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_7720872
_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_absolute_configuration rm
_chemical_formula_moiety         'C16 H28 Cl2 Dy N4 O12 Ru'
_chemical_formula_sum            'C16 H28 Cl2 Dy N4 O12 Ru'
_chemical_formula_weight         802.888
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_Int_Tables_number      33
_atom_sites_solution_primary     dual
_audit_creation_date             2026-02-23
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6127(2)
_cell_length_b                   14.5103(3)
_cell_length_c                   18.1012(3)
_cell_measurement_reflns_used    6486
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.1620
_cell_measurement_theta_min      2.3730
_cell_volume                     2787.47(9)
_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 0.9996
_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     12.00  38.00   1.00    7.50    --   -0.62  77.00-180.00   26
  2  \w     10.00  36.00   1.00    7.50    --   -0.62  77.00-120.00   26
  3  \w     16.00  41.00   1.00   30.00    --   30.43  77.00  90.00   25
  4  \w      1.00  41.00   1.00   30.00    --   30.43  77.00 -60.00   40
  5  \w      9.00  42.00   1.00   30.00    --  -31.68  77.00   0.00   33
  6  \w    -65.00  42.00   1.00   30.00    --  -31.68  77.00-150.00  107
  7  \w     -3.00  30.00   1.00   30.00    --   30.43  37.00 -60.00   33
  8  \w    -23.00   4.00   1.00   30.00    --  -31.68  19.00-150.00   27
  9  \w     16.00  50.00   1.00   30.00    --  -31.68  19.00-150.00   34
 10  \w    -59.00 -33.00   1.00   30.00    --  -31.68  19.00-150.00   26
;
_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      0.0089183000
_diffrn_orient_matrix_UB_12      -0.0412515000
_diffrn_orient_matrix_UB_13      0.0203536000
_diffrn_orient_matrix_UB_21      -0.0512051000
_diffrn_orient_matrix_UB_22      -0.0205436000
_diffrn_orient_matrix_UB_23      -0.0190297000
_diffrn_orient_matrix_UB_31      0.0420072000
_diffrn_orient_matrix_UB_32      -0.0162937000
_diffrn_orient_matrix_UB_33      -0.0275599000
_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  0.0302
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.9996
_diffrn_reflns_Laue_measured_fraction_max 0.9992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15933
_diffrn_reflns_point_group_measured_fraction_full 0.9186
_diffrn_reflns_point_group_measured_fraction_max 0.8994
_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    3.458
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.687
_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    1.913
_exptl_crystal_description       plate
_exptl_crystal_F_000             1565.372
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.5568
_refine_diff_density_min         -0.5644
_refine_diff_density_rms         0.1228
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   -0.013(8)
_refine_ls_d_res_high            0.7401
_refine_ls_d_res_low             11.3217
_refine_ls_goodness_of_fit_ref   1.0397
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    51
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6490
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.0309
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          -0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0257P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0634
_reflns_Friedel_coverage         0.793
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              19
_reflns_limit_k_min              -19
_reflns_limit_l_max              22
_reflns_limit_l_min              -24
_reflns_number_gt                5661
_reflns_number_total             6490
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d6dt00473c2.cif
_cod_data_source_block           CP02
_cod_depositor_comments
'Adding full bibliography for 7720871--7720873.cif.'
_cod_original_sg_symbol_Hall     ' P 2c -2n'
_cod_database_code               7720872
_chemical_oxdiff_formula         'C16 H25 Cl2 O12 N4 Ru1 Dy1'
_diffrn_oxdiff_ac3_digest_hkl    41f51b61b6aa84471293cca47bcbbe36979a15
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.576(9)
 0.424(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 Dy1-O41A \\sim Dy1-O41B
 with sigma of 0.02
 O41A-C41A \\sim O41B-C41B
 with sigma of 0.02
 C42A-N4A \\sim C43B-N4B
 with sigma of 0.02
 C41A-N4A \\sim C41B-N4B
 with sigma of 0.02
 N4A-C43A \\sim N4B-C42B
 with sigma of 0.02
 Dy1-C41A \\sim Dy1-C41B
 with sigma of 0.04
 O41A-N4A \\sim O41B-N4B
 with sigma of 0.04
 C42A-C41A \\sim C43B-C41B
 with sigma of 0.04
 C42A-C43A \\sim C43B-C42B
 with sigma of 0.04
 C41A-C43A \\sim C41B-C42B
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
C41A \\sim N4A \\sim C42A \\sim C43A: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(N4B) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O41B) \\sim Ueq, Uanis(O41A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 O41A, C42A, C41A, N4A, C43A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O41B, C43B, C41B, N4B, C42B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O41B)=Sof(C43B)=Sof(H43d)=Sof(H43e)=Sof(H43f)=Sof(C41B)=Sof(H41B)=
 Sof(N4B)=Sof(C42B)=Sof(H42d)=Sof(H42e)=Sof(H42f)=1-FVAR(1)
 Sof(O41A)=Sof(C42A)=Sof(H42a)=Sof(H42b)=Sof(H42c)=Sof(C41A)=Sof(H41A)=
 Sof(N4A)=Sof(C43A)=Sof(H43a)=Sof(H43b)=Sof(H43c)=FVAR(1)
7.a Me refined with riding coordinates:
 C13(H13a,H13b,H13c), C22(H22a,H22b,H22c), C23(H23a,H23b,H23c)
7.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C11(H11), C21(H21), C41A(H41A), C41B(H41B)
7.c Idealised Me refined as rotating group:
 C33(H33a,H33b,H33c), C12(H12a,H12b,H12c), C32(H32a,H32b,H32c), C42A(H42a,H42b,
 H42c), C43A(H43a,H43b,H43c), C43B(H43d,H43e,H43f), C42B(H42d,H42e,H42f)
;
_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 1.191
_oxdiff_exptl_absorpt_empirical_full_min 0.841