367
_refine_ls_number_reflns         7457
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.0316
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          -0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0263P)^2^+1.0135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0705
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              15
_reflns_limit_h_min              -13
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                6561
_reflns_number_total             7457
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d6dt00473c2.cif
_cod_data_source_block           CP01
_cod_depositor_comments
'Adding full bibliography for 7720871--7720873.cif.'
_cod_database_code               7720871
_chemical_oxdiff_formula         'C16 H30 Cl2 La1 N4 O13 Ru'
_diffrn_oxdiff_ac3_digest_hkl    412c4b8ef87a6b07b378dafb25871b4ab869b7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O11-C11 \\sim O11-C11a
 with sigma of 0.02
 N3-C12 \\sim N3a-C12a
 with sigma of 0.02
 N3-C11 \\sim N3a-C11a
 with sigma of 0.02
 N3-C13 \\sim N3a-C13a
 with sigma of 0.02
 O11-N3 \\sim O11-N3a
 with sigma of 0.04
 C12-C11 \\sim C12a-C11a
 with sigma of 0.04
 C12-C13 \\sim C12a-C13a
 with sigma of 0.04
 C11-C13 \\sim C11a-C13a
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C11a) = Uanis(N3a) = Uanis(C13a) = Uanis(C12a)
4. Rigid body (RIGU) restrains
 O11, C11, N3, C13, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11, N3, C13, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11a, N3a, C13a, C12a
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C11a)=Sof(H11a)=Sof(N3a)=Sof(C13a)=Sof(H13d)=Sof(H13e)=Sof(H13f)=
 Sof(C12a)=Sof(H12d)=Sof(H12e)=Sof(H12f)=1-FVAR(1)
 Sof(N3)=Sof(C12)=Sof(H12a)=Sof(H12b)=Sof(H12c)=Sof(C11)=Sof(H11)=Sof(C13)=
 Sof(H13a)=Sof(H13b)=Sof(H13c)=FVAR(1)
6.a Rotating group:
 O1W(H1Wa,H1Wb)
6.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C5(H5), C8(H8), C11(H11), C11a(H11a)
6.c Idealised Me refined as rotating group:
 C10(H10a,H10b,H10c), C9(H9a,H9b,H9c), C12(H12a,H12b,H12c), C6(H6a,H6b,H6c),
 C15(H15a,H15b,H15c), C16(H16a,H16b,H16c), C7(H7a,H7b,H7c), C13(H13a,H13b,H13c),
  C13a(H13d,H13e,H13f), C12a(H12d,H12e,H12f)
;
_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 1.172
_oxdiff_exptl_absorpt_empirical_full_min 0.897