Impact of the Zinc complexation of polytopic polyaza ligands on the interaction with double and single stranded DNA/RNA and antimicrobial activity
Gonzalez, Jorge; Galiana, Carolina; Dea-Ayuela, M. Auxiliadora; Radic Stojkovic, Marijana; López-Molina, Sonia; Galiana-Rosello, Cristina; Blasco, Salvador; Piantanida, Ivo; García-España, Enrique; Dalton Transactions  (2023) –; doi:10.1039/D3DT00395G

data_7712678
_publ_section_title
;
 Impact of the Zinc complexation of polytopic polyaza ligands on the
 interaction with double and single stranded DNA/RNA and antimicrobial
 activity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00395G
_journal_year                    2023
_chemical_formula_moiety         'C66 H102 Cl2 N22 Na Zn4, 7(Cl O4), 2(H2 O)'
_chemical_formula_sum            'C66 H106 Cl9 N22 Na O30 Zn4'
_chemical_formula_weight         2291.24
_chemical_name_systematic        znpypod
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-07-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-07-18 deposited with the CCDC.	2023-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1143(2)
_cell_length_b                   18.5283(2)
_cell_length_c                   38.6732(5)
_cell_measurement_reflns_used    195581
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      34.972
_cell_measurement_theta_min      2.910
_cell_volume                     9397.0(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0630182
_diffrn_orient_matrix_UB_12      0.0022235
_diffrn_orient_matrix_UB_13      -0.0145195
_diffrn_orient_matrix_UB_21      0.0366252
_diffrn_orient_matrix_UB_22      -0.0308688
_diffrn_orient_matrix_UB_23      0.0171944
_diffrn_orient_matrix_UB_31      -0.0224000
_diffrn_orient_matrix_UB_32      -0.0442165
_diffrn_orient_matrix_UB_33      -0.0127341
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1013
_diffrn_reflns_av_unetI/netI     0.0778
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            58315
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         3.045
_exptl_absorpt_coefficient_mu    1.357
_exptl_absorpt_correction_T_max  0.9274
_exptl_absorpt_correction_T_min  0.4225
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
MULABS - Empirical Correction for Absorption Anisotropy. 
c.f. R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_description       plate
_exptl_crystal_F_000             4720
_exptl_crystal_size_max          0.803
_exptl_crystal_size_mid          0.339
_exptl_crystal_size_min          0.059
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         10672
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1386
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1289P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1978
_refine_ls_wR_factor_ref         0.2313
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5471
_reflns_number_total             10672
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00395g2.cif
_cod_data_source_block           pypzn
_cod_database_code               7712678
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.409
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All O(H,H) groups
2. Restrained distances
 O2-H2C = O2-H2D
 0.82 with sigma of 0.02
 Cl1-O11 \\sim Cl1-O12 \\sim Cl1-O13 \\sim Cl1-O14
 with sigma of 0.02
 O11-O12 \\sim O11-O13 \\sim O11-O14 \\sim O12-O13 \\sim O12-O14 \\sim O13-O14
 with sigma of 0.02
3. Rigid bond restraints
 N3, C6, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(O13) \\sim Ueq, Uanis(O14) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(Na1) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O2) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Others
 Fixed X: H2C(0.69044) H2D(0.747869)
 Fixed Y: H2C(0.14529) H2D(0.14423)
 Fixed Z: H2C(0.118761) H2D(0.15437)
6.a Ternary CH refined with riding coordinates:
 N2(H2), N3(H3), N5(H5), N8(H8), N9(H9), N11(H11)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C20(H20A,H20B), C21(H21A,H21B),
  C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,
 H26B), C27(H27A,H27B), C28(H28A,H28B)
6.c Aromatic/amide H refined with riding coordinates:
 C8(H8A), C9(H9A), C10(H10), C16(H16), C17(H17), C18(H18), C30(H30), C31(H31),
 C32(H32)
;
_shelx_res_checksum              99296
_olex2_date_sample_completion    2010-06-12
_olex2_date_sample_data_collection 2010-06-11
_olex2_date_sample_submission    2010-06-11
_olex2_submission_original_sample_id pypzn
_olex2_submission_special_instructions 'No special instructions were received'