Synthesis, structure, and magnetic properties of Fe3+ and Ru3+ metal chalcogenide (O,S) complexes with bidentate ligands
Raza, Arsen; Carneiro Neto, José Severiano; Lanza, Arianna; Bendix, Jesper; Briganti, Matteo; Sorace, Lorenzo; Perfetti, Mauro; Dalton Transactions  (2026) –; doi:10.1039/D6DT00055J

data_7720707
_publ_section_title
;
 Synthesis, structure, and magnetic properties of Fe<sup>3+</sup> and
 Ru<sup>3+</sup> metal chalcogenide (O,S) complexes with bidentate
 ligands.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8119
_journal_page_last               8127
_journal_paper_doi               10.1039/d6dt00055j
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C42 H48 N6 Na O6 Ru2 S6, OH'
_chemical_formula_sum            'C42 H49 N6 Na O7 Ru2 S6'
_chemical_formula_weight         1167.42
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-09-02
_audit_creation_method
;
FinalCif V142 by Daniel Kratzert, Freiburg 2024,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2026-01-05 deposited with the CCDC.	2026-03-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   13.922(3)
_cell_length_b                   13.922(3)
_cell_length_c                   41.850(4)
_cell_measurement_reflns_used    934
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0.7720
_cell_measurement_theta_min      0.0690
_cell_volume                     7025(2)
_computing_cell_refinement       'CrysAlisPro 1.171.44.66a (Rigaku OD, 2024)'
_computing_data_collection
;
CrysAlisPro system (CCD 43.128a 64-bit (release 20-06-2024))
;
_computing_data_reduction        'CrysAlisPro 1.171.44.66a (Rigaku OD, 2024)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn.ambient_environment      vacuum
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix-ED
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -67.00  54.00   0.25    1.00    --    0.00   0.00   0.00  484
;
_diffrn_measurement_device       'electron diffractometer'
_diffrn_measurement_device_type
;
XtaLAB Synergy-ED, HyPix-ED, electron source at 200keV
;
_diffrn_measurement_method       'continuous rotation electron diffraction'
_diffrn_measurement.method       'continuous rotation electron diffraction'
_diffrn_measurement.specimen_support
;
continuous carbon film on copper grid, 200 mesh
;
_diffrn_orient_matrix_type
;
CrysAlisPro convention (1999,Acta A55,543-557)
;
_diffrn_orient_matrix_UB_11      0.0001693000
_diffrn_orient_matrix_UB_12      0.0016938000
_diffrn_orient_matrix_UB_13      0.0002634000
_diffrn_orient_matrix_UB_21      0.0005117000
_diffrn_orient_matrix_UB_22      0.0009909000
_diffrn_orient_matrix_UB_23      -0.0005276000
_diffrn_orient_matrix_UB_31      -0.0020148000
_diffrn_orient_matrix_UB_32      -0.0006853000
_diffrn_orient_matrix_UB_33      -0.0001118000
_diffrn_radiation_monochromator  none
_diffrn_radiation.monochromator  none
_diffrn_radiation_probe          electron
_diffrn_radiation.probe          electron
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.0251
_diffrn_reflns_av_R_equivalents  0.1244
_diffrn_reflns_av_sigmaI/netI    0.2088
_diffrn_reflns_av_unetI/netI     0.0731
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            8760
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        0.836
_diffrn_reflns_theta_max         0.836
_diffrn_reflns_theta_min         0.069
_diffrn_source                   'electron diffractometer'
_diffrn_source.size
;
SAED nominal aperture diameter 100 um, corresponding to a diameter of about 2 um
at the image plane.
;
_diffrn_source_type              'JEOL JSM-2300ED, LaB6'
_diffrn_source_voltage           200
_diffrn_source.voltage           200
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.66a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal.colour            'dark brown'
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_description       block
_exptl_crystal.description       irregular
_exptl_crystal_F_000             1279
_exptl_crystal.preparation       'dry powder deposited on grid'
_exptl_crystal_size_max          0.0013
_exptl_crystal_size_mid          0.00052
_exptl_crystal_size_min          0.0002
_exptl.crystals_number           1
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       11(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1299
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.2048
_refine_ls_R_factor_gt           0.1492
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.2483P)^2^+8.4600P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4222
_refine_ls_wR_factor_ref         0.4598
_reflns_Friedel_coverage         0.000
_reflns_number_gt                737
_reflns_number_total             1299
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00055j2.cif
_cod_data_source_block           exp_725_v67
_cod_depositor_comments
'Adding full bibliography for 7720704--7720707.cif.'
_cod_original_cell_volume        7025(3)
_cod_database_code               7720707
_chemical_oxdiff_formula         'C7 H8 N1 O1 Na0.330 S1 Ru0.330 '
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     0.90
_reflns_odcompleteness_completeness 99.89
_diffrn_oxdiff_scatteringfactors_ed
;
UCLA (2022) https://srv.mbi.ucla.edu/faes/data
;
_diffrn_oxdiff_digest_creation   'CAP 1.171.44.66a, AC 1.5-ac7-004'
_diffrn_oxdiff_digest_hkl        4370d4cba1ccde0976ab299b7d1d308df4ae5e
_oxdiff_exptl_crystal_thickness  1000.0
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.054
_oxdiff_exptl_absorpt_empirical_full_min 0.700
_cell_oxdiff_measurement_reflns_used 935
_cell_oxdiff_volume              7025(2)
_cell_oxdiff_angle_gamma         120.11(2)
_cell_oxdiff_angle_beta          89.996(9)
_cell_oxdiff_angle_alpha         89.999(11)
_cell_oxdiff_length_c            41.819(3)
_cell_oxdiff_length_b            13.958(3)
_cell_oxdiff_length_a            13.911(2)
_shelx_shelxl_version_number     2019/3
_shelx_res_checksum              92981
_shelx_hkl_checksum              54091
_diffrn.ambient_temperature      298
_diffrn_radiation_wavelength.value 0.0251
_diffrn_source.device            'electron gun'
_diffrn_source.make              'JEOL JSM-2300ED, LaB6'
_diffrn_detector.description     'hybrid pixel array detector'
_diffrn_detector.make            'Rigaku HyPix-ED'
_diffrn_measurement.device_class 'electron diffractometer'
_diffrn_measurement.device_make  'Rigaku XtaLAB Synergy-ED'
_exptl.special_details
;
Gatan Elsa cryo-transfer holder model 698. Temperature controller model 1905
;
_diffrn_source.ed_diffracting_area_selection SAED
_diffrn_measurement.rotation_mode rotation
_refine.diffraction_theory       kinematical
_diffrn_measurement.sample_tracking no
_diffrn_radiation.illumination_mode parallel
_diffrn_measurement.method_precession no
_diffrn.total_exposure_time      2