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_7710636
_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
'C42 H56 P Pd, Cl O4, 0.75(C4 H10 O), 0.25(C H Cl3)'
_chemical_formula_sum            'C45.25 H63.75 Cl1.75 O4.75 P Pd'
_chemical_formula_weight         883.12
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                96.61(3)
_cell_angle_beta                 101.71(3)
_cell_angle_gamma                100.32(3)
_cell_formula_units_Z            2
_cell_length_a                   10.196(2)
_cell_length_b                   11.919(2)
_cell_length_c                   18.601(4)
_cell_measurement_reflns_used    1035
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.275
_cell_measurement_theta_min      0.987
_cell_volume                     2150.6(8)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'Elettra XRD1 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 0.987
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type
;
'Huber 4-circles Kappa Goniometer, Pilatus 2M detector'
;
_diffrn_measurement_method       'Rotating crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.620
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            117819
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        21.835
_diffrn_reflns_theta_max         32.275
_diffrn_reflns_theta_min         0.987
_diffrn_source                   'Elettra Synchrotron - XRD1 BL'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.426
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_description       'Thin rods'
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.629
_refine_diff_density_min         -1.935
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       0.0177(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         22062
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+1.8393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.1602
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18285
_reflns_number_total             22062
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01821g2.cif
_cod_data_source_block           EB6
_cod_original_cell_volume        2150.5(8)
_cod_database_code               7710636
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.959
_shelx_estimated_absorpt_t_max   0.992
_shelx_res_checksum              45090
_shelx_hkl_checksum              13860