Structural, spectroscopic, theoretical, and magnetic investigations of a novel cubane-like tetranuclear copper(II)-hydrazone complex.
Santa Maria de la Parra, Lucía; Riafrecha, Leonardo E.; Echeverría, Gustavo A; Lezama, Luis; Piro, Oscar E.; Gil, Diego M.; Frontera, Antonio; León, Ignacio E; Dalton transactions (Cambridge, England : 2003) 54 (2025) 13976–13989; doi:10.1039/d5dt01463h

data_7719239
_publ_section_title
;
 Structural, spectroscopic, theoretical, and magnetic investigations of a
 novel cubane-like tetranuclear copper(II)-hydrazone complex.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13976
_journal_page_last               13989
_journal_paper_doi               10.1039/d5dt01463h
_journal_volume                  54
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_sum            'C13 H11 Cl N2 O3 S'
_chemical_formula_weight         310.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2023-05-05 deposited with the CCDC.	2025-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.617(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.8111(5)
_cell_length_b                   18.9792(5)
_cell_length_c                   12.8573(5)
_cell_measurement_reflns_used    3857
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      26.8540
_cell_measurement_theta_min      4.9970
_cell_volume                     2770.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'ORTEP for Windows (Farrugia, 2012)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0604
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.865
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.865
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10731
_diffrn_reflns_point_group_measured_fraction_full 0.873
_diffrn_reflns_point_group_measured_fraction_max 0.722
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.722
_diffrn_reflns_theta_min         3.349
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92512
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.457
_exptl_crystal_size_mid          0.314
_exptl_crystal_size_min          0.255
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details
;
Flack x determined using 1418 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         5170
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0400P)^2^+0.9088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0937
_reflns_Friedel_coverage         0.666
_reflns_Friedel_fraction_full    0.748
_reflns_Friedel_fraction_max     0.578
_reflns_number_gt                4101
_reflns_number_total             5170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01463h2.cif
_cod_data_source_block           shelx_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7719238--7719239.cif.'
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7719239
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.826
_shelx_estimated_absorpt_t_max   0.897
_oxdiff_exptl_absorpt_empirical_full_min 0.953
_oxdiff_exptl_absorpt_empirical_full_max 1.076
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              13207
_shelx_hkl_checksum              6249