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#$Date: 2025-08-21 12:25:49 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301846 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/69/7006970.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_7006970
loop_
_publ_author_name
'Siedle, Gabriel'
'Kersting, Berthold'
_publ_section_title
;
 Preparation and characterization of dinuclear Pd(II) complexes of
 binucleating tetraaza-thiophenolate ligands.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2114
_journal_page_last               2126
_journal_paper_doi               10.1039/b516071E
_journal_year                    2006
_chemical_compound_source
;
Crystals were grown by recrystallization from a mixed
acetone/methanol solvent system
;
_chemical_formula_structural
;
[(L3)Pd2(OAc)](ClO4)2
;
_chemical_formula_sum            'C22 H36 Cl2 N4 O10 Pd2 S'
_chemical_formula_weight         832.31
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 102.20(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.410(3)
_cell_length_b                   12.245(2)
_cell_length_c                   22.395(4)
_cell_measurement_temperature    210(2)
_cell_volume                     3058.3(11)
_computing_cell_refinement       SMART
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP3 (FARRUGIA)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'BRUKER AXS'
_diffrn_measurement_method       hemisphere
_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  0.1677
_diffrn_reflns_av_sigmaI/netI    0.1194
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            26837
_diffrn_reflns_theta_full        28.77
_diffrn_reflns_theta_max         28.77
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    1.476
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.808
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.288
_refine_diff_density_min         -1.158
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         7412
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1105
_refine_ls_R_factor_gt           0.0563
_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)+(0.0491P)²+1.8932P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1187
_refine_ls_wR_factor_ref         0.1464
_reflns_number_gt                4259
_reflns_number_total             7412
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b516071E.txt
_cod_data_source_block           9
_cod_original_cell_volume        3058.2(11)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7006970
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 1.12458(4) 0.76735(4) 0.90397(2) 0.03494(15) Uani 1 1 d . . .
Pd2 Pd 0.86818(4) 0.83557(4) 0.97322(2) 0.03587(15) Uani 1 1 d . . .
S S 1.01329(14) 0.90355(12) 0.92947(6) 0.0331(3) Uani 1 1 d . . .
O1 O 1.1460(5) 0.7076(5) 0.9902(2) 0.0687(15) Uani 1 1 d . . .
O2 O 0.9507(5) 0.6918(5) 0.9991(3) 0.0697(16) Uani 1 1 d . . .
N1 N 1.1146(5) 0.8200(4) 0.8195(2) 0.0342(11) Uani 1 1 d . . .
N2 N 1.2341(5) 0.6442(4) 0.8803(2) 0.0422(13) Uani 1 1 d . . .
N3 N 0.7729(5) 0.9725(4) 0.9553(2) 0.0382(12) Uani 1 1 d . . .
N4 N 0.7343(5) 0.7882(5) 1.0190(2) 0.0450(14) Uani 1 1 d . . .
C1 C 0.9446(5) 0.9808(4) 0.8661(2) 0.0303(13) Uani 1 1 d . . .
C2 C 0.8473(6) 1.0510(5) 0.8697(3) 0.0346(14) Uani 1 1 d . . .
C3 C 0.8062(6) 1.1272(5) 0.8241(3) 0.0420(16) Uani 1 1 d . . .
H3 H 0.7452 1.1747 0.8289 0.050 Uiso 1 1 calc R . .
C4 C 0.8528(6) 1.1356(5) 0.7714(3) 0.0402(15) Uani 1 1 d . . .
C5 C 0.9433(6) 1.0623(5) 0.7678(3) 0.0385(15) Uani 1 1 d . . .
H5 H 0.9765 1.0654 0.7333 0.046 Uiso 1 1 calc R . .
C6 C 0.9881(6) 0.9852(5) 0.8115(3) 0.0355(14) Uani 1 1 d . . .
C7 C 1.0692(5) 0.9061(5) 0.7934(3) 0.0348(14) Uani 1 1 d . . .
H7 H 1.0913 0.9216 0.7566 0.042 Uiso 1 1 calc R . .
