#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/62/2206243.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_2206243
loop_
_publ_author_name
'Nobuhiro Takeda'
'Daisuke Shimizu'
'Takahiro Sasamori'
'Norihiro Tokitoh'
_publ_section_title
;
 [1,2-Bis(phenylsulfanyl)benzene]dichloropalladium(II)
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1408
_journal_page_last               m1410
_journal_paper_doi               10.1107/S1600536805019409
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Pd Cl2 (C18 H14 S2)]'
_chemical_formula_moiety         'C18 H14 Cl2 Pd S2'
_chemical_formula_sum            'C18 H14 Cl2 Pd S2'
_chemical_formula_weight         471.71
_chemical_name_systematic
;
dichloro[1,2-bis(phenylsulfanyl)benzene]palladium
;
_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     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                76.905(10)
_cell_angle_beta                 63.051(9)
_cell_angle_gamma                67.639(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9145(14)
_cell_length_b                   10.214(2)
_cell_length_c                   10.521(2)
_cell_measurement_reflns_used    3041
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      2.96
_cell_volume                     876.4(3)
_computing_cell_refinement
;
CrystalClear
;
_computing_data_collection
;
CrystalClear (Rigaku, 2004)
;
_computing_data_reduction
;
CrystalClear
;
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF99 (Beurskens et al., 1999)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0115
_diffrn_reflns_av_sigmaI/netI    0.0174
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5768
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    1.596
_exptl_absorpt_correction_T_max  0.6459
_exptl_absorpt_correction_T_min  0.5336
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.787
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.470
_refine_ls_extinction_coef       0.0058(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3140
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0186
_refine_ls_R_factor_gt           0.0173
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0179P)²+0.6226P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0426
_refine_ls_wR_factor_ref         0.0431
_reflns_number_gt                2982
_reflns_number_total             3140
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            lh6454.cif
_cod_data_source_block           I
_cod_database_code               2206243
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_type_symbol
Pd1 0.160038(16) 0.351156(13) 0.983833(13) 0.00798(7) Uani d . 1 Pd
Cl1 0.04224(6) 0.23695(5) 1.20125(5) 0.01444(11) Uani d . 1 Cl
Cl2 0.21687(5) 0.49290(4) 1.08310(5) 0.01212(10) Uani d . 1 Cl
S1 0.10134(5) 0.21948(5) 0.88101(5) 0.00895(10) Uani d . 1 S
S2 0.28534(5) 0.44949(5) 0.76502(5) 0.00928(10) Uani d . 1 S
C1 0.1561(2) 0.29199(19) 0.69950(19) 0.0106(4) Uani d . 1 C
C2 0.1229(2) 0.2452(2) 0.6058(2) 0.0149(4) Uani d . 1 C
H1 0.0820 0.1680 0.6345 0.018 Uiso calc R 1 H
C3 0.1498(2) 0.3121(2) 0.4703(2) 0.0183(4) Uani d . 1 C
H2 0.1304 0.2787 0.4050 0.022 Uiso calc R 1 H
C4 0.2049(2) 0.4278(2) 0.4299(2) 0.0175(4) Uani d . 1 C
H3 0.2188 0.4755 0.3383 0.021 Uiso calc R 1 H
C5 0.2396(2) 0.4740(2) 0.5219(2) 0.0145(4) Uani d . 1 C
H4 0.2774 0.5531 0.4942 0.017 Uiso calc R 1 H
C6 0.2185(2) 0.40306(19) 0.65582(19) 0.0106(4) Uani d . 1 C
C7 0.2427(2) 0.04404(19) 0.86291(19) 0.0109(4) Uani d . 1 C
C8 0.1953(2) -0.0608(2) 0.8468(2) 0.0141(4) Uani d . 1 C
H5 0.0941 -0.0374 0.8444 0.017 Uiso calc R 1 H
C9 0.2972(2) -0.1998(2) 0.8343(2) 0.0172(4) Uani d . 1 C
H6 0.2665 -0.2722 0.8223 0.021 Uiso calc R 1 H
C10 0.4437(2) -0.2325(2) 0.8393(2) 0.0178(4) Uani d . 1 C
H7 0.5128 -0.3278 0.8317 0.021 Uiso calc R 1 H
C11 0.4909(2) -0.1276(2) 0.8553(2) 0.0170(4) Uani d . 1 C
H8 0.5922 -0.1511 0.8576 0.020 Uiso calc R 1 H
C12 0.3894(2) 0.0122(2) 0.8679(2) 0.0140(4) Uani d . 1 C
H9 0.4201 0.0846 0.8797 0.017 Uiso calc R 1 H
C13 0.4855(2) 0.32451(19) 0.71152(19) 0.0110(4) Uani d . 1 C
C14 0.5671(2) 0.3127(2) 0.7943(2) 0.0156(4) Uani d . 1 C
H10 0.5192 0.3709 0.8721 0.019 Uiso calc R 1 H
C15 0.7185(2) 0.2154(2) 0.7619(2) 0.0204(4) Uani d . 1 C
H11 0.7742 0.2055 0.8187 0.024 Uiso calc R 1 H
C16 0.7896(2) 0.1318(2) 0.6464(2) 0.0227(5) Uani d . 1 C
H12 0.8928 0.0637 0.6256 0.027 Uiso calc R 1 H
C17 0.7098(2) 0.1481(2) 0.5620(2) 0.0214(5) Uani d . 1 C
H13 0.7602 0.0932 0.4814 0.026 Uiso calc R 1 H
C18 0.5569(2) 0.2437(2) 0.5939(2) 0.0158(4) Uani d . 1 C
H14 0.5018 0.2539 0.5364 0.019 Uiso calc R 1 H
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'
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_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S1 Pd1 S2 . 89.86(2) yes
S1 Pd1 Cl2 . 177.782(16) yes
S2 Pd1 Cl2 . 88.56(2) yes
S1 Pd1 Cl1 . 87.95(2) yes
S2 Pd1 Cl1 . 176.378(17) yes
Cl2 Pd1 Cl1 . 93.70(2) yes
C7 S1 C1 . 102.47(8) yes
C7 S1 Pd1 . 109.26(6) yes
C1 S1 Pd1 . 103.51(6) yes
C7 S1 Cl2 2_567 166.57(6) ?
