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_7062448
_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         'C36 H24 Cu3 N20 O9, 6(O H2)'
_chemical_formula_sum            'C36 H36 Cu3 N20 O15'
_chemical_formula_weight         1179.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-01-17 deposited with the CCDC.	2023-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.8400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9458(4)
_cell_length_b                   19.8921(6)
_cell_length_c                   17.8258(5)
_cell_measurement_reflns_used    7354
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      25.65
_cell_measurement_theta_min      2.31
_cell_volume                     4557.8(2)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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 0.999
_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  0.0725
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21633
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.691
_diffrn_reflns_theta_min         1.886
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.479
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0792 before and 0.0614 after correction.
The Ratio of minimum to maximum transmission is 0.8868.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_description       block
_exptl_crystal_F_000             2347
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         4347
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0607P)^2^+8.2069P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1287
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3174
_reflns_number_total             4347
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj00568b2.cif
_cod_data_source_block           tza-28_1
_cod_depositor_comments
'Adding full bibliography for 7062447--7062454.cif.'
_cod_database_code               7062448
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.866
_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 O(H) groups, All O(H,H) groups
2. Restrained distances
 Cu2-H5a \\sim Cu2-H5b
 with sigma of 0.02
 C18A-C17 \\sim C18-C17
 with sigma of 0.02
3. Others
 Sof(O4A)=Sof(O3A)=Sof(C18A)=1-FVAR(1)
 Sof(O4)=Sof(H4)=Sof(O3)=Sof(C18)=FVAR(1)
 Fixed Sof: H5a(0.5) H5b(0.5) O8(0.5) O9(0.5)
4.a Free rotating group:
 O5(H5a,H5b)
4.b Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b)
4.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C8(H8), C6(H6), C4(H4a), C5(H5), C9(H9), C10(H10), C12(H12)
4.d Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_shelx_res_checksum              54235
_olex2_submission_special_instructions 'No special instructions were received'