C8 C 1.1755(8) 0.7435(6) 0.7841(3) 0.057(2) Uani 1 1 d . . .
H8A H 1.1173 0.6925 0.7618 0.068 Uiso 1 1 calc R . .
H8B H 1.2095 0.7843 0.7548 0.068 Uiso 1 1 calc R . .
C9 C 1.2684(9) 0.6847(7) 0.8242(4) 0.079(3) Uani 1 1 d . . .
H9A H 1.3378 0.7319 0.8358 0.094 Uiso 1 1 calc R . .
H9B H 1.2919 0.6230 0.8022 0.094 Uiso 1 1 calc R . .
C10 C 1.1675(9) 0.5401(7) 0.8687(5) 0.088(3) Uani 1 1 d . . .
H10A H 1.2190 0.4848 0.8579 0.132 Uiso 1 1 calc R . .
H10B H 1.0993 0.5497 0.8357 0.132 Uiso 1 1 calc R . .
H10C H 1.1410 0.5183 0.9048 0.132 Uiso 1 1 calc R . .
C11 C 1.3493(8) 0.6296(9) 0.9256(4) 0.091(3) Uani 1 1 d . . .
H11A H 1.3949 0.5720 0.9122 0.136 Uiso 1 1 calc R . .
H11B H 1.3328 0.6111 0.9646 0.136 Uiso 1 1 calc R . .
H11C H 1.3945 0.6963 0.9290 0.136 Uiso 1 1 calc R . .
C12 C 0.7758(6) 1.0476(5) 0.9167(3) 0.0386(15) Uani 1 1 d . . .
H12 H 0.7268 1.1077 0.9186 0.046 Uiso 1 1 calc R . .
C13 C 0.6876(7) 0.9824(6) 0.9968(3) 0.0519(19) Uani 1 1 d . . .
H13A H 0.6241 1.0335 0.9802 0.062 Uiso 1 1 calc R . .
H13B H 0.7288 1.0083 1.0367 0.062 Uiso 1 1 calc R . .
C14 C 0.6371(6) 0.8707(6) 1.0018(3) 0.0518(18) Uani 1 1 d . . .
H14A H 0.5881 0.8715 1.0323 0.062 Uiso 1 1 calc R . .
H14B H 0.5862 0.8506 0.9629 0.062 Uiso 1 1 calc R . .
C15 C 0.6869(8) 0.6777(6) 1.0020(4) 0.062(2) Uani 1 1 d . . .
H15A H 0.6263 0.6604 1.0244 0.093 Uiso 1 1 calc R . .
H15B H 0.7509 0.6255 1.0116 0.093 Uiso 1 1 calc R . .
H15C H 0.6528 0.6755 0.9590 0.093 Uiso 1 1 calc R . .
C16 C 0.7873(8) 0.7903(7) 1.0859(3) 0.064(2) Uani 1 1 d . . .
H16A H 0.7276 0.7689 1.1081 0.095 Uiso 1 1 calc R . .
H16B H 0.8145 0.8629 1.0978 0.095 Uiso 1 1 calc R . .
H16C H 0.8538 0.7406 1.0949 0.095 Uiso 1 1 calc R . .
C17 C 0.8025(7) 1.2187(6) 0.7224(3) 0.055(2) Uani 1 1 d . . .
C18 C 0.8143(9) 1.3320(6) 0.7485(4) 0.077(3) Uani 1 1 d . . .
H18A H 0.7738 1.3360 0.7819 0.116 Uiso 1 1 calc R . .
H18B H 0.7789 1.3833 0.7175 0.116 Uiso 1 1 calc R . .
H18C H 0.8976 1.3491 0.7628 0.116 Uiso 1 1 calc R . .
C19 C 0.8684(10) 1.2153(7) 0.6697(4) 0.087(3) Uani 1 1 d . . .
H19A H 0.8613 1.1437 0.6518 0.130 Uiso 1 1 calc R . .
H19B H 0.9515 1.2322 0.6848 0.130 Uiso 1 1 calc R . .
H19C H 0.8338 1.2680 0.6393 0.130 Uiso 1 1 calc R . .
