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_7063244
_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         'C22 H30 Cu2 N6 O2 S2'
_chemical_formula_sum            'C22 H30 Cu2 N6 O2 S2'
_chemical_formula_weight         601.72
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-10
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-06-03 deposited with the CCDC.	2024-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                93.979(2)
_cell_angle_beta                 111.0990(10)
_cell_angle_gamma                113.0480(10)
_cell_formula_units_Z            4
_cell_length_a                   12.7043(2)
_cell_length_b                   13.4872(3)
_cell_length_c                   17.5847(3)
_cell_measurement_reflns_used    5526
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.598267874846563
_cell_measurement_theta_min      1.305157955923132
_cell_volume                     2507.85(9)
_computing_data_reduction
;
DIALS 3.8.0-gdc8ae18-release (Winter, G. et al., 2018) 
dials.scale (Beilsten-Edmands, J. et al., 2020) 
XIA2 3.8.0-g3d57088-dials-3.8 (Winter, G., 2010) 
;
_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      100.15
_diffrn_measured_fraction_theta_full 0.871
_diffrn_measured_fraction_theta_max 0.696
_diffrn_measurement_device_type  'PROXIMA 2A - Synchrotron SOLEIL'
_diffrn_measurement_method       '\f scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.72932
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_Laue_measured_fraction_full 0.871
_diffrn_reflns_Laue_measured_fraction_max 0.696
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23226
_diffrn_reflns_point_group_measured_fraction_full 0.871
_diffrn_reflns_point_group_measured_fraction_max 0.696
_diffrn_reflns_theta_full        25.950
_diffrn_reflns_theta_max         30.649
_diffrn_reflns_theta_min         1.314
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    2.031
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9708905694910015
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
DIALS 3.8.0-gdc8ae18-release (Winter, G. et al., 2018) 
dials.scale (Beilsten-Edmands, J. et al., 2020) 
XIA2 3.8.0-g3d57088-dials-3.8 (Winter, G., 2010) 
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.235
_refine_diff_density_min         -1.574
_refine_diff_density_rms         0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         9980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0640
_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^)+(0.0899P)^2^+10.6102P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1808
_refine_ls_wR_factor_ref         0.1835
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8820
_reflns_number_total             9980
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj00342j2.cif
_cod_data_source_block           dc289_2_a
_cod_depositor_comments
'Adding full bibliography for 7063243--7063248.cif.'
_cod_original_cell_volume        2507.84(8)
_cod_database_code               7063244
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.905
_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
2.a Secondary CH2 refined with riding coordinates:
 C13A(H13A,H13B), C13B(H13C,H13D), C2(H2A,H2B), C13C(H13E,H13F), C13D(H13G,
 H13H), C5(H5E,H5F)
2.b Aromatic/amide H refined with riding coordinates:
 N1A(H1A), C5A(H5A), C7A(H7A), C14A(H14A), N1B(H1B), C5B(H5B), C7B(H7B),
 C14B(H14B), N1C(H1C), C5C(H5C), C7C(H7C), C14C(H14C), N1D(H1D), C5D(H5D),
 C7D(H7D), C14D(H14D)
2.c X=CH2 refined with riding coordinates:
 C15A(H15A,H15B), C15B(H15C,H15D), C15C(H15E,H15F), C15D(H15G,H15H)
2.d Idealised Me refined as rotating group:
 C11A(H11A,H11B,H11C), C11B(H11D,H11E,H11F), C11C(H11G,H11H,H11I), C3(H3A,H3B,
 H3C), C11D(H11J,H11K,H11L), C11E(H11M,H11N,H11O), C11F(H11P,H11Q,H11R), C6(H6A,
 H6B,H6C)
;
_shelx_res_checksum              35262
_shelx_hkl_checksum              41032
_olex2_submission_special_instructions 'No special instructions were received'