Structural features and antiproliferative activity of Pd(II) complexes with halogenated ligands: a comparative study between Schiff base and reduced Schiff base complexes.
Forooghi, Kimia; Amiri Rudbari, Hadi; Stagno, Claudio; Iraci, Nunzio; Cuevas-Vicario, José V; Kordestani, Nazanin; Schirmeister, Tanja; Efferth, Thomas; Omer, Ejlal A.; Moini, Nakisa; Aryaeifar, Mahnaz; Blacque, Olivier; Azadbakht, Reza; Micale, Nicola; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10571–10591; doi:10.1039/d4dt00132j

data_7716173
_publ_section_title
;
 Structural features and antiproliferative activity of Pd(II) complexes
 with halogenated ligands: a comparative study between Schiff base and
 reduced Schiff base complexes.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10571
_journal_page_last               10591
_journal_paper_doi               10.1039/d4dt00132j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C14 H14 Br Cl3 N2 O Pd, C2 H3 N'
_chemical_formula_sum            'C16 H17 Br Cl3 N3 O Pd'
_chemical_formula_weight         559.98
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-07
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-08-28 deposited with the CCDC.	2024-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                114.694(2)
_cell_angle_beta                 98.595(2)
_cell_angle_gamma                96.125(2)
_cell_formula_units_Z            2
_cell_length_a                   8.6207(2)
_cell_length_b                   10.6773(2)
_cell_length_c                   11.9875(3)
_cell_measurement_reflns_used    17907
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      33.3210
_cell_measurement_theta_min      3.2200
_cell_volume                     973.51(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -5.00  64.00   0.50    1.40    --   10.95  57.00  60.00  138
  2  \w     -5.00  84.00   0.50    1.40    --   10.95  57.00 -60.00  178
  3  \w     -3.00  90.00   0.50    1.40    --   10.95  38.00-180.00  186
  4  \w    -43.00  14.00   0.50    1.40    --  -11.88  94.00  43.13  114
  5  \w    -28.00  61.00   0.50    1.40    --  -11.88  57.00  30.00  178
  6  \w    -35.00  62.00   0.50    1.40    --  -11.88  77.00-150.00  194
  7  \w    -90.00   4.00   0.50    1.40    --  -11.88 -38.00-120.00  188
  8  \w    -23.00  22.00   0.50    1.40    --  -11.88 -99.00-150.00   90
  9  \w    -23.00  22.00   0.50    1.40    --  -11.88 -99.00 -60.00   90
 10  \w    -23.00  22.00   0.50    1.40    --  -11.88 -99.00 150.00   90
 11  \w     11.00  59.00   0.50    1.40    --   10.95-124.00   7.00   96
 12  \w     14.00  62.00   0.50    1.40    --   10.95-129.00  41.58   96
 13  \w     39.00  90.00   0.50    1.40    --   10.95-178.00 -90.00  102
 14  \w     24.00  73.00   0.50    1.40    --   10.95-147.00-158.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0678443000
_diffrn_orient_matrix_UB_12      -0.0465801000
_diffrn_orient_matrix_UB_13      -0.0455443000
_diffrn_orient_matrix_UB_21      0.0418933000
_diffrn_orient_matrix_UB_22      -0.0077163000
_diffrn_orient_matrix_UB_23      -0.0484157000
_diffrn_orient_matrix_UB_31      0.0286542000
_diffrn_orient_matrix_UB_32      -0.0575614000
_diffrn_orient_matrix_UB_33      0.0052986000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30934
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.150
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.427
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_correction_T_min  0.486
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.910
_exptl_crystal_description       plate
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         5955
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0235
_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^)+(0.0244P)^2^+0.6000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0546
_refine_ls_wR_factor_ref         0.0557
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5362
_reflns_number_total             5955
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00132j2.cif
_cod_data_source_block           hadi0402
_cod_depositor_comments
'Adding full bibliography for 7716171--7716173.cif.'
_cod_database_code               7716173
_shelx_estimated_absorpt_t_max   0.847
_shelx_estimated_absorpt_t_min   0.458
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H,H,H,H) groups
2. Restrained distances
 N3A-C16A = N3B-C16B
 1.15 with sigma of 0.003
 C16B-C15 = C16A-C15
 1.45 with sigma of 0.003
 O1-H1A
 0.82 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C15 \\sim C16A \\sim N3A \\sim C16B \\sim N3B: within 3A with sigma of 0.005
and sigma for terminal atoms of 0.01 within 3A
4. Others
 Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16B)=Sof(N3B)=1-FVAR(1)
 Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16A)=Sof(N3A)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C12(H12), C14(H14)
5.c Idealised Me refined as rotating group:
 C15(H15D,H15E,H15F), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              54967