#------------------------------------------------------------------------------
#$Date: 2016-03-05 11:01:17 +0200 (Sat, 05 Mar 2016) $
#$Revision: 177740 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/38/7223841.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_7223841
loop_
_publ_author_name
'Tan, Yee Seng'
'Halim, Siti Nadiah Abdul'
'Molloy, Kieran C.'
'Sudlow, Anna L.'
'Otero-de-la-Roza, A.'
'Tiekink, Edward R. T.'
_publ_section_title
;
 Persistence of C--H⋯π(chelate ring) interactions in the crystal
 structures of Pd(S2COR)2. The utility of Pd(S2COR)2as precursors for
 palladium sulphide materials
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              1105
_journal_paper_doi               10.1039/C5CE02126J
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C10 H18 O2 Pd S4'
_chemical_formula_sum            'C10 H18 O2 Pd S4'
_chemical_formula_weight         404.88
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-04-09 deposited with the CCDC.
2016-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                72.420(6)
_cell_angle_beta                 78.467(6)
_cell_angle_gamma                79.852(5)
_cell_formula_units_Z            1
_cell_length_a                   5.7038(4)
_cell_length_b                   6.7822(4)
_cell_length_c                   10.5967(8)
_cell_measurement_reflns_used    2755
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4981
_cell_measurement_theta_min      3.1689
_cell_volume                     379.94(5)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2012)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2012)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2012)'
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg, 2006)
;
_computing_publication_material  'SHELXL (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4041
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Agilent Technologies SuperNova Dual diffractometer with Atlas detector'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_monochromator  Mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5606
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.496
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         3.175
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.758
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58086
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis PRO (Agilent, 2012)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_description       prism
_exptl_crystal_F_000             204
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.984
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     80
_refine_ls_number_reflns         1752
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0240
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0357P)²+0.2633P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0613
_refine_ls_wR_factor_ref         0.0638
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1646
_reflns_number_total             1752
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ce02126j2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7223837--7223848.cif.'
_cod_database_code               7223841
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.720
_shelx_estimated_absorpt_t_max   0.917
_shelx_res_file
;

    shelx.res created by SHELXL-2014/7

TITL  5
CELL  0.71073 5.7038 6.7822 10.5967 72.420 78.467 79.852
ZERR  1       0.0004 0.0004  0.0008  0.006  0.006  0.005
LATT  1
SFAC  C  H  O  S  Pd
UNIT  10 18 2 4 1
L.S.  100
ACTA  55.0
OMIT  -3 55.0
TEMP -173
SIZE  0.05 0.05 0.2
BOND  $H
CONF
FMAP 2
PLAN -1
WGHT    0.035700    0.263300
FVAR       6.72422
PD    5    0.500000    0.500000    0.500000    10.50000    0.01181    0.01350 =
         0.02039   -0.00662   -0.00217   -0.00274
S1    4    0.682022    0.409987    0.305079    11.00000    0.01480    0.01963 =
         0.02337   -0.00909    0.00118   -0.00674
S2    4    0.261969    0.264376    0.482553    11.00000    0.01341    0.01708 =
         0.02047   -0.00764   -0.00001   -0.00476
O1    3    0.450537    0.148944    0.258439    11.00000    0.01731    0.02002 =
         0.02080   -0.00805    0.00143   -0.00839
C1    1    0.458580    0.257150    0.339735    11.00000    0.01451    0.01430 =
         0.02119   -0.00455   -0.00312   -0.00029
C2    1    0.256504    0.018282    0.286613    11.00000    0.01469    0.01845 =
         0.02333   -0.00771   -0.00134   -0.00628
AFIX  23
H2A   2    0.096761    0.102772    0.294543    11.00000   -1.20000
H2B   2    0.267195   -0.094225    0.371089    11.00000   -1.20000
AFIX   0
C3    1    0.293371   -0.071874    0.168808    11.00000    0.01673    0.02005 =
         0.02028   -0.00693   -0.00063   -0.00531
AFIX  23
H3A   2    0.457154   -0.149578    0.160300    11.00000   -1.20000
H3B   2    0.282657    0.043509    0.085697    11.00000   -1.20000
AFIX   0
C4    1    0.108899   -0.217041    0.182978    11.00000    0.02052    0.02210 =
         0.02036   -0.00715   -0.00029   -0.00761
AFIX  23
H4A   2   -0.054391   -0.137655    0.185679    11.00000   -1.20000
H4B   2    0.112714   -0.328228    0.268527    11.00000   -1.20000
AFIX   0
C5    1    0.158888   -0.315848    0.067080    11.00000    0.03362    0.03408 =
         0.02506   -0.01458    0.00153   -0.01548
AFIX 137
H5A   2    0.032534   -0.402732    0.076833    11.00000   -1.50000
H5B   2    0.315864   -0.402270    0.067905    11.00000   -1.50000
H5C   2    0.160372   -0.205997   -0.017932    11.00000   -1.50000

AFIX   0
HKLF 4

REM   5
REM R1 =  0.0240 for    1646 Fo > 4sig(Fo)  and  0.0263 for all    1752 data
REM     80 parameters refined using      0 restraints

