Cytotoxic mixed-ligand copper(ii) complexes with 1H-tetrazole-5-acetic acid and oligopyridine derivatives
Ermakova, Ekaterina A.; Golubeva, Yuliya A.; Smirnova, Ksenia S.; Klyushova, Lyubov S.; Berezin, Alexey S.; Fetisov, Leonid N.; Svyatogorova, Alexandra E.; Andros, Natalia O.; Zubenko, Alexander A.; Lider, Elizaveta V.; New Journal of Chemistry 47 (2023) 9472–9482; doi:10.1039/D3NJ00568B

data_7062454
_publ_section_title
;
 Cytotoxic mixed-ligand copper(ii) complexes with 1H-tetrazole-5-acetic
 acid and oligopyridine derivatives
;
_journal_issue                   19
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              9472
_journal_page_last               9482
_journal_paper_doi               10.1039/D3NJ00568B
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C30 H18 Cl2 Cu2 N12 O4, C2 H6 O S, 3(H2 O)'
_chemical_formula_sum            'C32 H30 Cl2 Cu2 N12 O8 S'
_chemical_formula_weight         940.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-11
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-01-17 deposited with the CCDC.	2023-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.2310(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0581(7)
_cell_length_b                   9.1854(4)
_cell_length_c                   21.4525(9)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      27.64
_cell_measurement_theta_min      2.40
_cell_volume                     3683.5(3)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            50153
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.324
_diffrn_reflns_theta_min         2.028
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.426
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6305
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0917 before and 0.0599 after correction.
The Ratio of minimum to maximum transmission is 0.8455.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_description       plate
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.025
_refine_diff_density_max         2.343
_refine_diff_density_min         -1.298
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         9177
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.1192
_refine_ls_R_factor_gt           0.0899
_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^)+(0.0079P)^2^+31.7640P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1948
_refine_ls_wR_factor_ref         0.2079
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6729
_reflns_number_total             9177
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj00568b2.cif
_cod_data_source_block           tza-56
_cod_depositor_comments
'Adding full bibliography for 7062447--7062454.cif.'
_cod_database_code               7062454
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.894
_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, All O(H,H) groups
2.a Free rotating group:
 O6(H6A,H6B), O8(H8A,H8B), O7(H7A,H7B)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C17(H17A,H17B)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C12(H12), C28(H28), C4(H4), C11(H11), C23(H23), C5(H5), C9(H9),
 C27(H27), C26(H26), C6(H6), C19(H19), C21(H21), C20(H20)
2.d Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C31(H31A,H31B,H31C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              81266
_olex2_submission_special_instructions 'No special instructions were received'