C1 S1 Cl2 2_567 79.63(6) ?
Pd1 S1 Cl2 2_567 82.80(2) ?
C6 S2 C13 . 100.23(9) yes
C6 S2 Pd1 . 102.86(6) yes
C13 S2 Pd1 . 101.01(6) yes
C6 S2 Cl1 2_567 83.45(6) ?
C13 S2 Cl1 2_567 162.70(6) ?
Pd1 S2 Cl1 2_567 94.54(2) ?
C6 C1 C2 . 119.81(17) ?
C6 C1 S1 . 120.08(14) ?
C2 C1 S1 . 119.87(15) ?
C3 C2 C1 . 119.60(18) ?
C3 C2 H1 . 120.2 ?
C1 C2 H1 . 120.2 ?
C2 C3 C4 . 120.21(18) ?
C2 C3 H2 . 119.9 ?
C4 C3 H2 . 119.9 ?
C5 C4 C3 . 120.49(18) ?
C5 C4 H3 . 119.8 ?
C3 C4 H3 . 119.8 ?
C4 C5 C6 . 119.10(18) ?
C4 C5 H4 . 120.5 ?
C6 C5 H4 . 120.5 ?
C1 C6 C5 . 120.65(17) ?
C1 C6 S2 . 120.43(14) ?
C5 C6 S2 . 118.79(15) ?
C12 C7 C8 . 121.26(17) ?
C12 C7 S1 . 122.77(14) ?
C8 C7 S1 . 115.96(14) ?
C9 C8 C7 . 119.44(18) ?
C9 C8 H5 . 120.3 ?
C7 C8 H5 . 120.3 ?
C10 C9 C8 . 119.65(18) ?
C10 C9 H6 . 120.2 ?
C8 C9 H6 . 120.2 ?
C9 C10 C11 . 120.85(18) ?
C9 C10 H7 . 119.6 ?
C11 C10 H7 . 119.6 ?
C10 C11 C12 . 119.82(18) ?
C10 C11 H8 . 120.1 ?
C12 C11 H8 . 120.1 ?
C7 C12 C11 . 118.98(18) ?
C7 C12 H9 . 120.5 ?
C11 C12 H9 . 120.5 ?
C18 C13 C14 . 120.88(18) ?
C18 C13 S2 . 122.61(15) ?
C14 C13 S2 . 116.51(14) ?
C15 C14 C13 . 119.27(18) ?
C15 C14 H10 . 120.4 ?
C13 C14 H10 . 120.4 ?
C14 C15 C16 . 120.34(19) ?
C14 C15 H11 . 119.8 ?
C16 C15 H11 . 119.8 ?
C17 C16 C15 . 119.83(19) ?
C17 C16 H12 . 120.1 ?
C15 C16 H12 . 120.1 ?
C16 C17 C18 . 120.72(19) ?
C16 C17 H13 . 119.6 ?
C18 C17 H13 . 119.6 ?
C17 C18 C13 . 118.90(18) ?
C17 C18 H14 . 120.5 ?
C13 C18 H14 . 120.5 ?
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
Pd1 S1 . 2.2679(5) yes
Pd1 S2 . 2.2719(6) yes
Pd1 Cl2 . 2.3116(5) yes
Pd1 Cl1 . 2.3159(6) yes
S1 C7 . 1.7924(18) yes
S1 C1 . 1.7932(19) yes
S1 Cl2 2_567 3.3311(9) yes
S2 C6 . 1.7774(18) yes
S2 C13 . 1.8085(19) yes
S2 Cl1 2_567 3.5338(9) yes
C1 C6 . 1.386(3) ?
C1 C2 . 1.391(3) ?
C2 C3 . 1.387(3) ?
C2 H1 . 0.9500 ?
C3 C4 . 1.389(3) ?
C3 H2 . 0.9500 ?
