Role of hydrazone substituents in determining the nuclearity and antibacterial activity of Zn(II) complexes with pyrazolone-based hydrazones
Marchetti, Fabio; Pettinari, Riccardo; Verdicchio, Federico; Tombesi, Alessia; Scuri, Stefania; Xhafa, Sonila; Olivieri, Laura; Pettinari, Claudio; Choquesillo-Lazarte, Duane; García-García, Amalia; Rodríguez Diéguez, Antonio; Galindo, Agustin; Dalton Transactions  (2022) –; doi:10.1039/D2DT02430F

data_7711052
_publ_section_title
;
 Role of hydrazone substituents in determining the nuclearity and
 antibacterial activity of Zn(II) complexes with pyrazolone-based
 hydrazones
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02430F
_journal_year                    2022
_chemical_formula_moiety         'C48 H44 N8 O6 S2 Zn, 2[CH4O]'
_chemical_formula_sum            'C50 H52 N8 O8 S2 Zn'
_chemical_formula_weight         1022.48
_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
_audit_creation_date             2022-02-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-03-13 deposited with the CCDC.	2022-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.95(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.44(3)
_cell_length_b                   13.34(2)
_cell_length_c                   22.28(4)
_cell_measurement_reflns_used    2677
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      22.20
_cell_measurement_theta_min      2.31
_cell_volume                     4984(14)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.979
_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  0.0480
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            12211
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.036
_diffrn_reflns_theta_min         2.018
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.637
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0856 before and 0.0639 after correction.
The Ratio of minimum to maximum transmission is 0.7873.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2136
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         4833
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0561
_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^)+(0.0672P)^2^+3.4724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1585
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3522
_reflns_number_total             4833
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02430f2.cif
_cod_data_source_block           Complex2
_cod_original_cell_volume        4987(16)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7711052
_shelx_shelxl_version_number     2019/1
_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. Rigid body (RIGU) restrains
 C19A, C20A, C21A, C22A, C23A, C24A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C19B, C20B, C21B, C22B, C23B, C24B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C19B)=Sof(C20B)=Sof(H20B)=Sof(C21B)=Sof(H21B)=Sof(C22B)=Sof(H22B)=
 Sof(C23B)=Sof(H23B)=Sof(C24B)=Sof(H24B)=1-FVAR(1)
 Sof(C19A)=Sof(C24A)=Sof(H24A)=Sof(C23A)=Sof(H23A)=Sof(C22A)=Sof(H22A)=
 Sof(C21A)=Sof(H21A)=Sof(C20A)=Sof(H20A)=FVAR(1)
4.a Riding coordinates:
 N2(H2)
4.b Aromatic/amide H refined with riding coordinates:
 N4(H4), C6(H6), C10(H10), C7(H7), C12(H12), C16(H16), C8(H8), C15(H15),
 C9(H9), C13(H13), C20B(H20B), C21B(H21B), C22B(H22B), C23B(H23B), C24B(H24B),
 C24A(H24A), C23A(H23A), C22A(H22A), C21A(H21A), C20A(H20A)
4.c Fitted hexagon refined as free rotating group:
 C19B(C20B,C21B,C22B,C23B,C24B), C19A(C24A,C23A,C22A,C21A,C20A)
4.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C17(H17A,H17B,H17C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 136 electrons were 
found in a volume of 716\%A^3^ in 1 void per unit cell.
This is consistent with the presence of 2[CH4O] per 
Asymmetric Unit which account for 144 electrons per 
unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              62925
_shelx_hkl_checksum              31414
_shelx_fab_checksum              40652
_olex2_submission_special_instructions 'No special instructions were received'