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_7062453
_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 H34 Cu3 N20 O8, 2(H2 O), 2(C2 H6 O)'
_chemical_formula_sum            'C40 H50 Cu3 N20 O12'
_chemical_formula_weight         1193.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 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                 93.8720(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.6079(4)
_cell_length_b                   9.0225(2)
_cell_length_c                   19.8301(5)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      30.31
_cell_measurement_theta_min      2.48
_cell_volume                     2429.13(11)
_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 0.998
_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  0.0483
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_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            31733
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.509
_diffrn_reflns_theta_min         2.059
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.384
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6450
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0634 before and 0.0521 after correction.
The Ratio of minimum to maximum transmission is 0.8645.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_description       plate
_exptl_crystal_F_000             1222
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.919
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         7411
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0814P)^2^+2.6517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1469
_refine_ls_wR_factor_ref         0.1642
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5370
_reflns_number_total             7411
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj00568b2.cif
_cod_data_source_block           tza-29
_cod_depositor_comments
'Adding full bibliography for 7062447--7062454.cif.'
_cod_database_code               7062453
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.830
_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) groups, All O(H,H) groups
2. Restrained distances
 H5c-O4
 1.89 with sigma of 0.04
 H5d-O4_$1
 2.02 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uiso(O6) = Uiso(C16) = Uiso(C1A)
Uiso(O7) = Uiso(C6) = Uiso(C1B)
4. Others
 Sof(O7)=Sof(C6)=Sof(H6a)=Sof(H6b)=Sof(C1B)=Sof(H1Ba)=Sof(H1Bb)=Sof(H1Bc)=1-
 FVAR(1)
 Sof(O6)=Sof(C16)=Sof(H16a)=Sof(H16b)=Sof(C1A)=Sof(H1Aa)=Sof(H1Ab)=Sof(H1Ac)=
 FVAR(1)
5.a Free rotating group:
 O5(H5c,H5d), O6(C16,C1A), O7(C6,C1B)
5.b Secondary CH2 refined with riding coordinates:
 C5(H5a,H5b), C2(H2a,H2b), C16(H16a,H16b), C6(H6a,H6b)
5.c Me refined with riding coordinates:
 C1A(H1Aa,H1Ab,H1Ac), C1B(H1Ba,H1Bb,H1Bc)
5.d Aromatic/amide H refined with riding coordinates:
 C11(H11), C14(H14), C19(H19), C18(H18), C8(H8), C7(H7)
5.e Idealised Me refined as rotating group:
 C10(H10a,H10b,H10c), C17(H17a,H17b,H17c)
5.f Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              49319
_olex2_submission_special_instructions 'No special instructions were received'