C20 C 0.6691(9) 1.1923(9) 0.6984(4) 0.096(3) Uani 1 1 d . . .
H20A H 0.6279 1.1951 0.7316 0.144 Uiso 1 1 calc R . .
H20B H 0.6614 1.1205 0.6808 0.144 Uiso 1 1 calc R . .
H20C H 0.6347 1.2449 0.6679 0.144 Uiso 1 1 calc R . .
C21 C 1.0635(7) 0.6747(6) 1.0176(3) 0.0462(17) Uani 1 1 d . . .
C22 C 1.0974(8) 0.6088(9) 1.0743(4) 0.090(3) Uani 1 1 d . . .
H22A H 1.0265 0.5900 1.0888 0.134 Uiso 1 1 calc R . .
H22B H 1.1504 0.6504 1.1050 0.134 Uiso 1 1 calc R . .
H22C H 1.1370 0.5432 1.0659 0.134 Uiso 1 1 calc R . .
Cl1 Cl 1.4092(2) 0.99021(18) 0.82924(10) 0.0708(6) Uani 1 1 d . . .
Cl2 Cl 1.44735(17) 0.63874(15) 1.11366(8) 0.0521(5) Uani 1 1 d . . .
O3 O 1.5082(8) 1.0523(10) 0.8315(6) 0.190(5) Uani 1 1 d . . .
O4 O 1.3915(8) 0.9180(7) 0.7794(3) 0.127(3) Uani 1 1 d . . .
O5 O 1.4111(9) 0.9294(7) 0.8825(3) 0.132(3) Uani 1 1 d . . .
O6 O 1.3071(8) 1.0562(7) 0.8195(4) 0.129(3) Uani 1 1 d . . .
O7 O 1.4023(7) 0.5429(6) 1.0833(4) 0.110(2) Uani 1 1 d . . .
O8 O 1.3906(6) 0.6617(6) 1.1624(3) 0.099(2) Uani 1 1 d . . .
O9 O 1.5723(5) 0.6272(6) 1.1364(3) 0.0841(19) Uani 1 1 d . . .
O10 O 1.4223(7) 0.7275(5) 1.0716(3) 0.088(2) Uani 1 1 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'
O O 0.0106 0.0060 '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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
N1 Pd1 O1 175.8(2) . . ?
N1 Pd1 N2 84.83(19) . . ?
O1 Pd1 N2 91.3(2) . . ?
N1 Pd1 S 94.58(14) . . ?
O1 Pd1 S 89.24(16) . . ?
N2 Pd1 S 177.81(16) . . ?
N3 Pd2 O2 172.47(19) . . ?
N3 Pd2 N4 84.7(2) . . ?
O2 Pd2 N4 87.8(2) . . ?
N3 Pd2 S 91.21(15) . . ?
O2 Pd2 S 96.06(15) . . ?
N4 Pd2 S 173.87(16) . . ?
C1 S Pd1 112.15(18) . . ?
C1 S Pd2 108.0(2) . . ?
Pd1 S Pd2 110.10(7) . . ?
C21 O1 Pd1 127.6(5) . . ?
C21 O2 Pd2 127.5(5) . . ?
C7 N1 C8 118.1(5) . . ?
C7 N1 Pd1 130.5(4) . . ?
C8 N1 Pd1 111.3(4) . . ?
C9 N2 C10 111.0(7) . . ?
C9 N2 C11 105.3(7) . . ?
C10 N2 C11 111.3(7) . . ?
C9 N2 Pd1 104.6(4) . . ?
C10 N2 Pd1 110.6(5) . . ?
C11 N2 Pd1 113.6(5) . . ?
C12 N3 C13 118.8(5) . . ?
C12 N3 Pd2 131.0(4) . . ?
C13 N3 Pd2 110.1(4) . . ?
C15 N4 C14 110.0(6) . . ?
C15 N4 C16 108.9(6) . . ?
C14 N4 C16 111.7(5) . . ?
C15 N4 Pd2 113.1(4) . . ?
