#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/92/2219249.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_2219249
loop_
_publ_author_name
'Fierro-Arias, Jaime'
'Morales-Morales, David'
'Hernández-Ortega, Simón'
_publ_section_title
cis-Bis[2-(diphenylphosphino)benzenethiolato-κ²P,S]palladium(II)
_journal_coeditor_code           BT2741
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1196
_journal_paper_doi               10.1107/S1600536808026718
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Pd (C18 H14 P S)2]'
_chemical_formula_moiety         'C36 H28 P2 Pd S2'
_chemical_formula_sum            'C36 H28 P2 Pd S2'
_chemical_formula_weight         693.04
_chemical_name_systematic
;
cis-Bis[2-(diphenylphosphino)benzenethiolato-
κ²P,S]palladium(II)
;
_space_group_IT_number           154
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   9.3060(10)
_cell_length_b                   9.3060(10)
_cell_length_c                   30.069(8)
_cell_measurement_reflns_used    2935
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      19.93
_cell_measurement_theta_min      2.53
_cell_volume                     2255.2(7)
_computing_cell_refinement       'SMART (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 0.83
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       'omega scans'
_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  0.1126
_diffrn_reflns_av_sigmaI/netI    0.1194
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            18737
_diffrn_reflns_theta_full        25.31
_diffrn_reflns_theta_max         25.31
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.888
_exptl_absorpt_correction_T_max  0.9668
_exptl_absorpt_correction_T_min  0.8766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.395
_refine_diff_density_min         -0.313
_refine_ls_abs_structure_details 'Flack (1983), 1113 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.05(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.816
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2749
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.816
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0250P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0836
_reflns_number_gt                1811
_reflns_number_total             2749
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bt2741.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     ' P 32 2"'
_cod_original_sg_symbol_H-M      'P 32 21'
_cod_database_code               2219249
_cod_database_fobs_code          2219249
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'y, x, -z'
'x-y, -y, -z+1/3'
'-x, -x+y, -z+2/3'
loop_
_atom_site_type_symbol
_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
Pd Pd 0.48559(7) 0.48559(7) 0.0000 0.0377(2) Uani d S 1
P P1 0.2993(2) 0.3605(2) 0.05647(6) 0.0399(5) Uani d . 1
S S1 0.6481(2) 0.6901(2) 0.05082(7) 0.0592(6) Uani d . 1
C C1 0.5327(8) 0.6409(8) 0.0997(2) 0.0408(18) Uani d . 1
C C2 0.3770(9) 0.4982(8) 0.1037(2) 0.0397(18) Uani d . 1
C C3 0.2892(10) 0.4667(9) 0.1433(2) 0.060(2) Uani d . 1
H H3 0.1854 0.3719 0.1458 0.072 Uiso calc R 1
C C4 0.3528(12) 0.5730(12) 0.1790(2) 0.072(3) Uani d . 1
H H4 0.2918 0.5509 0.2051 0.086 Uiso calc R 1
C C5 0.5077(12) 0.7126(11) 0.1757(3) 0.069(3) Uani d . 1
H H5 0.5526 0.7837 0.1999 0.083 Uiso calc R 1
C C6 0.5958(10) 0.7467(9) 0.1367(2) 0.059(2) Uani d . 1
H H6 0.6995 0.8419 0.1347 0.070 Uiso calc R 1
C C7 0.2670(9) 0.1641(8) 0.0782(2) 0.0457(19) Uani d . 1
C C8 0.1239(11) 0.0432(10) 0.0973(3) 0.076(3) Uani d . 1
H H8 0.0317 0.0570 0.0987 0.091 Uiso calc R 1
C C9 0.1143(15) -0.0996(12) 0.1145(3) 0.095(3) Uani d . 1
H H9 0.0142 -0.1808 0.1265 0.114 Uiso calc R 1
C C10 0.2415(15) -0.1239(12) 0.1144(3) 0.083(3) Uani d . 1
H H10 0.2336 -0.2182 0.1275 0.100 Uiso calc R 1
C C11 0.3848(12) -0.0089(12) 0.0949(3) 0.085(3) Uani d . 1
H H11 0.4754 -0.0254 0.0939 0.102 Uiso calc R 1
C C12 0.3967(11) 0.1320(11) 0.0765(2) 0.064(2) Uani d . 1
H H12 0.4949 0.2079 0.0625 0.077 Uiso calc R 1
C C13 0.0948(8) 0.3330(8) 0.0457(2) 0.0414(19) Uani d . 1
C C14 0.0640(11) 0.4611(12) 0.0535(2) 0.064(2) Uani d . 1
H H14 0.1450 0.5570 0.0673 0.076 Uiso calc R 1
C C15 -0.0844(10) 0.4507(12) 0.0413(3) 0.065(3) Uani d . 1
H H15 -0.1031 0.5386 0.0465 0.078 Uiso calc R 1
C C16 -0.2044(12) 0.3062(16) 0.0212(3) 0.094(4) Uani d . 1
H H16 -0.3033 0.2980 0.0118 0.113 Uiso calc R 1
C C17 -0.1781(11) 0.1752(13) 0.0151(3) 0.105(3) Uani d . 1
H H17 -0.2609 0.0766 0.0029 0.125 Uiso calc R 1
C C18 -0.0297(10) 0.1907(11) 0.0272(3) 0.080(3) Uani d . 1
H H18 -0.0127 0.1014 0.0228 0.096 Uiso calc R 1
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'
P P 0.1023 0.0942 '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
P1 Pd P1 4 . 101.33(9) y
P1 Pd S1 4 . 171.41(7) y
P1 Pd S1 . . 86.90(7) y
P1 Pd S1 4 4 86.90(7) ?
