Novel tetranuclear grid-like Zn(II) complexes derived from dihydrazone pyrimidine derivatives as antitumor agents.
Yuan, Juan; Lan, Hai-Rong; Xing, Ai-Ping; Zeng, Dai; Hao, Ya-Ting; Song, Jun-Ying; Lu, Jia-Xing; Zhang, Bin; Wang, Jing; Zhang, Zhen-Qiang; Dalton transactions (Cambridge, England : 2003) 53 (2024) 2193–2206; doi:10.1039/d3dt02833j

data_7714826
_publ_section_title
;
 Novel tetranuclear grid-like Zn(II) complexes derived from dihydrazone
 pyrimidine derivatives as antitumor agents.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2193
_journal_page_last               2206
_journal_paper_doi               10.1039/d3dt02833j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'C64 H44 Br8 N32 Zn4, 4(ClO4), 4(CH4O),[4(CH4O)], [5(H2O)]'
_chemical_formula_sum            'C72 H86 Br8 Cl4 N32 O29 Zn4'
_chemical_formula_weight         2906.28
_space_group_crystal_system      tetragonal
_space_group_IT_number           137
_space_group_name_Hall           '-P 4ac 2a'
_space_group_name_H-M_alt        'P 42/n m c :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-07-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6257)
;
_audit_update_record
;
2023-11-10 deposited with the CCDC.	2023-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.5744(9)
_cell_length_b                   22.5744(9)
_cell_length_c                   12.3918(7)
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      56.175
_cell_measurement_theta_min      4.610
_cell_volume                     6314.9(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker BIS V6.2.14'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Metaljet PHOTON II'
_diffrn_measurement_method       '\w and \f shutterless scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            41132
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.290
_diffrn_reflns_theta_min         4.610
_diffrn_source_current           2.86
_diffrn_source_power             0.1993706
_diffrn_source_voltage           69.71
_exptl_absorpt_coefficient_mu    3.465
_exptl_absorpt_correction_T_max  0.7518
_exptl_absorpt_correction_T_min  0.5718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1504 before and 0.1071 after correction.
The Ratio of minimum to maximum transmission is 0.7606.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_description       block
_exptl_crystal_F_000             2884
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         3735
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.205
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.086
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1367P)^2^+1.5445P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2026
_refine_ls_wR_factor_ref         0.2192
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2679
_reflns_number_total             3735
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02833j2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7714826--7714828.cif.'
_cod_original_cell_volume        6314.9(6)
_cod_original_sg_symbol_H-M      'P 42/n m c'
_cod_database_code               7714826
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.723
_shelx_estimated_absorpt_t_min   0.681
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl1-O2 = Cl1-O3 = Cl1-O4
 1.4 with sigma of 0.02
 O2_$1-O4 \\sim O3-O4 \\sim O2_$1-O3 \\sim O2-O3 \\sim O2-O2_$1 \\sim O2-O4
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim O2 \\sim O3 \\sim O4: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(O3) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O2) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: H3(0.5) H1(0.5) H10A(0.5) H10B(0.5) H10C(0.5)
5.a Riding coordinates:
 O1(H1)
5.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C2(H2), C3(H3A), C4(H4), C6(H6), C8(H8), C9(H9)
5.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;
_smtbx_masks_special_details
;     
A solvent mask was calculated and 234 electrons were 
found in a volume of 2220.1\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 4[CH4O], 4[H2O]
per Formula Unit which account for 224 electrons per unit cell.
A solvent mask was calculated and 5.5 electrons were 
found in a volume of 20\%A^3^ both in voids 2 and 3. 
This is consistent with the presence of 0.5[H2O]
per Formula Unit which account for 5 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              34189
_shelx_hkl_checksum              46626
_shelx_fab_checksum              3166
_olex2_submission_special_instructions 'No special instructions were received'