C4 C5 . 1.383(3) ?
C4 H3 . 0.9500 ?
C5 C6 . 1.393(3) ?
C5 H4 . 0.9500 ?
C7 C12 . 1.388(3) ?
C7 C8 . 1.389(3) ?
C8 C9 . 1.388(3) ?
C8 H5 . 0.9500 ?
C9 C10 . 1.384(3) ?
C9 H6 . 0.9500 ?
C10 C11 . 1.390(3) ?
C10 H7 . 0.9500 ?
C11 C12 . 1.393(3) ?
C11 H8 . 0.9500 ?
C12 H9 . 0.9500 ?
C13 C18 . 1.392(3) ?
C13 C14 . 1.394(3) ?
C14 C15 . 1.383(3) ?
C14 H10 . 0.9500 ?
C15 C16 . 1.392(3) ?
C15 H11 . 0.9500 ?
C16 C17 . 1.383(3) ?
C16 H12 . 0.9500 ?
C17 C18 . 1.388(3) ?
C17 H13 . 0.9500 ?
C18 H14 . 0.9500 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C3 H2 Cl1 1_554 0.95 2.82 3.753(2) 169
C4 H3 Cl2 1_554 0.95 2.66 3.513(2) 150
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_4
_geom_torsion
S2 Pd1 S1 C7 . . 99.18(6)
Cl1 Pd1 S1 C7 . . -77.93(7)
S2 Pd1 S1 C1 . . -9.44(6)
Cl1 Pd1 S1 C1 . . 173.45(6)
S2 Pd1 S1 Cl2 . 2_567 -86.91(2)
Cl1 Pd1 S1 Cl2 . 2_567 95.98(2)
S1 Pd1 S2 C6 . . 14.66(6)
Cl2 Pd1 S2 C6 . . -163.78(6)
S1 Pd1 S2 C13 . . -88.64(6)
Cl2 Pd1 S2 C13 . . 92.92(6)
S1 Pd1 S2 Cl1 . 2_567 98.96(2)
Cl2 Pd1 S2 Cl1 . 2_567 -79.48(2)
C7 S1 C1 C6 . . -113.41(16)
Pd1 S1 C1 C6 . . 0.21(16)
Cl2 S1 C1 C6 2_567 . 80.13(15)
C7 S1 C1 C2 . . 72.25(16)
Pd1 S1 C1 C2 . . -174.13(14)
Cl2 S1 C1 C2 2_567 . -94.22(15)
C6 C1 C2 C3 . . -1.2(3)
S1 C1 C2 C3 . . 173.13(15)
C1 C2 C3 C4 . . -2.0(3)
C2 C3 C4 C5 . . 2.6(3)
C3 C4 C5 C6 . . 0.0(3)
C2 C1 C6 C5 . . 3.8(3)
S1 C1 C6 C5 . . -170.53(14)
C2 C1 C6 S2 . . -171.97(14)
S1 C1 C6 S2 . . 13.7(2)
C4 C5 C6 C1 . . -3.2(3)
C4 C5 C6 S2 . . 172.68(15)
C13 S2 C6 C1 . . 84.25(16)
Pd1 S2 C6 C1 . . -19.65(16)
Cl1 S2 C6 C1 2_567 . -112.84(15)
C13 S2 C6 C5 . . -91.62(16)
Pd1 S2 C6 C5 . . 164.48(14)
Cl1 S2 C6 C5 2_567 . 71.29(15)
C1 S1 C7 C12 . . 90.40(17)
Pd1 S1 C7 C12 . . -18.92(17)
Cl2 S1 C7 C12 2_567 . -171.98(17)
C1 S1 C7 C8 . . -91.11(15)
Pd1 S1 C7 C8 . . 159.58(13)
Cl2 S1 C7 C8 2_567 . 6.5(4)
C12 C7 C8 C9 . . -0.5(3)
S1 C7 C8 C9 . . -179.05(15)
C7 C8 C9 C10 . . 0.6(3)
C8 C9 C10 C11 . . -0.6(3)
C9 C10 C11 C12 . . 0.6(3)
C8 C7 C12 C11 . . 0.5(3)
S1 C7 C12 C11 . . 178.93(14)
C10 C11 C12 C7 . . -0.6(3)
C6 S2 C13 C18 . . 11.13(17)
Pd1 S2 C13 C18 . . 116.53(15)
Cl1 S2 C13 C18 2_567 . -89.8(3)
C6 S2 C13 C14 . . -169.13(14)
Pd1 S2 C13 C14 . . -63.73(14)
Cl1 S2 C13 C14 2_567 . 90.0(2)
C18 C13 C14 C15 . . -2.5(3)
S2 C13 C14 C15 . . 177.73(15)
C13 C14 C15 C16 . . 1.1(3)
C14 C15 C16 C17 . . 1.2(3)
C15 C16 C17 C18 . . -2.2(3)
C16 C17 C18 C13 . . 0.7(3)
C14 C13 C18 C17 . . 1.6(3)
S2 C13 C18 C17 . . -178.65(15)