P1 Pd S1 . 4 171.41(7) ?
S1 Pd S1 . 4 85.00(11) y
C2 P1 C7 . . 103.7(3) .
C2 P1 C13 . . 105.1(3) ?
C7 P1 C13 . . 106.7(3) .
C2 P1 Pd . . 106.9(2) .
C7 P1 Pd . . 118.7(2) .
C13 P1 Pd . . 114.4(2) .
C1 S1 Pd . . 106.1(2) .
C2 C1 C6 . . 117.9(7) ?
C2 C1 S1 . . 122.3(5) .
C6 C1 S1 . . 119.8(6) .
C3 C2 C1 . . 119.7(6) ?
C3 C2 P1 . . 122.7(6) ?
C1 C2 P1 . . 117.6(6) .
C4 C3 C2 . . 121.3(8) ?
C4 C3 H3 . . 119.3 ?
C2 C3 H3 . . 119.3 ?
C3 C4 C5 . . 119.5(8) ?
C3 C4 H4 . . 120.2 ?
C5 C4 H4 . . 120.2 ?
C6 C5 C4 . . 120.0(7) ?
C6 C5 H5 . . 120.0 ?
C4 C5 H5 . . 120.0 ?
C5 C6 C1 . . 121.5(7) ?
C5 C6 H6 . . 119.2 ?
C1 C6 H6 . . 119.2 ?
C8 C7 C12 . . 115.7(8) ?
C8 C7 P1 . . 125.5(6) ?
C12 C7 P1 . . 118.8(6) ?
C7 C8 C9 . . 121.0(9) ?
C7 C8 H8 . . 119.5 ?
C9 C8 H8 . . 119.5 ?
C10 C9 C8 . . 122.2(11) ?
C10 C9 H9 . . 118.9 ?
C8 C9 H9 . . 118.9 ?
C9 C10 C11 . . 118.7(11) ?
C9 C10 H10 . . 120.6 ?
C11 C10 H10 . . 120.6 ?
C10 C11 C12 . . 120.3(10) ?
C10 C11 H11 . . 119.9 ?
C12 C11 H11 . . 119.9 ?
C11 C12 C7 . . 122.0(9) ?
C11 C12 H12 . . 119.0 ?
C7 C12 H12 . . 119.0 ?
C18 C13 C14 . . 117.7(7) ?
C18 C13 P1 . . 122.0(6) ?
C14 C13 P1 . . 120.2(6) ?
C13 C14 C15 . . 121.8(10) ?
C13 C14 H14 . . 119.1 ?
C15 C14 H14 . . 119.1 ?
C14 C15 C16 . . 118.3(10) ?
C14 C15 H15 . . 120.8 ?
C16 C15 H15 . . 120.8 ?
C17 C16 C15 . . 120.4(9) ?
C17 C16 H16 . . 119.8 ?
C15 C16 H16 . . 119.8 ?
C18 C17 C16 . . 119.5(10) ?
C18 C17 H17 . . 120.3 ?
C16 C17 H17 . . 120.3 ?
C17 C18 C13 . . 122.2(8) ?
C17 C18 H18 . . 118.9 ?
C13 C18 H18 . . 118.9 ?
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 P1 4 2.2861(18) ?
