Antiferromagnetic cyclic tetrameric copper(ii) complex and 8-azaxanthine derived from 1,3-dimethyl-5-(5′-methyl-3′-isoxazolyl-azo)-6-aminouracil: structures, non-covalent interactions and magnetism
Das, Nishan; Nandi, Nishithendu Bikash; Kłak, Julia; Sieroń, Lesław; Novikov, Alexander S.; Maniukiewicz, Waldemar; Misra, Tarun Kumar; New Journal of Chemistry 49 (2025) 20024–20038; doi:10.1039/D5NJ03321G

data_7064112
_publ_section_title
;
 Antiferromagnetic cyclic tetrameric copper(ii) complex and 8-azaxanthine
 derived from
 1,3-dimethyl-5-(5&#x2032;-methyl-3&#x2032;-isoxazolyl-azo)-6-aminouracil:
 structures, non-covalent interactions and magnetism
;
_journal_issue                   46
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              20024
_journal_page_last               20038
_journal_paper_doi               10.1039/D5NJ03321G
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         '2(C10 H12 N6 O3), H2 O'
_chemical_formula_sum            'C20 H26 N12 O7'
_chemical_formula_weight         546.53
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2025-04-21 deposited with the CCDC.	2025-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.741(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.8768(5)
_cell_length_b                   5.8611(1)
_cell_length_c                   19.6178(4)
_cell_measurement_reflns_used    23579
_cell_measurement_temperature    100
_cell_measurement_theta_max      78.907
_cell_measurement_theta_min      4.249
_cell_volume                     2392.24(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.814
_diffrn_detector_type            'Pilatus 300K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_measurement_method       '\w scans'
_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  0.0342
_diffrn_reflns_av_unetI/netI     0.0124
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28635
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        66.60
_diffrn_reflns_theta_max         66.60
_diffrn_reflns_theta_min         4.25
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.006
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.654
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       needle
_exptl_crystal_F_000             1144
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMF'
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.222
_refine_diff_density_min         -0.160
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       0.00091(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'shelxl-2018/3 (sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         2109
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+2.6302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0680
_reflns_number_gt                2042
_reflns_number_total             2109
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            d5nj03321g2.cif
_cod_data_source_block           SN1
_cod_depositor_comments
'Adding full bibliography for 7064111--7064113.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7064112
_shelx_res_checksum              33463