#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:25:00 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180504 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/73/7217329.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_7217329
loop_
_publ_author_name
'Pérez, José'
'Serrano, J. Luis'
'da Silva, Ivan'
'Espinosa, Arturo'
'Pérez, Eduardo'
'García, Luis'
_publ_section_title
;
 Ligand hierarchy on driving the crystal packing. Effect of supramolecular
 interactions on solid-state conformations adopted by saccharinate Pd(ii)
 complexes
;
_journal_issue                   30
_journal_name_full               CrystEngComm
_journal_page_first              7124
_journal_paper_doi               10.1039/C4CE00518J
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C22 H16 N6 O6 Pd S2'
_chemical_formula_weight         630.93
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.788(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.0530(3)
_cell_length_b                   9.7220(4)
_cell_length_c                   16.0510(4)
_cell_measurement_temperature    293(2)
_cell_volume                     1247.84(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0667
_diffrn_reflns_av_sigmaI/netI    0.0548
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10326
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    0.962
_exptl_absorpt_correction_T_max  0.8692
_exptl_absorpt_correction_T_min  0.7950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.572
_refine_diff_density_min         -1.229
_refine_diff_density_rms         0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2890
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0397
_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)+(0.0732P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1269
_reflns_number_gt                1945
_reflns_number_total             2890
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7215906
_cod_data_source_file            c4ce00518j2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7217329
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
O1 O 0.3839(4) 0.1226(4) 0.0267(2) 0.0562(8) Uani 1 1 d .
O2 O -0.0680(4) 0.2671(4) 0.1455(2) 0.0705(11) Uani 1 1 d .
O3 O 0.0265(5) 0.0622(5) 0.2235(2) 0.0787(12) Uani 1 1 d .
N2 N 0.1144(5) -0.1748(4) 0.0413(2) 0.0445(8) Uani 1 1 d .
N3 N 0.0186(6) -0.2652(5) 0.0739(3) 0.0687(13) Uani 1 1 d .
C11 C 0.2722(6) -0.1998(5) 0.0319(3) 0.0526(11) Uani 1 1 d .
H11 H 0.3345 -0.1320 0.0090 0.063 Uiso 1 1 calc R
C10 C 0.3467(8) -0.3233(6) 0.0549(4) 0.0750(16) Uani 1 1 d .
H10 H 0.4576 -0.3411 0.0478 0.090 Uiso 1 1 calc R
C9 C 0.2501(9) -0.4183(7) 0.0888(4) 0.088(2) Uani 1 1 d .
H9 H 0.2941 -0.5034 0.1062 0.106 Uiso 1 1 calc R
C8 C 0.0860(10) -0.3863(6) 0.0968(4) 0.0833(19) Uani 1 1 d .
H8 H 0.0199 -0.4519 0.1192 0.100 Uiso 1 1 calc R
Pd1 Pd 0.0000 0.0000 0.0000 0.03572(17) Uani 1 2 d S
S1 S 0.06360(14) 0.17205(12) 0.17043(7) 0.0461(3) Uani 1 1 d .
N1 N 0.1425(4) 0.1115(4) 0.0882(2) 0.0414(8) Uani 1 1 d .
C2 C 0.3678(5) 0.2365(4) 0.1588(3) 0.0405(9) Uani 1 1 d .
C7 C 0.2480(5) 0.2586(4) 0.2118(3) 0.0404(9) Uani 1 1 d .
C1 C 0.3034(5) 0.1519(4) 0.0837(3) 0.0425(10) Uani 1 1 d .
C4 C 0.5551(7) 0.3708(6) 0.2504(3) 0.0642(14) Uani 1 1 d .
H4 H 0.6603 0.4093 0.2647 0.077 Uiso 1 1 calc R
C3 C 0.5250(6) 0.2929(5) 0.1786(3) 0.0534(12) Uani 1 1 d .
H3 H 0.6085 0.2787 0.1441 0.064 Uiso 1 1 calc R
C6 C 0.2762(6) 0.3353(5) 0.2843(3) 0.0524(11) Uani 1 1 d .
H6 H 0.1941 0.3478 0.3197 0.063 Uiso 1 1 calc R
C5 C 0.4325(7) 0.3923(6) 0.3012(3) 0.0635(14) Uani 1 1 d .
H5 H 0.4558 0.4472 0.3486 0.076 Uiso 1 1 calc R
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'
Pd Pd -0.9988 1.0072 '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'
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 N2 C11 122.6(4) . .
N3 N2 Pd1 115.3(3) . .
C11 N2 Pd1 121.9(3) . .
N2 N3 C8 117.4(5) . .
N2 C11 C10 121.8(5) . .
C9 C10 C11 116.7(5) . .
C10 C9 C8 118.9(6) . .
N3 C8 C9 122.6(6) . .
N2 Pd1 N2 180.0(3) . 3
N2 Pd1 N1 88.74(14) . 3
N2 Pd1 N1 91.26(14) 3 3
N2 Pd1 N1 91.26(14) . .
N2 Pd1 N1 88.74(14) 3 .
N1 Pd1 N1 180.0(2) 3 .
O3 S1 O2 117.0(3) . .
O3 S1 N1 110.0(2) . .
O2 S1 N1 110.6(2) . .
O3 S1 C7 111.1(2) . .
O2 S1 C7 111.1(2) . .
N1 S1 C7 94.90(19) . .
C1 N1 S1 113.6(3) . .
C1 N1 Pd1 125.4(3) . .
S1 N1 Pd1 120.84(19) . .
C3 C2 C7 119.1(4) . .
C3 C2 C1 128.5(4) . .
C7 C2 C1 112.5(3) . .
C6 C7 C2 123.3(4) . .
C6 C7 S1 128.5(3) . .
C2 C7 S1 108.2(3) . .
O1 C1 N1 124.5(4) . .
O1 C1 C2 124.7(4) . .
N1 C1 C2 110.8(4) . .
C5 C4 C3 121.0(5) . .
C4 C3 C2 118.4(4) . .
C5 C6 C7 116.2(4) . .
C4 C5 C6 122.0(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 C1 1.215(5) .
O2 S1 1.427(4) .
O3 S1 1.420(4) .
N2 N3 1.318(5) .
N2 C11 1.320(6) .
N2 Pd1 2.008(4) .
N3 C8 1.330(7) .
C11 C10 1.373(7) .
C10 C9 1.361(8) .
C9 C8 1.379(9) .
Pd1 N2 2.008(4) 3
Pd1 N1 2.028(3) 3
Pd1 N1 2.028(3) .
S1 N1 1.640(3) .
S1 C7 1.767(4) .
N1 C1 1.365(5) .
C2 C3 1.382(6) .
C2 C7 1.377(6) .
C2 C1 1.500(6) .
C7 C6 1.377(6) .
C4 C5 1.368(7) .
C4 C3 1.377(7) .
C6 C5 1.373(7) .
