#------------------------------------------------------------------------------
#$Date: 2016-02-19 23:18:51 +0100 (vie 19 de feb de 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/23/2012386.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_2012386
loop_
_publ_author_name
'Miyashita, Yoshitaro'
'Arai, Satoshi'
'Yamada, Yasunori'
'Fujisawa, Kiyoshi'
'Okamoto, Ken-ichi'
_publ_section_title
;anti-Bis(μ-2-ammonioethanethiolato-κ²S:S)bis[dichloropalladium(II)]
 dihydrate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1393
_journal_page_last               1394
_journal_paper_doi               10.1107/S0108270101015736
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          '[Pd2 Cl4 (C2 H7 N S)2], 2H2 O'
_chemical_formula_moiety         'C4 H14 Cl4 N2 Pd2 S2, 2H2 O'
_chemical_formula_sum            'C4 H18 Cl4 N2 O2 Pd2 S2'
_chemical_formula_weight         544.93
_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'
_cell_angle_alpha                90
_cell_angle_beta                 91.680(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.4490(10)
_cell_length_b                   8.941(3)
_cell_length_c                   11.984(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      14.1
_cell_measurement_theta_min      11.2
_cell_volume                     797.8(3)
_computing_cell_refinement       WinAFC
_computing_data_collection       'WinAFC (Rigaku Corporation, 1999)'
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1999)'
_computing_publication_material  TEXSAN
_computing_structure_refinement  TEXSAN
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_measured_fraction_theta_full .5153
_diffrn_measured_fraction_theta_max .5153
_diffrn_measurement_device_type  'Rigaku AFC-7S'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .7107
_diffrn_reflns_av_R_equivalents  .063
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            1970
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_standards_decay_%        .08
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.174
_exptl_absorpt_correction_T_max  .776
_exptl_absorpt_correction_T_min  .729
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_size_max          .150
_exptl_crystal_size_mid          .100
_exptl_crystal_size_min          .080
_refine_diff_density_max         1.11
_refine_diff_density_min         -1.05
_refine_ls_extinction_coef       .0034(9)
_refine_ls_extinction_method
'Zachariasen (1967), type 2, Gaussian isotropic'
_refine_ls_goodness_of_fit_ref   .969
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     74
_refine_ls_number_reflns         1833
_refine_ls_R_factor_gt           .0437
_refine_ls_shift/su_max          .0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²) + {0.03[max(Fo²,0) + 2Fc²]/3}²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1082
_reflns_number_gt                982
_reflns_number_total             1833
_reflns_threshold_expression     F²>2σ(F²)
_cod_data_source_file            oa1118.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2012386
_cod_database_fobs_code          2012386
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,1/2+y,1/2-z
-x,-y,-z
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
Pd1 .68536(9) .44120(8) .43119(6) .0283(2) Uani d . 1.00 . . Pd
Cl1 .7901(3) .4937(3) .2517(2) .0462(7) Uani d . 1.00 . . Cl
Cl2 .9194(4) .2732(3) .4737(2) .0547(9) Uani d . 1.00 . . Cl
S1 .4609(3) .6140(3) .4108(2) .0294(6) Uani d . 1.00 . . S
