Palladium (II) complexes with thiosemicarbazones derived from pyrene as topoisomerase IB inhibitors
Oliveira, Carolina Gonçalves; Romero-Canelon, Isolda; Silva, Monize M.; Coverdale, James; da Silva Maia, Pedro Ivo; Batista, Alzir A.; Castelli, Silvia; Desideri, Alessandro; Sadler, Peter J.; Deflon, Victor Marcelo Marcelo; Dalton Transactions  (2019) –; doi:10.1039/C9DT02570G

data_7701458
_publ_section_title
;
 Palladium (II) complexes with thiosemicarbazones derived from pyrene as
 topoisomerase IB inhibitors
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT02570G
_journal_year                    2019
_chemical_formula_sum            'C40 H34 N6 S2'
_chemical_formula_weight         662.85
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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   mixed
_audit_creation_method           SHELXL-2016/4
_audit_update_record
;
2018-09-09 deposited with the CCDC.    2019-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                94.574(2)
_cell_angle_beta                 92.802(2)
_cell_angle_gamma                112.551(2)
_cell_formula_units_Z            2
_cell_length_a                   7.8769(3)
_cell_length_b                   8.6861(3)
_cell_length_c                   26.3559(10)
_cell_measurement_reflns_used    3777
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.96
_cell_measurement_theta_min      2.33
_cell_volume                     1653.88(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0343
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            20426
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.078
_diffrn_reflns_theta_max         25.078
_diffrn_reflns_theta_min         1.556
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       Needle
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         5829
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0619P)^2^+0.5873P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1296
_refine_ls_wR_factor_ref         0.1521
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3569
_reflns_number_total             5829
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02570g2.cif
_cod_data_source_block           shelx_CCDC2
_cod_database_code               7701458
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.889
_shelx_estimated_absorpt_t_max   0.984
_shelx_res_checksum              64341