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_7714827
_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         'C120 H84 N32 Zn4, 4(ClO4), 13(H2O), (CH3CN)'
_chemical_formula_sum            'C122 H113 Cl4 N33 O29 Zn4'
_chemical_formula_weight         2908.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-07-24
_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                 90.818(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.0319(3)
_cell_length_b                   19.2008(6)
_cell_length_c                   27.1911(7)
_cell_measurement_reflns_used    6352
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      66.9250
_cell_measurement_theta_min      3.9530
_cell_volume                     6803.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_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      173.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_unetI/netI     0.0604
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            28425
_diffrn_reflns_point_group_measured_fraction_full 0.661
_diffrn_reflns_point_group_measured_fraction_max 0.635
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.942
_diffrn_reflns_theta_min         3.741
_exptl_absorpt_coefficient_mu    2.225
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78434
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            Dark-red
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2992
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.684
_refine_diff_density_min         -1.183
_refine_diff_density_rms         0.146
_refine_ls_abs_structure_details
;
 Flack x determined using 2418 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.054(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1796
_refine_ls_number_reflns         17545
_refine_ls_number_restraints     238
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.1292
_refine_ls_R_factor_gt           0.1019
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2778
_refine_ls_wR_factor_ref         0.3126
_reflns_Friedel_coverage         0.299
_reflns_Friedel_fraction_full    0.323
_reflns_Friedel_fraction_max     0.293
_reflns_number_gt                12540
_reflns_number_total             17545
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02833j2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7714826--7714828.cif.'
_cod_database_code               7714827
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl5-O17 = Cl5-O18 = Cl5-O19 = Cl5-O20
 1.44 with sigma of 0.01
 O17-O18 = O17-O19 = O17-O20 = O18-O19 = O18-O20 = O19-O20
 2.35 with sigma of 0.02
 Cl3-O9 = Cl3-O10 = Cl3-O11 = Cl3-O12
 1.44 with sigma of 0.01
 O9-O10 = O9-O11 = O9-O12 = O10-O11 = O10-O12 = O11-O12
 2.35 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O9) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O29) \\sim Ueq, Uanis(O20)
\\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(O10) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C79)
\\sim Ueq, Uanis(C93) \\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C114) \\sim Ueq,
Uanis(C116) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O11) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O15)
\\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O23) \\sim Ueq,
Uanis(O25) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(O28) \\sim Ueq, Uanis(O32)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C35) \\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(C96) \\sim Ueq, Uanis(C97)
\\sim Ueq, Uanis(C117) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(C13) \\sim Ueq,
Uanis(O26) \\sim Ueq, Uanis(O27) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(O2)
\\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of 0.002 and sigma for terminal
atoms of 0.001
4. Others
 Sof(O28A)=1-FVAR(1)
 Sof(O28)=FVAR(1)
 Sof(Cl5)=Sof(O17)=Sof(O18)=Sof(O19)=Sof(O20)=1-FVAR(2)
 Sof(Cl1)=Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=FVAR(2)
 Sof(O27A)=1-FVAR(3)
 Sof(O27)=FVAR(3)
 Fixed Sof: H3(0.5) H6(0.5) H11(0.5) H14(0.5) H19(0.5) H22(0.5) H27(0.5)
 H30(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 N3(H3), N6(H6), N11(H11), N14(H14), N19(H19), N22(H22), N27(H27), N30(H30),
 C2(H2), C3(H3A), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C12(H12), C15(H15),
 C17(H17), C18(H18), C20(H20), C21(H21), C22(H22A), C23(H23), C26(H26),
 C27(H27A), C28(H28), C29(H29), C30(H30A), C32(H32), C33(H33), C34(H34),
 C35(H35), C37(H37), C38(H38), C40(H40), C42(H42), C46(H46), C47(H47), C48(H48),
  C49(H49), C50(H50), C51(H51), C53(H53), C54(H54), C56(H56), C57(H57),
 C58(H58), C59(H59), C62(H62), C64(H64), C65(H65), C67(H67), C68(H68), C70(H70),
  C72(H72), C76(H76), C77(H77), C78(H78), C79(H79), C80(H80), C81(H81),
 C83(H83), C84(H84), C86(H86), C87(H87), C88(H88), C89(H89), C92(H92), C93(H93),
  C94(H94), C95(H95), C97(H97), C98(H98), C100(H100), C102(H102), C105(H105),
 C107(H107), C108(H108), C109(H109), C110(H110), C111(H111), C113(H113),
 C114(H114), C116(H116), C117(H117), C118(H118), C119(H119)
5.b Idealised Me refined as rotating group:
 C122(H12A,H12B,H12C)
;
_shelx_res_checksum              84606
_shelx_hkl_checksum              7615
_olex2_submission_special_instructions 'No special instructions were received'