#------------------------------------------------------------------------------
#$Date: 2025-08-04 09:03:09 +0200 (Mon 04 de Aug de 2025) $
#$Revision: 301442 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/52/7055219.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7055219
loop_
_publ_author_name
'Spodine, Evgenia'
'Hernández, Wilfredo'
'Vaisberg, Abraham'
'Tobar, Mabel'
'Alvarez, Melisa'
'Manzur, Jorge'
'Echevarría, Yuri'
_publ_section_title
;
 In Vitro Antiproliferative Activity of Palladium(II) Thiosemicarbazone
 Complexes and the Corresponding Functionalized Chitosan Coated Magnetite
 Nanoparticles
;
_journal_issue                   2
_journal_name_full               'New J. Chem.'
_journal_page_first              1853
_journal_page_last               1860
_journal_paper_doi               10.1039/C5NJ02429C
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C36 H28 N6 Pd S2, 4(C3 H6 O)'
_chemical_formula_sum            'C48 H52 N6 O4 Pd S2'
_chemical_formula_weight         947.50
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-09-09 deposited with the CCDC.
2015-12-10 downloaded from the CCDC.
;
_cell_angle_alpha                80.061(9)
_cell_angle_beta                 80.638(9)
_cell_angle_gamma                82.591(9)
_cell_formula_units_Z            1
_cell_length_a                   7.957(5)
_cell_length_b                   9.112(5)
_cell_length_c                   16.833(10)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      48.579
_cell_measurement_theta_min      4.845
_cell_volume                     1179.7(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0556
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9945
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.530
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.821
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Orenge
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.037
_refine_diff_density_min         -1.218
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         5103
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0975P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1525
_reflns_number_gt                4424
_reflns_number_total             5103
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj02429c2.cif
_cod_data_source_block           aijm_c3_ab1
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7055219
#BEGIN Tags that were not found in dictionaries:
_publcif_datablock.id            {d9eb1296-3fc6-4e21-a547-51486f56eaae}
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pd1 Pd 1.0000 0.0000 0.5000 0.03500(15) Uani 1 2 d S
S1 S 0.80444(12) -0.02146(11) 0.61536(6) 0.0496(3) Uani 1 1 d .
C1 C 0.9088(4) -0.1800(4) 0.6660(2) 0.0387(7) Uani 1 1 d .
C2 C 0.8713(5) -0.3606(4) 0.7957(2) 0.0455(8) Uani 1 1 d .
C3 C 0.7923(7) -0.3655(6) 0.8748(3) 0.0682(12) Uani 1 1 d .
H3 H 0.7138 -0.2862 0.8890 0.082 Uiso 1 1 calc R
C4 C 0.8276(9) -0.4862(7) 0.9334(3) 0.0899(18) Uani 1 1 d .
H4 H 0.7724 -0.4893 0.9867 0.108 Uiso 1 1 calc R
C5 C 0.9472(8) -0.6038(6) 0.9118(3) 0.0848(16) Uani 1 1 d .
H5 H 0.9733 -0.6855 0.9508 0.102 Uiso 1 1 calc R
C6 C 1.0245(7) -0.5987(5) 0.8344(3) 0.0703(13) Uani 1 1 d .
H6 H 1.1046 -0.6773 0.8206 0.084 Uiso 1 1 calc R
C7 C 0.9879(6) -0.4788(5) 0.7746(3) 0.0564(10) Uani 1 1 d .
H7 H 1.0410 -0.4779 0.7211 0.068 Uiso 1 1 calc R
C8 C 0.7190(4) 0.2334(4) 0.4626(2) 0.0400(8) Uani 1 1 d .
H8 H 0.6671 0.1868 0.5125 0.048 Uiso 1 1 calc R
C9 C 0.6200(4) 0.3637(4) 0.4231(2) 0.0386(7) Uani 1 1 d .
C10 C 0.6773(4) 0.5101(4) 0.4055(2) 0.0383(7) Uani 1 1 d .