Pd P1 . 2.2861(18) y
Pd S1 . 2.316(2) y
Pd S1 4 2.316(2) ?
P1 C2 . 1.805(7) .
P1 C7 . 1.818(7) .
P1 C13 . 1.818(7) .
S1 C1 . 1.740(7) .
C1 C2 . 1.398(8) ?
C1 C6 . 1.405(8) ?
C2 C3 . 1.390(9) ?
C3 C4 . 1.376(9) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.379(11) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.374(9) ?
C5 H5 . 0.9300 ?
C6 H6 . 0.9300 ?
C7 C8 . 1.368(9) ?
C7 C12 . 1.382(8) ?
C8 C9 . 1.386(10) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.312(10) ?
C9 H9 . 0.9300 ?
C10 C11 . 1.358(11) ?
C10 H10 . 0.9300 ?
C11 C12 . 1.375(10) ?
C11 H11 . 0.9300 ?
C12 H12 . 0.9300 ?
C13 C18 . 1.367(9) ?
C13 C14 . 1.379(9) ?
C14 C15 . 1.384(9) ?
C14 H14 . 0.9300 ?
C15 C16 . 1.386(11) ?
C15 H15 . 0.9300 ?
C16 C17 . 1.369(12) ?
C16 H16 . 0.9300 ?
C17 C18 . 1.364(10) ?
C17 H17 . 0.9300 ?
C18 H18 . 0.9300 ?
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
P1 Pd P1 C2 4 -177.7(2)
S1 Pd P1 C2 . 4.8(2)
S1 Pd P1 C2 4 -14.7(6)
P1 Pd P1 C7 4 65.6(2)
S1 Pd P1 C7 . -111.9(3)
S1 Pd P1 C7 4 -131.4(5)
P1 Pd P1 C13 4 -61.9(2)
S1 Pd P1 C13 . 120.6(3)
S1 Pd P1 C13 4 101.1(5)
P1 Pd S1 C1 4 -167.4(5)
P1 Pd S1 C1 . -4.1(2)
S1 Pd S1 C1 4 173.0(2)
Pd S1 C1 C2 . 2.5(6)
Pd S1 C1 C6 . -177.4(5)
C6 C1 C2 C3 . 1.0(10)
S1 C1 C2 C3 . -178.9(5)
C6 C1 C2 P1 . -178.5(5)
S1 C1 C2 P1 . 1.6(8)
C7 P1 C2 C3 . -58.1(6)
C13 P1 C2 C3 . 53.8(6)
Pd P1 C2 C3 . 175.7(5)
C7 P1 C2 C1 . 121.4(6)
C13 P1 C2 C1 . -126.8(5)
Pd P1 C2 C1 . -4.9(6)
C1 C2 C3 C4 . -0.3(11)
P1 C2 C3 C4 . 179.1(6)
C2 C3 C4 C5 . -0.9(11)
C3 C4 C5 C6 . 1.5(12)
C4 C5 C6 C1 . -0.8(11)
C2 C1 C6 C5 . -0.4(10)
S1 C1 C6 C5 . 179.5(6)
C2 P1 C7 C8 . 89.7(7)
C13 P1 C7 C8 . -21.0(8)
Pd P1 C7 C8 . -152.0(6)
C2 P1 C7 C12 . -89.0(7)
C13 P1 C7 C12 . 160.3(6)
Pd P1 C7 C12 . 29.3(7)
C12 C7 C8 C9 . 1.4(12)
P1 C7 C8 C9 . -177.3(7)
C7 C8 C9 C10 . 1.8(16)
C8 C9 C10 C11 . -3.2(18)
C9 C10 C11 C12 . 1.5(16)
C10 C11 C12 C7 . 1.8(14)
C8 C7 C12 C11 . -3.1(12)
P1 C7 C12 C11 . 175.7(6)
C2 P1 C13 C18 . -150.7(6)
C7 P1 C13 C18 . -40.9(7)
Pd P1 C13 C18 . 92.5(6)
C2 P1 C13 C14 . 33.4(6)
C7 P1 C13 C14 . 143.1(5)
Pd P1 C13 C14 . -83.5(6)
C18 C13 C14 C15 . -3.0(11)
P1 C13 C14 C15 . 173.1(6)
C13 C14 C15 C16 . 0.7(12)
C14 C15 C16 C17 . 2.4(14)
C15 C16 C17 C18 . -3.0(14)
C16 C17 C18 C13 . 0.5(14)
C14 C13 C18 C17 . 2.4(12)
P1 C13 C18 C17 . -173.6(6)
