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#$Revision: 301776 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/51/71/1517149.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.
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data_1517149
loop_
_publ_author_name
'Subhi A. Al-Jibori'
'Qusay K.A. Al-Jibori'
'Harry Schmidt'
'Kurt Merzweiler'
'Christoph Wagner'
'Graeme Hogarth'
_publ_section_title
;
 Palladium(II) saccharinate (sac) and thiosaccharinate (tsac) complexes
 with 2-aminopyridine (2-ampy), 2-acetylaminopyridine (2-aampy) and
 2-acetylaminopyrimidine (2-aampym) co-ligands: X-ray crystal structures
 of trans-[Pd(sac)2(ampy)2] and solvatomorphs trans-[Pd(sac)2(2-aampy)2].S
 (S = CHCl3, thf)
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              69
_journal_page_last               74
_journal_volume                  402
_journal_year                    2013
_chemical_formula_sum            'C24 H20 N6 O6 Pd S2'
_chemical_formula_weight         658.98
_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     heavy
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                84.691(5)
_cell_angle_beta                 71.313(5)
_cell_angle_gamma                72.822(5)
_cell_formula_units_Z            1
_cell_length_a                   7.992(3)
_cell_length_b                   8.493(3)
_cell_length_c                   10.489(4)
_cell_measurement_temperature    150(2)
_cell_volume                     644.3(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.876
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_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  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0811
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5163
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.20
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    0.935
_exptl_absorpt_correction_T_max  0.9725
_exptl_absorpt_correction_T_min  0.9123
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             332
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.383
_refine_diff_density_min         -1.248
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2782
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0599
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0891P)²+1.2819P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1571
_refine_ls_wR_factor_ref         0.1652
_reflns_number_gt                2312
_reflns_number_total             2782
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ICA-2013-402-69-74-1.cif
_cod_data_source_block           str0841
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1517149
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 0.0000 1.0000 1.0000 0.0182(2) Uani 1 2 d S
S1 S 0.2033(2) 0.80332(18) 0.71731(15) 0.0258(3) Uani 1 1 d .
N1 N 0.2087(6) 0.9296(6) 0.8250(5) 0.0231(10) Uani 1 1 d .
N2 N 0.1272(7) 0.7987(6) 1.0898(5) 0.0238(10) Uani 1 1 d .
N3 N -0.0834(7) 0.6593(6) 1.0876(5) 0.0256(11) Uani 1 1 d .
H3A H -0.1452 0.7477 1.0541 0.031 Uiso 1 1 calc R
H3B H -0.1218 0.5703 1.1033 0.031 Uiso 1 1 calc R
O1 O 0.4048(6) 1.0537(5) 0.8644(4) 0.0286(9) Uani 1 1 d .
O2 O 0.1995(7) 0.6445(6) 0.7778(5) 0.0380(11) Uani 1 1 d .
O3 O 0.0651(6) 0.8801(6) 0.6540(5) 0.0410(12) Uani 1 1 d .
C1 C 0.3719(8) 0.9648(7) 0.7939(6) 0.0254(12) Uani 1 1 d .
C2 C 0.5035(8) 0.8809(7) 0.6680(6) 0.0246(12) Uani 1 1 d .
C3 C 0.4280(8) 0.7898(7) 0.6097(6) 0.0248(12) Uani 1 1 d .
C4 C 0.5254(9) 0.7007(8) 0.4946(6) 0.0315(14) Uani 1 1 d .
H4A H 0.4714 0.6413 0.4546 0.038 Uiso 1 1 calc R
C5 C 0.7081(9) 0.7015(9) 0.4390(7) 0.0369(16) Uani 1 1 d .
H5A H 0.7811 0.6386 0.3599 0.044 Uiso 1 1 calc R
C6 C 0.7858(10) 0.7886(9) 0.4934(7) 0.0395(17) Uani 1 1 d .
H6A H 0.9114 0.7851 0.4519 0.047 Uiso 1 1 calc R
C7 C 0.6857(8) 0.8825(8) 0.6082(7) 0.0305(14) Uani 1 1 d .
H7A H 0.7392 0.9459 0.6450 0.037 Uiso 1 1 calc R
C8 C 0.2789(8) 0.8031(8) 1.1163(6) 0.0282(13) Uani 1 1 d .
H8A H 0.3158 0.9015 1.0983 0.034 Uiso 1 1 calc R
C9 C 0.3828(10) 0.6704(9) 1.1684(7) 0.0368(15) Uani 1 1 d .
H9A H 0.4902 0.6759 1.1862 0.044 Uiso 1 1 calc R
C10 C 0.3259(10) 0.5265(9) 1.1944(8) 0.0424(18) Uani 1 1 d .
H10A H 0.3943 0.4334 1.2317 0.051 Uiso 1 1 calc R
C11 C 0.1733(10) 0.5192(8) 1.1668(7) 0.0351(15) Uani 1 1 d .
H11A H 0.1366 0.4206 1.1821 0.042 Uiso 1 1 calc R
C12 C 0.0704(8) 0.6602(7) 1.1148(6) 0.0235(12) 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'
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
N2 Pd1 N2 180.000(1) 2_577 .
N2 Pd1 N1 91.54(19) 2_577 .
N2 Pd1 N1 88.46(19) . .
