#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/33/2013313.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2013313
loop_
_publ_author_name
'Ara, Irene'
'El Bahij, Fatima'
'Lachkar, Mohamed'
'Ben Larbi, Najib'
_publ_section_title
;
 Bis(O-ethyl
 dithiocarbonato-κ²S,S')palladium(II)
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m199
_journal_page_last               m200
_journal_paper_doi               10.1107/S0108270103007406
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Pd (C3 H5 O1 S2)2]'
_chemical_formula_moiety         'C6 H10 O2 Pd S4'
_chemical_formula_sum            'C6 H10 O2 Pd S4'
_chemical_formula_weight         348.78
_chemical_melting_point          424
_chemical_name_common            palladium-ethylxanthate
_chemical_name_systematic
;
bis(O-ethyl dithiocarbonato)palladium(II)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.4958(6)
_cell_length_b                   7.1942(6)
_cell_length_c                   20.7522(18)
_cell_measurement_reflns_used    2030
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.62
_cell_measurement_theta_min      3.92
_cell_volume                     1119.09(16)
_computing_cell_refinement       'SAINT-Plus (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    'XP in SHELXTL (Bruker, 2000)'
_computing_publication_material  'XP in SHELXTL'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'ω rotation'
_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  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            6401
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.369
_exptl_absorpt_correction_T_max  0.7641
_exptl_absorpt_correction_T_min  0.4826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1999)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.070
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.415
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         1324
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0257
_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)+(0.0251P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0545
_refine_ls_wR_factor_ref         0.0569
_reflns_number_gt                992
_reflns_number_total             1324
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ln1165.cif
_cod_data_source_block           I
_cod_database_code               2013313
_cod_database_fobs_code          2013313
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Pd 0.5000 0.0000 0.5000 0.01919(10) Uani d S 1 . . Pd
S1 0.38861(9) 0.28725(11) 0.53224(4) 0.02173(18) Uani d . 1 . . S
S2 0.61448(9) 0.04312(10) 0.60364(4) 0.02177(18) Uani d . 1 . . S
O 0.5053(2) 0.3577(3) 0.65159(10) 0.0213(4) Uani d . 1 . . O
C1 0.5020(3) 0.2483(4) 0.60151(14) 0.0194(6) Uani d . 1 . . C
C2 0.4117(4) 0.5357(4) 0.64662(15) 0.0223(7) Uani d . 1 . . C
H2A 0.2829 0.5150 0.6391 0.027 Uiso calc R 1 . . H
H2B 0.4602 0.6096 0.6104 0.027 Uiso calc R 1 . . H
C3 0.4402(4) 0.6353(5) 0.70905(15) 0.0301(8) Uani d . 1 . . C
H3A 0.3791 0.7557 0.7078 0.045 Uiso calc R 1 . . H
H3B 0.5681 0.6550 0.7158 0.045 Uiso calc R 1 . . H
H3C 0.3918 0.5604 0.7444 0.045 Uiso calc R 1 . . H
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Pd 0.01655(15) 0.02276(18) 0.01827(18) 0.00076(14) -0.00097(14) 0.00178(14)
S1 0.0203(3) 0.0240(4) 0.0209(4) 0.0023(3) -0.0026(3) 0.0024(3)
S2 0.0199(3) 0.0250(4) 0.0204(4) 0.0034(3) -0.0024(3) 0.0019(3)
O 0.0195(9) 0.0230(11) 0.0212(12) 0.0030(9) -0.0011(9) 0.0006(9)
C1 0.0124(12) 0.0258(15) 0.0198(16) -0.0041(12) 0.0018(12) 0.0039(13)
C2 0.0181(14) 0.0236(16) 0.0252(17) 0.0041(13) -0.0012(13) 0.0012(13)
C3 0.0316(16) 0.032(2) 0.0268(19) 0.0044(14) -0.0007(14) -0.0010(16)
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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S1 Pd S1 5_656 . 180.00(4) y
S1 Pd S2 5_656 . 104.53(3) y
S1 Pd S2 . . 75.47(3) y
S1 Pd S2 5_656 5_656 75.47(3) ?
S1 Pd S2 . 5_656 104.53(3) ?
S2 Pd S2 . 5_656 180.0 ?
C1 S1 Pd . . 85.24(11) y
C1 S2 Pd . . 84.78(10) y
C1 O C2 . . 117.6(2) y
O C1 S1 . . 125.9(2) ?
O C1 S2 . . 119.6(2) ?
S1 C1 S2 . . 114.50(17) ?
O C2 C3 . . 106.8(2) ?
O C2 H2A . . 110.4 ?
C3 C2 H2A . . 110.4 ?
O C2 H2B . . 110.4 ?
C3 C2 H2B . . 110.4 ?
H2A C2 H2B . . 108.6 ?
C2 C3 H3A . . 109.5 ?
C2 C3 H3B . . 109.5 ?
H3A C3 H3B . . 109.5 ?
C2 C3 H3C . . 109.5 ?
H3A C3 H3C . . 109.5 ?
H3B C3 H3C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd S1 5_656 2.3271(8) ?
Pd S1 . 2.3271(8) y
Pd S2 . 2.3363(8) y
Pd S2 5_656 2.3363(8) ?
S1 C1 . 1.693(3) y
S2 C1 . 1.700(3) y
O C1 . 1.304(3) y
O C2 . 1.463(3) y
C2 C3 . 1.496(4) y
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C3 H3A . 0.9800 ?
C3 H3B . 0.9800 ?
C3 H3C . 0.9800 ?
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_site_symmetry_1
_geom_torsion
S2 Pd S1 C1 . 0.10(9)
S2 Pd S1 C1 5_656 -179.90(9)
S1 Pd S2 C1 5_656 179.91(9)
S1 Pd S2 C1 . -0.09(9)
C2 O C1 S1 . -3.8(3)
C2 O C1 S2 . 177.88(18)
Pd S1 C1 O . -178.5(2)
Pd S1 C1 S2 . -0.14(13)
Pd S2 C1 O . 178.6(2)
Pd S2 C1 S1 . 0.14(13)
C1 O C2 C3 . -178.5(2)
