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_7063247
_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 H31 Cu2 N6 O2 S2, N O3'
_chemical_formula_sum            'C22 H31 Cu2 N7 O5 S2'
_chemical_formula_weight         664.74
_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             2024-03-27
_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                67.663(2)
_cell_angle_beta                 75.254(2)
_cell_angle_gamma                76.278(2)
_cell_formula_units_Z            2
_cell_length_a                   8.3539(5)
_cell_length_b                   13.0012(7)
_cell_length_c                   15.5862(8)
_cell_measurement_reflns_used    8791
_cell_measurement_temperature    294.00
_cell_measurement_theta_max      27.33
_cell_measurement_theta_min      2.55
_cell_volume                     1495.45(14)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX3'
_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      294.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0884
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            54362
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.512
_diffrn_reflns_theta_min         2.553
_diffrn_source                   microsource
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.604
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6441
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1321 before and 0.0727 after correction.
The Ratio of minimum to maximum transmission is 0.8639.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_description       block
_exptl_crystal_F_000             684
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         6855
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0507
_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^)+(0.0678P)^2^+2.3701P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.1543
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4852
_reflns_number_total             6855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj00342j2.cif
_cod_data_source_block           dc263d_a_ref
_cod_depositor_comments
'Adding full bibliography for 7063243--7063248.cif.'
_cod_original_cell_volume        1495.45(15)
_cod_database_code               7063247
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.807
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C13A-C14A
 1.5 with sigma of 0.02
 C13C-C14C
 1.5 with sigma of 0.02
 C14A-C15A
 1.3 with sigma of 0.02
 C14C-C15C
 1.3 with sigma of 0.02
 C14B-C14D
 1.3 with sigma of 0.02
 C15B-C15D
 1.3 with sigma of 0.02
 C11A-C11B
 2.5 with sigma of 0.02
 C11D-C11E
 2.5 with sigma of 0.02
 C11A-C11C
 2.5 with sigma of 0.02
 C11D-C11F
 2.5 with sigma of 0.02
 C11B-C11C
 2.5 with sigma of 0.02
 C11E-C11F
 2.5 with sigma of 0.02
 C13B-C14B
 -1.5 with sigma of 0.02
 C13D-C14D
 -1.5 with sigma of 0.02
 C14B-C15B
 1.25 with sigma of 0.02
 C14D-C15D
 1.25 with sigma of 0.02
 C10D-C11E
 -1.5 with sigma of 0.02
 C10D-C11D
 1.5 with sigma of 0.02
 C10D-C11F
 1.5 with sigma of 0.02
 C8A-C10D
 1.5 with sigma of 0.02
 N2-O5
 1.24 with sigma of 0.02
 N2-O6
 -1.24 with sigma of 0.02
 N2-O7
 -1.24 with sigma of 0.02
 O6-O7
 2.12 with sigma of 0.02
 O5-O6
 2.12 with sigma of 0.02
 O5-O7
 2.12 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C10A) = Uanis(C10D)
Uiso(C14B) = Uiso(C15B)
Uiso(C14D) = Uiso(C15D)
4. Others
 Sof(N2)=Sof(O5)=Sof(O6)=Sof(O7)=1-FVAR(1)
 Sof(N1)=Sof(O2)=Sof(O3)=Sof(O4)=FVAR(1)
 Fixed Sof: C10A(0.5) C11A(0.5) H11A(0.5) H11B(0.5) H11C(0.5) C11B(0.5)
 H11D(0.5) H11E(0.5) H11F(0.5) C11C(0.5) H11G(0.5) H11H(0.5) H11I(0.5)
 C13A(0.5) H13A(0.5) H13B(0.5) C14A(0.5) H14A(0.5) C15A(0.5) H15A(0.5)
 H15B(0.5) C13C(0.5) H13C(0.5) H13D(0.5) C14C(0.5) H14C(0.5) C15C(0.5)
 H15C(0.5) H15D(0.5) C10D(0.5) C11D(0.5) H11J(0.5) H11K(0.5) H11L(0.5)
 C11E(0.5) H11M(0.5) H11N(0.5) H11O(0.5) C11F(0.5) H11P(0.5) H11Q(0.5)
 H11R(0.5) C13B(0.5) H13E(0.5) H13F(0.5) C14B(0.5) H14B(0.5) C15B(0.5)
 H15E(0.5) H15F(0.5) C13D(0.5) H13G(0.5) H13H(0.5) C14D(0.5) H14D(0.5)
 C15D(0.5) H15G(0.5) H15H(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C13A(H13A,H13B), C13C(H13C,H13D), C13B(H13E,H13F), C13D(H13G,H13H), C17(H17A,
 H17B)
5.b Aromatic/amide H refined with riding coordinates:
 C5A(H5A), C7A(H7A), C14A(H14A), C14C(H14C), C5B(H5B), C7B(H7B), C14B(H14B),
 C14D(H14D)
5.c X=CH2 refined with riding coordinates:
 C15A(H15A,H15B), C15C(H15C,H15D), C15B(H15E,H15F), C15D(H15G,H15H)
5.d Idealised Me refined as rotating group:
 C11A(H11A,H11B,H11C), C11B(H11D,H11E,H11F), C11C(H11G,H11H,H11I), C11D(H11J,
 H11K,H11L), C11E(H11M,H11N,H11O), C11F(H11P,H11Q,H11R), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              69444
_shelx_hkl_checksum              13313
_olex2_submission_special_instructions 'No special instructions were received'