END

WGHT      0.0357      0.2742

REM Highest difference peak  0.984,  deepest hole -0.818,  1-sigma level  0.102
Q1    1   0.4926  0.4581  0.5918  11.00000  0.05    0.98
;
_shelx_res_checksum              98876
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pd Pd 0.5000 0.5000 0.5000 0.01470(9) Uani 1 2 d S . P
S1 S 0.68202(10) 0.40999(9) 0.30508(6) 0.01858(13) Uani 1 1 d . . .
S2 S 0.26197(9) 0.26438(8) 0.48255(5) 0.01645(13) Uani 1 1 d . . .
O1 O 0.4505(3) 0.1489(2) 0.25844(16) 0.0187(3) Uani 1 1 d . . .
C1 C 0.4586(4) 0.2572(3) 0.3397(2) 0.0169(4) Uani 1 1 d . . .
C2 C 0.2565(4) 0.0183(3) 0.2866(2) 0.0181(4) Uani 1 1 d . . .
H2A H 0.0968 0.1028 0.2945 0.022 Uiso 1 1 calc R U .
H2B H 0.2672 -0.0942 0.3711 0.022 Uiso 1 1 calc R U .
C3 C 0.2934(4) -0.0719(4) 0.1688(2) 0.0187(4) Uani 1 1 d . . .
H3A H 0.4572 -0.1496 0.1603 0.022 Uiso 1 1 calc R U .
H3B H 0.2827 0.0435 0.0857 0.022 Uiso 1 1 calc R U .
C4 C 0.1089(4) -0.2170(4) 0.1830(2) 0.0205(5) Uani 1 1 d . . .
H4A H -0.0544 -0.1377 0.1857 0.025 Uiso 1 1 calc R U .
H4B H 0.1127 -0.3282 0.2685 0.025 Uiso 1 1 calc R U .
C5 C 0.1589(5) -0.3158(4) 0.0671(3) 0.0289(5) Uani 1 1 d . . .
H5A H 0.0325 -0.4027 0.0768 0.043 Uiso 1 1 calc R U .
H5B H 0.3159 -0.4023 0.0679 0.043 Uiso 1 1 calc R U .
H5C H 0.1604 -0.2060 -0.0179 0.043 Uiso 1 1 calc R U .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd 0.01181(13) 0.01350(13) 0.02039(14) -0.00662(9) -0.00217(9) -0.00274(8)
S1 0.0148(3) 0.0196(3) 0.0234(3) -0.0091(2) 0.0012(2) -0.0067(2)
S2 0.0134(2) 0.0171(3) 0.0205(3) -0.0076(2) 0.0000(2) -0.0048(2)
O1 0.0173(8) 0.0200(8) 0.0208(8) -0.0081(6) 0.0014(6) -0.0084(6)
C1 0.0145(10) 0.0143(10) 0.0212(11) -0.0045(8) -0.0031(8) -0.0003(8)
C2 0.0147(10) 0.0185(10) 0.0233(11) -0.0077(8) -0.0013(8) -0.0063(8)
C3 0.0167(10) 0.0201(11) 0.0203(11) -0.0069(8) -0.0006(8) -0.0053(8)
C4 0.0205(11) 0.0221(11) 0.0204(11) -0.0072(9) -0.0003(9) -0.0076(9)
C5 0.0336(14) 0.0341(14) 0.0251(13) -0.0146(10) 0.0015(10) -0.0155(11)
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
S1 Pd S1 180.0 2_666 .
S1 Pd S2 104.43(2) 2_666 .
S1 Pd S2 75.57(2) . .
S1 Pd S2 75.57(2) 2_666 2_666
S1 Pd S2 104.43(2) . 2_666
S2 Pd S2 180.0 . 2_666
C1 S1 Pd 85.35(8) . .
C1 S2 Pd 84.73(8) . .
C1 O1 C2 119.73(18) . .
O1 C1 S1 119.29(17) . .
O1 C1 S2 126.35(17) . .
S1 C1 S2 114.36(13) . .
O1 C2 C3 105.43(17) . .
O1 C2 H2A 110.7 . .
C3 C2 H2A 110.7 . .
O1 C2 H2B 110.7 . .
C3 C2 H2B 110.7 . .
H2A C2 H2B 108.8 . .
C2 C3 C4 112.57(18) . .
C2 C3 H3A 109.1 . .
C4 C3 H3A 109.1 . .
C2 C3 H3B 109.1 . .
C4 C3 H3B 109.1 . .
H3A C3 H3B 107.8 . .
C3 C4 C5 111.54(19) . .
C3 C4 H4A 109.3 . .
C5 C4 H4A 109.3 . .
C3 C4 H4B 109.3 . .
C5 C4 H4B 109.3 . .
H4A C4 H4B 108.0 . .
C4 C5 H5A 109.5 . .
C4 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C4 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd S1 2.3233(6) 2_666
Pd S1 2.3233(6) .
Pd S2 2.3398(5) .
Pd S2 2.3398(5) 2_666
S1 C1 1.698(2) .
S2 C1 1.702(2) .
O1 C1 1.301(3) .
O1 C2 1.467(3) .
C2 C3 1.512(3) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.520(3) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 C5 1.526(3) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 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
C2 O1 C1 S1 -179.27(15)
C2 O1 C1 S2 0.4(3)
Pd S1 C1 O1 179.36(17)
Pd S1 C1 S2 -0.38(11)
Pd S2 C1 O1 -179.3(2)
Pd S2 C1 S1 0.38(11)
C1 O1 C2 C3 176.37(18)
O1 C2 C3 C4 178.73(18)
C2 C3 C4 C5 -176.6(2)