O1 .3120(10) .4740(10) .0091(7) .104(4) Uani d . 1.00 . . O
N1 .1654(10) .3422(10) .1990(7) .046(2) Uani d . 1.00 . . N
C1 .3200(10) .5540(10) .2942(7) .040(3) Uani d . 1.00 . . C
C2 .2890(10) .3880(10) .2924(8) .040(3) Uani d . 1.00 . . C
H1 .0526 .3901 .2065 .0548 Uiso calc . 1.00 . . H
H2 .2154 .3704 .1300 .0548 Uiso calc . 1.00 . . H
H3 .1495 .2369 .2006 .0548 Uiso calc . 1.00 . . H
H4 .2068 .6026 .2985 .0474 Uiso calc . 1.00 . . H
H5 .3753 .5817 .2270 .0474 Uiso calc . 1.00 . . H
H6 .2378 .3590 .3609 .0475 Uiso calc . 1.00 . . H
H7 .4007 .3390 .2845 .0475 Uiso calc . 1.00 . . 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
Pd1 .0250(3) .0335(4) .0264(3) .0023(4) .0033(2) -.0018(4)
Cl1 .0440(10) .066(2) .0290(10) .0090(10) .0100(10) .0040(10)
Cl2 .044(2) .063(2) .058(2) .0240(10) .0080(10) .0130(10)
S1 .0320(10) .0290(10) .0280(10) -.0010(10) .0026(10) -.0015(10)
O1 .134(9) .118(9) .058(5) -.032(8) -.029(6) .018(5)
N1 .026(4) .052(6) .058(5) -.001(4) -.015(4) -.025(5)
C1 .043(5) .038(5) .037(5) .010(6) -.005(4) -.003(5)
C2 .032(5) .048(6) .039(5) -.002(5) .007(4) -.008(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .003 .002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H .000 .000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
N N .006 .003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
S S .125 .123
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Cl Cl .148 .159
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Pd Pd -.999 1.007
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
O O .011 .006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 Pd1 Cl2 1_555 1_555 93.55(9) yes
Cl1 Pd1 S1 1_555 1_555 91.62(9) yes
Cl1 Pd1 S1 1_555 3_666 170.40(9) yes
Cl2 Pd1 S1 1_555 1_555 173.35(9) yes
Cl2 Pd1 S1 1_555 3_666 92.94(9) yes
S1 Pd1 S1 1_555 3_666 82.46(9) yes
Pd1 S1 Pd1 1_555 3_666 97.54(9) yes
Pd1 S1 C1 1_555 1_555 106.8(3) yes
Pd1 S1 C1 3_666 3_666 107.3(3) yes
S1 C1 C2 1_555 1_555 113.1(7) no
N1 C2 C1 1_555 1_555 112.1(8) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 Cl1 . . 2.357(2) yes
Pd1 Cl2 . . 2.346(3) yes
Pd1 S1 . . 2.285(3) yes
Pd1 S1 . 3_666 2.267(2) yes
S1 C1 . . 1.806(9) no
N1 C2 . . 1.480(10) no
C1 C2 . . 1.500(10) no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
Cl1 N1 3.186(8) 1_655
Cl1 N1 3.188(9) 2_655
Cl1 O1 3.208(9) 3_665
Cl2 O1 3.190(10) 2_645
Cl2 N1 3.380(8) 4_655
O1 N1 2.810(10) .
O1 O1 2.86(2) 3_665
O1 C2 3.490(10) .
O1 C1 3.490(10) .
Pd1 Pd1 3.4230(10) 3_666
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_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Pd1 S1 Pd1 Cl1 1_555 1_555 3_666 3_666 52.3(6) no
Pd1 S1 Pd1 Cl2 1_555 1_555 3_666 3_666 -175.20(10) no
Pd1 S1 Pd1 S1 1_555 1_555 3_666 3_666 .0 no
Pd1 S1 C1 C2 1_555 1_555 1_555 1_555 40.6(7) no
Pd1 S1 Pd1 Cl1 1_555 3_666 3_666 3_666 -172.41(10) no
Pd1 S1 Pd1 Cl2 1_555 3_666 3_666 3_666 46.5(9) no
Pd1 S1 Pd1 S1 1_555 3_666 3_666 1_555 .0 no
Pd1 S1 C1 C2 1_555 3_666 3_666 3_666 63.1(7) no
Cl1 Pd1 S1 C1 1_555 1_555 1_555 1_555 61.7(3) no
Cl1 Pd1 S1 C1 1_555 1_555 3_666 3_666 -162.6(6) no
Cl2 Pd1 S1 C1 1_555 1_555 1_555 1_555 -157.2(9) no
Cl2 Pd1 S1 C1 1_555 1_555 3_666 3_666 64.9(4) no
S1 Pd1 S1 Pd1 1_555 1_555 3_666 3_666 .0 no
S1 Pd1 S1 C1 1_555 1_555 3_666 3_666 -110.3(4) no
S1 Pd1 S1 Pd1 1_555 3_666 3_666 1_555 .0 no
S1 Pd1 S1 C1 1_555 3_666 3_666 3_666 110.7(4) no
S1 C1 C2 N1 1_555 1_555 1_555 1_555 177.3(6) no