C14 N4 Pd2 105.4(4) . . ?
C16 N4 Pd2 107.7(4) . . ?
C6 C1 C2 116.6(5) . . ?
C6 C1 S 122.9(4) . . ?
C2 C1 S 120.3(4) . . ?
C3 C2 C1 120.7(5) . . ?
C3 C2 C12 113.3(5) . . ?
C1 C2 C12 125.8(5) . . ?
C2 C3 C4 122.7(6) . . ?
C5 C4 C3 115.1(6) . . ?
C5 C4 C17 124.5(6) . . ?
C3 C4 C17 120.4(6) . . ?
C6 C5 C4 124.9(5) . . ?
C5 C6 C1 119.7(5) . . ?
C5 C6 C7 114.9(5) . . ?
C1 C6 C7 125.1(5) . . ?
N1 C7 C6 130.6(5) . . ?
C9 C8 N1 110.5(6) . . ?
C8 C9 N2 114.1(7) . . ?
N3 C12 C2 127.6(6) . . ?
N3 C13 C14 106.6(5) . . ?
N4 C14 C13 111.2(6) . . ?
C18 C17 C4 110.4(6) . . ?
C18 C17 C19 107.9(7) . . ?
C4 C17 C19 111.6(6) . . ?
C18 C17 C20 109.3(8) . . ?
C4 C17 C20 107.9(6) . . ?
C19 C17 C20 109.7(8) . . ?
O2 C21 O1 125.3(6) . . ?
O2 C21 C22 115.3(6) . . ?
O1 C21 C22 119.4(7) . . ?
O3 Cl1 O6 110.1(7) . . ?
O3 Cl1 O5 113.8(7) . . ?
O6 Cl1 O5 107.6(5) . . ?
O3 Cl1 O4 111.2(6) . . ?
O6 Cl1 O4 105.4(6) . . ?
O5 Cl1 O4 108.3(5) . . ?
O7 Cl2 O8 111.2(5) . . ?
O7 Cl2 O9 109.2(4) . . ?
O8 Cl2 O9 109.5(4) . . ?
O7 Cl2 O10 108.5(4) . . ?
O8 Cl2 O10 107.4(4) . . ?
O9 Cl2 O10 111.1(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 N1 1.979(5) . ?
Pd1 O1 2.031(5) . ?
Pd1 N2 2.097(5) . ?
Pd1 S 2.2421(15) . ?
Pd2 N3 1.993(5) . ?
Pd2 O2 2.022(5) . ?
Pd2 N4 2.093(5) . ?
Pd2 S 2.2538(16) . ?
S C1 1.747(6) . ?
O1 C21 1.292(8) . ?
O2 C21 1.283(8) . ?
N1 C7 1.262(7) . ?
N1 C8 1.490(7) . ?
N2 C9 1.478(9) . ?
N2 C10 1.478(10) . ?
N2 C11 1.491(10) . ?
N3 C12 1.267(7) . ?
N3 C13 1.486(7) . ?
N4 C15 1.477(9) . ?
N4 C14 1.491(9) . ?
N4 C16 1.494(8) . ?
C1 C6 1.415(7) . ?
C1 C2 1.420(8) . ?
C2 C3 1.390(9) . ?
C2 C12 1.462(8) . ?
C3 C4 1.399(8) . ?
C4 C5 1.382(8) . ?
C4 C17 1.517(9) . ?
C5 C6 1.379(8) . ?
C6 C7 1.455(8) . ?
C8 C9 1.431(11) . ?
C13 C14 1.497(10) . ?
C17 C18 1.501(11) . ?
C17 C19 1.528(9) . ?
C17 C20 1.537(13) . ?
C21 C22 1.487(10) . ?
Cl1 O3 1.354(9) . ?
Cl1 O6 1.396(8) . ?
Cl1 O5 1.402(7) . ?
Cl1 O4 1.405(7) . ?
Cl2 O7 1.399(7) . ?
Cl2 O8 1.410(5) . ?
Cl2 O9 1.416(6) . ?
Cl2 O10 1.427(6) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139152459
