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_7701459
_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            'C38 H31 Cl N3 P Pd S'
_chemical_formula_weight         734.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 109.283(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2704(11)
_cell_length_b                   12.0045(8)
_cell_length_c                   21.2465(16)
_cell_measurement_reflns_used    9526
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      2.65
_cell_volume                     3435.5(4)
_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 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0298
_diffrn_reflns_av_unetI/netI     0.0130
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            73175
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.420
_diffrn_reflns_theta_min         1.512
_exptl_absorpt_coefficient_mu    0.756
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       prism
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.590
_exptl_crystal_size_mid          0.540
_exptl_crystal_size_min          0.510
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.0077(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/4 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         7061
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0283
_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^)+(0.0316P)^2^+3.4139P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0766
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6549
_reflns_number_total             7061
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02570g2.cif
_cod_data_source_block           shelx_CCDC3
_cod_database_code               7701459
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.521
_shelx_estimated_absorpt_t_max   0.546
_shelx_res_checksum              50358
_shelx_fab_checksum              23638