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_7720873
_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
'2(C2 Cl O4 Ru0.5), 2(C24 H20 P), 3(H2 O), H5 O2'
_chemical_formula_sum            'C52 H51 Cl2 O13 P2 Ru'
_chemical_formula_weight         1117.83
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2026-02-20
_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                84.823(2)
_cell_angle_beta                 75.818(2)
_cell_angle_gamma                84.852(3)
_cell_formula_units_Z            2
_cell_length_a                   9.7876(3)
_cell_length_b                   14.6019(5)
_cell_length_c                   19.0198(5)
_cell_measurement_reflns_used    12470
_cell_measurement_temperature    298.0(5)
_cell_measurement_theta_max      71.7320
_cell_measurement_theta_min      3.9680
_cell_volume                     2618.22(14)
_computing_cell_refinement       'CrysAlisPro 1.171.42.75a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.75a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.75a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298.0(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.971
_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     -5.00  37.00   1.00    2.50    --  -41.86  19.00  90.00   42
  2  \w    -87.00  -7.00   1.00    2.50    --  -41.86 125.00  90.00   80
  3  \w    -19.00  23.00   1.00    2.50    --  -41.86  37.00  30.00   42
  4  \w   -104.00 -16.00   1.00    2.50    --  -41.86 -57.00 -60.00   88
  5  \w    -20.00  27.00   1.00    2.50    --  -41.86  37.00-120.00   47
  6  \w      0.00  28.00   1.00    2.50    --  -41.86  19.00 -60.00   28
  7  \w     53.00  97.00   1.00    2.50    --   41.86-125.00   0.00   44
  8  \w     41.00 112.00   1.00   20.00    --  103.13-125.00 -60.00   71
  9  \w     27.00  52.00   1.00   20.00    --  103.13 -30.00-180.00   25
 10  \w     48.00  76.00   1.00   20.00    --  103.13 -61.00-180.00   28
 11  \w     30.00  60.00   1.00   20.00    --  103.13-125.00 -30.00   30
 12  \w     29.00  56.00   1.00   20.00    --  103.13 -30.00  60.00   27
 13  \w     34.00 105.00   1.00   20.00    --  103.13 -94.00 -30.00   71
 14  \w     75.00 178.00   1.00   20.00    --  103.13  30.00  60.00  103
 15  \w     83.00 112.00   1.00   20.00    --  103.13-125.00-180.00   29
 16  \w     35.00  61.00   1.00   20.00    --  103.13-125.00-180.00   26
 17  \w     30.00  56.00   1.00   20.00    --  103.13 -45.00 150.00   26
 18  \w     48.00  93.00   1.00   20.00    --  103.13 -61.00  90.00   45
 19  \w     76.00 105.00   1.00   20.00    --  103.13 -94.00  30.00   29
 20  \w     31.00  57.00   1.00   20.00    --  103.13 -30.00 150.00   26
 21  \w     33.00  72.00   1.00   20.00    --  103.13 -45.00 -60.00   39
 22  \w    110.00 140.00   1.00   20.00    --  103.13  77.00 150.00   30
 23  \w    105.00 167.00   1.00   20.00    --  103.13 125.00-150.00   62
 24  \w     43.00  86.00   1.00   20.00    --  103.13 -61.00   0.00   43
 25  \w     82.00 107.00   1.00   20.00    --  103.13 -94.00-120.00   25
 26  \w     79.00 107.00   1.00   20.00    --  103.13 -94.00 150.00   28
 27  \w     79.00 172.00   1.00   20.00    --  103.13  61.00 -60.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1062073000
_diffrn_orient_matrix_UB_12      -0.0201680000
_diffrn_orient_matrix_UB_13      0.0731019000
_diffrn_orient_matrix_UB_21      0.0006020000
_diffrn_orient_matrix_UB_22      -0.1007897000
_diffrn_orient_matrix_UB_23      -0.0180971000
_diffrn_orient_matrix_UB_31      0.1233129000
_diffrn_orient_matrix_UB_32      -0.0266933000
_diffrn_orient_matrix_UB_33      0.0366497000
_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  0.0239
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20036
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.870
_diffrn_reflns_theta_min         3.745
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.461
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.604
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.75a (Rigaku Oxford Diffraction, 2022)
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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1150
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         9963
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+0.7335P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0921
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8674
_reflns_number_total             9963
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00473c2.cif
_cod_data_source_block           fm01
_cod_depositor_comments
'Adding full bibliography for 7720871--7720873.cif.'
_cod_database_code               7720873
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C52 H50 O13 P2 Cl2 Ru'
_shelx_estimated_absorpt_t_max   0.717
_shelx_estimated_absorpt_t_min   0.454
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O5W-H5WA = O5W-H5WB
 0.85 with sigma of 0.02
 H5WA-H5WB
 1.34 with sigma of 0.04
3.a Free rotating group:
 O1W(H1WA), O4W(H4WA), O3W(H3WA), O2W(H2WA,H2WB)
3.b Aromatic/amide H refined with riding coordinates:
 C41(H41), C42(H42), C32(H32), C6(H6), C40(H40), C38(H38), C39(H39), C44(H44),
 C24(H24), C28(H28), C30(H30), C12(H12), C48(H48), C33(H33), C14(H14), C34(H34),
  C11(H11), C4(H4), C5(H5), C26(H26), C22(H22), C45(H45), C29(H29), C18(H18),
 C16(H16), C2(H2), C36(H36), C20(H20), C10(H10), C23(H23), C17(H17), C46(H46),
 C21(H21), C27(H27), C3(H3), C15(H15), C47(H47), C35(H35), C8(H8), C9(H9)
;
_shelx_res_checksum              56303
_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 1.167
_oxdiff_exptl_absorpt_empirical_full_min 0.800