N2 Pd1 N1 88.46(19) 2_577 2_577
N2 Pd1 N1 91.54(19) . 2_577
N1 Pd1 N1 180.000(1) . 2_577
O3 S1 O2 116.8(3) . .
O3 S1 N1 111.1(3) . .
O2 S1 N1 110.7(3) . .
O3 S1 C3 112.5(3) . .
O2 S1 C3 108.8(3) . .
N1 S1 C3 94.8(3) . .
C1 N1 S1 113.6(4) . .
C1 N1 Pd1 123.8(4) . .
S1 N1 Pd1 122.2(3) . .
C8 N2 C12 120.3(5) . .
C8 N2 Pd1 117.2(4) . .
C12 N2 Pd1 122.4(4) . .
O1 C1 N1 123.3(6) . .
O1 C1 C2 125.4(5) . .
N1 C1 C2 111.3(5) . .
C7 C2 C3 119.7(6) . .
C7 C2 C1 127.6(6) . .
C3 C2 C1 112.7(5) . .
C4 C3 C2 122.6(6) . .
C4 C3 S1 129.7(5) . .
C2 C3 S1 107.6(5) . .
C3 C4 C5 116.4(6) . .
C6 C5 C4 122.4(7) . .
C5 C6 C7 121.2(6) . .
C6 C7 C2 117.6(6) . .
N2 C8 C9 122.3(6) . .
C8 C9 C10 118.0(6) . .
C11 C10 C9 120.5(6) . .
C10 C11 C12 119.0(6) . .
N3 C12 N2 119.0(5) . .
N3 C12 C11 121.1(5) . .
N2 C12 C11 119.9(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 N2 2.033(5) 2_577
Pd1 N2 2.033(5) .
Pd1 N1 2.040(5) .
Pd1 N1 2.040(5) 2_577
S1 O3 1.433(5) .
S1 O2 1.441(5) .
S1 N1 1.647(5) .
S1 C3 1.765(6) .
N1 C1 1.355(7) .
N2 C8 1.339(8) .
N2 C12 1.357(7) .
N3 C12 1.350(7) .
O1 C1 1.237(7) .
C1 C2 1.483(9) .
C2 C7 1.392(8) .
C2 C3 1.392(8) .
C3 C4 1.361(9) .
C4 C5 1.389(9) .
C5 C6 1.355(11) .
C6 C7 1.382(10) .
C8 C9 1.372(9) .
C9 C10 1.400(10) .
C10 C11 1.360(9) .
C11 C12 1.411(8) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
O3 S1 N1 C1 -118.7(4) .
O2 S1 N1 C1 109.9(4) .
C3 S1 N1 C1 -2.3(5) .
O3 S1 N1 Pd1 68.8(4) .
O2 S1 N1 Pd1 -62.6(4) .
C3 S1 N1 Pd1 -174.8(3) .
N2 Pd1 N1 C1 96.6(5) 2_577
N2 Pd1 N1 C1 -83.4(5) .
N1 Pd1 N1 C1 -141(100) 2_577
N2 Pd1 N1 S1 -91.7(3) 2_577
N2 Pd1 N1 S1 88.3(3) .
N1 Pd1 N1 S1 31(100) 2_577
N2 Pd1 N2 C8 171(100) 2_577
N1 Pd1 N2 C8 73.8(5) .
N1 Pd1 N2 C8 -106.2(5) 2_577
N2 Pd1 N2 C12 -4(100) 2_577
N1 Pd1 N2 C12 -101.9(5) .
N1 Pd1 N2 C12 78.1(5) 2_577
S1 N1 C1 O1 -178.0(5) .
Pd1 N1 C1 O1 -5.6(8) .
S1 N1 C1 C2 0.8(6) .
Pd1 N1 C1 C2 173.3(4) .
O1 C1 C2 C7 1.7(10) .
N1 C1 C2 C7 -177.1(6) .
O1 C1 C2 C3 -179.7(5) .
N1 C1 C2 C3 1.6(7) .
C7 C2 C3 C4 -0.2(9) .
C1 C2 C3 C4 -179.0(5) .
C7 C2 C3 S1 175.8(5) .
C1 C2 C3 S1 -3.0(6) .
O3 S1 C3 C4 -66.2(7) .
O2 S1 C3 C4 64.8(6) .
N1 S1 C3 C4 178.6(6) .
O3 S1 C3 C2 118.2(4) .
O2 S1 C3 C2 -110.8(4) .
N1 S1 C3 C2 3.0(4) .
C2 C3 C4 C5 1.6(9) .
S1 C3 C4 C5 -173.3(5) .
C3 C4 C5 C6 -1.5(10) .
C4 C5 C6 C7 -0.2(11) .
C5 C6 C7 C2 1.7(10) .
C3 C2 C7 C6 -1.5(9) .
C1 C2 C7 C6 177.1(6) .
C12 N2 C8 C9 0.3(9) .
Pd1 N2 C8 C9 -175.6(5) .
N2 C8 C9 C10 -0.1(11) .
C8 C9 C10 C11 0.9(11) .
C9 C10 C11 C12 -1.7(11) .
C8 N2 C12 N3 179.8(5) .
Pd1 N2 C12 N3 -4.6(8) .
C8 N2 C12 C11 -1.1(9) .
Pd1 N2 C12 C11 174.5(5) .
C10 C11 C12 N3 -179.1(6) .
C10 C11 C12 N2 1.8(10) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139043897