C11 C 0.8322(5) 0.5406(4) 0.4262(2) 0.0446(8) Uani 1 1 d .
H11 H 0.9028 0.4632 0.4514 0.053 Uiso 1 1 calc R
C12 C 0.8798(6) 0.6823(5) 0.4097(3) 0.0557(10) Uani 1 1 d .
H12 H 0.9830 0.7006 0.4234 0.067 Uiso 1 1 calc R
C13 C 0.7755(6) 0.8004(5) 0.3724(3) 0.0639(11) Uani 1 1 d .
H13 H 0.8094 0.8966 0.3614 0.077 Uiso 1 1 calc R
C14 C 0.6234(6) 0.7746(5) 0.3521(3) 0.0598(11) Uani 1 1 d .
H14 H 0.5546 0.8537 0.3271 0.072 Uiso 1 1 calc R
C15 C 0.5697(5) 0.6292(4) 0.3687(2) 0.0449(8) Uani 1 1 d .
C16 C 0.4103(5) 0.6029(5) 0.3521(2) 0.0538(10) Uani 1 1 d .
H16 H 0.3406 0.6816 0.3274 0.065 Uiso 1 1 calc R
C17 C 0.3563(5) 0.4649(5) 0.3715(3) 0.0553(10) Uani 1 1 d .
H17 H 0.2494 0.4495 0.3608 0.066 Uiso 1 1 calc R
C18 C 0.4612(5) 0.3446(4) 0.4078(2) 0.0479(9) Uani 1 1 d .
H18 H 0.4222 0.2503 0.4217 0.057 Uiso 1 1 calc R
C19 C 0.3517(6) 0.8359(6) 0.8091(3) 0.0681(12) Uani 1 1 d .
C20 C 0.3623(9) 0.6721(7) 0.8154(4) 0.103(2) Uani 1 1 d .
H20A H 0.4795 0.6328 0.8020 0.155 Uiso 1 1 calc R
H20B H 0.2948 0.6469 0.7783 0.155 Uiso 1 1 calc R
H20C H 0.3196 0.6296 0.8701 0.155 Uiso 1 1 calc R
C21 C 0.1803(8) 0.9185(9) 0.8285(5) 0.110(2) Uani 1 1 d .
H21A H 0.1925 1.0224 0.8270 0.166 Uiso 1 1 calc R
H21B H 0.1284 0.8775 0.8819 0.166 Uiso 1 1 calc R
H21C H 0.1092 0.9088 0.7891 0.166 Uiso 1 1 calc R
C22 C 0.3954(11) 0.8377(9) 0.0627(6) 0.111(2) Uani 1 1 d .
C23 C 0.5193(16) 0.7521(13) 0.1125(7) 0.205(6) Uani 1 1 d .
H23A H 0.5010 0.6480 0.1217 0.308 Uiso 1 1 calc R
H23B H 0.5054 0.7879 0.1638 0.308 Uiso 1 1 calc R
H23C H 0.6332 0.7640 0.0847 0.308 Uiso 1 1 calc R
C24 C 0.2627(12) 0.9305(12) 0.1004(9) 0.212(6) Uani 1 1 d .
H24A H 0.3083 1.0161 0.1117 0.319 Uiso 1 1 calc R
H24B H 0.2112 0.8758 0.1504 0.319 Uiso 1 1 calc R
H24C H 0.1779 0.9633 0.0647 0.319 Uiso 1 1 calc R
N1 N 0.8255(4) -0.2346(4) 0.73943(19) 0.0473(8) Uani 1 1 d D
N2 N 1.0579(4) -0.2456(3) 0.63873(18) 0.0412(7) Uani 1 1 d .
N3 N 0.8697(3) 0.1754(3) 0.43648(17) 0.0370(6) Uani 1 1 d .
O1 O 0.4770(4) 0.9018(4) 0.7877(2) 0.0827(10) Uani 1 1 d .
