Synthesis, structure and biological properties of a series of dicopper(bis-thiosemicarbazone) complexes
Cebotari, Diana; Calancea, Sergiu; Garbuz, Olga; Balan, Greta; Marrot, Jérôme; Shova, Sergiu; Guérineau, Vincent; Touboul, David; Tsapkov, Victor; Gulea, Aurelian; Floquet, Sébastien; New Journal of Chemistry 48 (2024) 12043–12053; doi:10.1039/D4NJ00342J

data_7063243
_publ_section_title
;
 Synthesis, structure and biological properties of a series of
 dicopper(bis-thiosemicarbazone) complexes
;
_journal_issue                   26
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              12043
_journal_page_last               12053
_journal_paper_doi               10.1039/D4NJ00342J
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C18 H28 Cu2 N6 O2 S2, 2(N O3), 0.5[]'
_chemical_formula_sum            'C19 H31 Cu2 N8 O8.75 S2'
_chemical_formula_weight         702.72
_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             2024-05-27
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-03 deposited with the CCDC.	2024-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                98.573(2)
_cell_angle_beta                 90.073(2)
_cell_angle_gamma                98.505(2)
_cell_formula_units_Z            2
_cell_length_a                   10.3405(6)
_cell_length_b                   11.1184(6)
_cell_length_c                   13.3824(8)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    180.00
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.239
_cell_volume                     1504.22(15)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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      180.00
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            79295
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.605
_diffrn_reflns_theta_min         1.992
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.609
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0689 before and 0.0487 after correction.
The Ratio of minimum to maximum transmission is 0.9038.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_description       plate
_exptl_crystal_F_000             722
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.447
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         6849
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0585P)^2^+2.1616P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1100
_refine_ls_wR_factor_ref         0.1136
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6403
_reflns_number_total             6849
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj00342j2.cif
_cod_data_source_block           dc247bis_a_ref
_cod_depositor_comments
'Adding full bibliography for 7063243--7063248.cif.'
_cod_database_code               7063243
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.699
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 N1D-O1D
 1.26 with sigma of 0.02
 N1D-O3D
 -1.26 with sigma of 0.02
 N1D-O2D1
 -1.26 with sigma of 0.02
 N1D-O2D2
 1.26 with sigma of 0.02
 C2E-C3E
 -1.54 with sigma of 0.02
 C2E-O1E
 -1.4 with sigma of 0.02
 O1E-C3E
 -2.5 with sigma of 0.02
 O2D1-O3C_$1
 -3.1 with sigma of 0.02
3. Others
 Fixed Sof: O2D1(0.5) O2D2(0.5) O1E(0.5) H1E(0.5) C2E(0.5) H2EA(0.5) H2EB(0.5)
 C3E(0.5) H3EA(0.5) H3EB(0.5) H3EC(0.5) O1W(0.25)
4.a Secondary CH2 refined with riding coordinates:
 C15A(H15A,H15B), C2E(H2EA,H2EB)
4.b Aromatic/amide H refined with riding coordinates:
 N1A(H1A), N3A(H3A), C5A(H5A), C7A(H7A), N1B(H1B), C5B(H5B), C7B(H7B)
4.c Idealised Me refined as rotating group:
 C11A(H11A,H11B,H11C), C11B(H11D,H11E,H11F), C11C(H11G,H11H,H11I), C13A(H13A,
 H13B,H13C), C16A(H16A,H16B,H16C), C13B(H13D,H13E,H13F), C3E(H3EA,H3EB,H3EC)
4.d Idealised tetrahedral OH refined as rotating group:
 O1E(H1E)
;
_shelx_res_checksum              12348
_shelx_hkl_checksum              98470
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'