Cationic Palladium(II)-Indenyl complexes bearing phosphines as ancillary ligands: synthesis, study of indenyl amination and anticancer activity
Scattolin, Thomas; Visentin, Fabiano; Bortolamiol, Enrica; Caligiuri, Isabella; Rizzolio, Flavio; Cavallo, Luigi; Zhang, Ziyun; Demitri, Nicola; Fama, Francesco; Dalton Transactions  (2022) –; doi:10.1039/D2DT01821G

data_7710633
_publ_section_title
;
 Cationic Palladium(II)-Indenyl complexes bearing phosphines as ancillary
 ligands: synthesis, study of indenyl amination and anticancer activity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01821G
_journal_year                    2022
_chemical_formula_moiety         'C35 H31 P2 Pd, C F3 S O3'
_chemical_formula_sum            'C36 H31 F3 O3 P2 Pd S'
_chemical_formula_weight         769.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-05-19 deposited with the CCDC.	2022-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.15(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.873(2)
_cell_length_b                   13.529(3)
_cell_length_c                   12.606(3)
_cell_measurement_reflns_used    7427
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.099
_cell_measurement_theta_min      1.460
_cell_volume                     1625.3(7)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'Elettra XRD2 Data Collection SW'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'Ortep3 for Windows - Coot'
_computing_publication_material  'enCIFer - publCIF'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type
;
'Arinax MD2s Goniometer, Pilatus 6M detector'
;
_diffrn_measurement_method       'Rotating crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.620
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            39534
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_theta_full        21.839
_diffrn_reflns_theta_max         31.099
_diffrn_reflns_theta_min         1.460
_diffrn_source                   'Elettra Synchrotron - XRD2 BL'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.539
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_description       'Thick rods'
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Flack x determined using 6510 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.008(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         14004
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0227
_refine_ls_R_factor_gt           0.0226
_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^)+(0.0310P)^2^+0.3499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0607
_reflns_Friedel_coverage         0.892
_reflns_Friedel_fraction_full    0.984
_reflns_Friedel_fraction_max     0.868
_reflns_number_gt                13919
_reflns_number_total             14004
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01821g2.cif
_cod_data_source_block           EB2
_cod_original_cell_volume        1625.3(6)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7710633
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.948
_shelx_estimated_absorpt_t_max   0.989
_shelx_res_checksum              54998
_shelx_hkl_checksum              64792