Cytotoxic activity of copper(ii), nickel(ii) and platinum(ii) thiosemicarbazone derivatives: interaction with DNA and the H2A histone peptide.
Bisceglie, Franco; Orsoni, Nicolò; Pioli, Marianna; Bonati, Beatrice; Tarasconi, Pieralberto; Rivetti, Claudio; Amidani, Davide; Montalbano, Serena; Buschini, Annamaria; Pelosi, Giorgio; Metallomics : integrated biometal science 11 (2019) 1729–1742; doi:10.1039/c9mt00166b

data_1552277
_publ_section_title
;
 Cytotoxic activity of copper(ii), nickel(ii) and platinum(ii)
 thiosemicarbazone derivatives: interaction with DNA and the H2A histone
 peptide.
;
_journal_issue                   10
_journal_name_full               'Metallomics : integrated biometal science'
_journal_page_first              1729
_journal_page_last               1742
_journal_paper_doi               10.1039/c9mt00166b
_journal_volume                  11
_journal_year                    2019
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C22 H40 N6 Pt S2, 2(C2 H6 O S)'
_chemical_formula_sum            'C26 H52 N6 O2 Pt S4'
_chemical_formula_weight         804.06
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-28 deposited with the CCDC.    2019-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                86.03
_cell_angle_beta                 75.35
_cell_angle_gamma                79.55
_cell_formula_units_Z            1
_cell_length_a                   6.189
_cell_length_b                   12.221
_cell_length_c                   12.196
_cell_measurement_reflns_used    118
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19
_cell_measurement_theta_min      12
_cell_volume                     877.396
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker AXS CCD diffractometer'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12082
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.555
_diffrn_reflns_theta_min         1.695
_exptl_absorpt_coefficient_mu    4.267
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4008
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2007/4 (Bruker,2007/4) was used for absorption correction.
wR2(int) was 0.1315 before and 0.0554 after correction.
The Ratio of minimum to maximum transmission is 0.5375.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       platelet
_exptl_crystal_F_000             408
_exptl_crystal_size_max          .6
_exptl_crystal_size_mid          .5
_exptl_crystal_size_min          .2
_refine_diff_density_max         2.526
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details
;
 Flack x determined using 4048 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.065(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         8671
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0314P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0800
_reflns_Friedel_coverage         0.950
_reflns_Friedel_fraction_full    0.960
_reflns_Friedel_fraction_max     0.943
_reflns_number_gt                8584
_reflns_number_total             8671
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9mt00166b2.cif
_cod_data_source_block           ar3bbt
_cod_depositor_comments          'Adding full bibliography for 1552277.cif.'
_cod_original_cell_volume        877.4
_cod_database_code               1552277
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C15(H15), C4(H4)
2.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C3(H3A,H3B), C17(H17A,H17B), C16(H16A,H16B), C5(H5A,H5B),
 C6(H6A,H6B)
2.c Me refined with riding coordinates:
 C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C24(H24A,H24B,H24C), C26(H26A,H26B,
 H26C)
2.d Aromatic/amide H refined with riding coordinates:
 C13(H13), C2(H2), C7(H7), C18(H18)
2.e X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N4(H4A,H4B)
2.f Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C22(H22A,H22B,
 H22C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_olex2_submission_special_instructions 'No special instructions were received'