O2 O 0.4130(10) 0.8231(9) -0.0068(4) 0.175(3) Uani 1 1 d .
H1N H 0.730(4) -0.191(5) 0.761(3) 0.075(15) Uiso 1 1 d D
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N3 Pd1 N3 180.00(15) 2_756 .
N3 Pd1 S1 96.89(9) 2_756 2_756
N3 Pd1 S1 83.11(9) . 2_756
N3 Pd1 S1 83.11(9) 2_756 .
N3 Pd1 S1 96.89(9) . .
S1 Pd1 S1 180.0 2_756 .
C1 S1 Pd1 96.52(12) . .
N2 C1 N1 120.0(3) . .
N2 C1 S1 125.1(3) . .
N1 C1 S1 114.9(3) . .
C3 C2 C7 119.4(4) . .
C3 C2 N1 117.3(4) . .
C7 C2 N1 123.3(4) . .
C2 C3 C4 121.0(5) . .
C3 C4 C5 119.2(5) . .
C6 C5 C4 119.8(4) . .
C5 C6 C7 121.6(5) . .
C2 C7 C6 119.1(4) . .
N3 C8 C9 127.6(3) . .
C18 C9 C10 119.7(3) . .
C18 C9 C8 117.4(3) . .
C10 C9 C8 122.7(3) . .
C11 C10 C15 119.1(3) . .
C11 C10 C9 122.8(3) . .
C15 C10 C9 118.1(3) . .
C12 C11 C10 120.7(4) . .
C11 C12 C13 120.7(4) . .
C14 C13 C12 120.0(4) . .
C13 C14 C15 120.7(4) . .
C16 C15 C10 120.0(3) . .
C16 C15 C14 121.2(4) . .
C10 C15 C14 118.8(3) . .
C17 C16 C15 121.0(4) . .
C16 C17 C18 120.1(4) . .
C9 C18 C17 121.1(4) . .
O1 C19 C20 121.3(5) . .
O1 C19 C21 120.8(5) . .
C20 C19 C21 117.9(5) . .
O2 C22 C24 124.4(11) . .
O2 C22 C23 117.6(9) . .
C24 C22 C23 118.0(9) . .
C1 N1 C2 130.0(3) . .
C1 N2 N3 113.7(3) . 2_756
C8 N3 N2 114.8(3) . 2_756
C8 N3 Pd1 124.0(2) . .
N2 N3 Pd1 121.2(2) 2_756 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 N3 2.029(3) 2_756
Pd1 N3 2.029(3) .
Pd1 S1 2.2792(13) 2_756
Pd1 S1 2.2792(13) .
S1 C1 1.732(4) .
C1 N2 1.308(4) .
C1 N1 1.349(5) .
C2 C3 1.372(6) .
C2 C7 1.383(6) .
C2 N1 1.406(5) .
C3 C4 1.377(7) .
C4 C5 1.395(8) .
C5 C6 1.343(7) .
C6 C7 1.388(6) .
C8 N3 1.287(4) .
C8 C9 1.460(5) .
C9 C18 1.367(5) .
C9 C10 1.433(5) .
C10 C11 1.406(5) .
C10 C15 1.412(5) .
C11 C12 1.363(6) .
C12 C13 1.394(6) .
C13 C14 1.369(6) .
C14 C15 1.412(6) .
C15 C16 1.401(5) .
C16 C17 1.351(6) .
C17 C18 1.404(5) .
C19 O1 1.203(6) .
C19 C20 1.470(8) .
C19 C21 1.486(8) .
C22 O2 1.183(9) .
C22 C24 1.403(11) .
C22 C23 1.459(11) .
N2 N3 1.387(4) 2_756
N3 N2 1.387(4) 2_756
#BEGIN Loops that were not found in dictionaries:
loop_
_publcif_info_exptl_table_extra_item
sin_theta_over_lambda_max
#END Loops that were not found in dictionaries
