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_7714828
_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
'C88 H72 N32 Zn4, 5(CH4O), 7(ClO4), 11(H2O)??[(ClO4)], [2(CH4 O)]'
_chemical_formula_sum            'C95 H122 Cl8 N32 O50 Zn4'
_chemical_formula_weight         3057.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-07-23
_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                 102.101(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.7935(4)
_cell_length_b                   24.8747(4)
_cell_length_c                   21.6340(4)
_cell_measurement_reflns_used    15820
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      73.6870
_cell_measurement_theta_min      4.0850
_cell_volume                     13045.9(4)
_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      100.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.967
_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  0.0908
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            27095
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.014
_diffrn_reflns_theta_min         3.528
_exptl_absorpt_coefficient_mu    3.202
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.69035
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       cube
_exptl_crystal_F_000             6288
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.242
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.153
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1631
_refine_ls_number_reflns         15547
_refine_ls_number_restraints     343
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.1061
_refine_ls_R_factor_gt           0.1011
_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^)+(0.1962P)^2^+90.8057P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2956
_refine_ls_wR_factor_ref         0.3019
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.967
_reflns_number_gt                14265
_reflns_number_total             15547
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02833j2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7714826--7714828.cif.'
_cod_database_code               7714828
_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
2. Restrained distances
 Cl6-O46 = Cl6-O47 = Cl6-O48 = Cl6-O49 = C42-C72
 1.44 with sigma of 0.01
 O46-O47 = O46-O48 = O46-O49 = O47-O48 = O47-O49 = O48-O49
 2.35 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N27) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C45)
\\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C62) \\sim Ueq,
Uanis(C72) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C40)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O10) \\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(O50) \\sim Ueq, Uanis(O34)
\\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C69) \\sim Ueq,
Uanis(C71) \\sim Ueq, Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C63) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(O37) \\sim Ueq, Uanis(C82)
\\sim Ueq, Uanis(O46) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(N15) \\sim Ueq,
Uanis(C23) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C39)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C87) \\sim Ueq, Uanis(N24) \\sim Ueq, Uanis(N18) \\sim Ueq, Uanis(C7)
\\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C91) \\sim Ueq,
Uanis(C34) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(O3) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C82)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(C66) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O33)
\\sim Ueq, Uanis(O35) \\sim Ueq, Uanis(O27) \\sim Ueq, Uanis(O4W) \\sim Ueq,
Uanis(O9W) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(N16) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.001
4. Others
 Sof(O3A)=1-FVAR(1)
 Sof(O3)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 N4(H4), N7(H7), N8(H8), N18(H18), N19(H19), N23(H23), N30(H30), N31(H31),
 C1(H1), C13(H13), C15(H15), C19(H19A), C20(H20), C22(H22), C23(H23A), C24(H24),
  C25(H25), C26(H26), C27(H27), C29(H29), C31(H31A), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41),
  C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48),
 C49(H49), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56),
  C57(H57), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63),
 C64(H64), C65(H65), C68(H68), C69(H69), C72(H72), C73(H73), C74(H74), C82(H82),
  C83(H83), C84(H84), C85(H85), C86(H86), C87(H87), C88(H88), C89(H89),
 C90(H90), C91(H91), C92(H92), C93(H93)
;
_shelx_res_checksum              19140
_shelx_hkl_checksum              80457
_shelx_fab_checksum              66722
_olex2_submission_special_instructions 'No special instructions were received'