#------------------------------------------------------------------------------
#$Date: 2016-03-05 11:01:17 +0200 (Sat, 05 Mar 2016) $
#$Revision: 177740 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/38/7223842.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_7223842
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                111.050(7)
_cell_angle_beta                 99.851(6)
_cell_angle_gamma                103.836(6)
_cell_formula_units_Z            1
_cell_length_a                   6.0243(4)
_cell_length_b                   8.0461(6)
_cell_length_c                   8.9366(7)
_cell_measurement_reflns_used    1947
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.2915
_cell_measurement_theta_min      5.5268
_cell_volume                     376.42(6)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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 (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0161
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_laue_measured_fraction_full 0.984
_diffrn_reflns_laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2501
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        74.949
_diffrn_reflns_theta_max         74.949
_diffrn_reflns_theta_min         5.531
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.036
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis PRO (Agilent, 2012)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_description       block
_exptl_crystal_F_000             204
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.824
_refine_diff_density_min         -1.602
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         1522
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0282
_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)+(0.0599P)²+0.1867P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0769
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1521
_reflns_number_total             1522
_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_original_cell_volume        376.42(5)
_cod_database_code               7223842
_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   0.197
_shelx_estimated_absorpt_t_max   0.466
_shelx_res_file
;

    shelx.res created by SHELXL-2014/7

TITL  6
CELL  1.54184 6.0243 8.0461 8.9366 111.050 99.851 103.836
ZERR  1       0.0004 0.0006 0.0007   0.007  0.006   0.006
LATT  1
SFAC  C H O S Pd
UNIT  10 18 2 4 1
ACTA  150
OMIT  -3 150
TEMP -173
SIZE  0.16 0.11 0.06
L.S.  24
FMAP  2
PLAN -1
BOND  $H
CONF
WGHT    0.059900    0.186700
FVAR       8.80688
PD    5    0.000000    0.500000    0.500000    10.50000    0.01315    0.00599 =
         0.01042    0.00228    0.00322    0.00128
S1    4    0.039404    0.404638    0.230459    11.00000    0.01562    0.00993 =
         0.01144    0.00085    0.00315   -0.00165
S2    4    0.371129    0.702030    0.530977    11.00000    0.01633    0.00834 =
         0.01091    0.00149    0.00311    0.00015
O1    3    0.442201    0.609397    0.226734    11.00000    0.01582    0.01015 =
         0.01280    0.00120    0.00360   -0.00343
C1    1    0.307135    0.579873    0.320528    11.00000    0.01742    0.00727 =
         0.01310    0.00318    0.00354    0.00334
C2    1    0.672633    0.760713    0.304606    11.00000    0.01460    0.00808 =
         0.01184    0.00129    0.00217   -0.00225
AFIX  23
H2A   2    0.781734    0.730728    0.379555    11.00000   -1.20000
H2B   2    0.651468    0.881113    0.371261    11.00000   -1.20000
AFIX   0
C3    1    0.773670    0.776214    0.164627    11.00000    0.01472    0.00899 =
         0.01301    0.00498    0.00445    0.00290
AFIX  13
H3    2    0.780300    0.649954    0.093882    11.00000   -1.20000
AFIX   0
C4    1    1.026383    0.915605    0.240006    11.00000    0.01697    0.01325 =
         0.01741    0.00668    0.00431    0.00009
AFIX 137
H4A   2    1.123294    0.873685    0.309456    11.00000   -1.50000
H4B   2    1.022508    1.040412    0.308982    11.00000   -1.50000
H4C   2    1.095973    0.922421    0.150089    11.00000   -1.50000
AFIX   0
C5    1    0.617239    0.836743    0.054369    11.00000    0.01840    0.01724 =
         0.01608    0.00960    0.00312    0.00476
AFIX 137
H5A   2    0.455815    0.745133    0.007304    11.00000   -1.50000
H5B   2    0.684824    0.842616   -0.036590    11.00000   -1.50000
H5C   2    0.610917    0.961234    0.121798    11.00000   -1.50000

AFIX   0
HKLF 4

REM   6
REM R1 =  0.0282 for    1521 Fo > 4sig(Fo)  and  0.0283 for all    1522 data
REM     81 parameters refined using      0 restraints

END

WGHT      0.0575      0.2169

REM Highest difference peak  0.824,  deepest hole -1.602,  1-sigma level  0.140
Q1    1   0.1220  0.5368  0.4833  11.00000  0.05    0.82
;
_shelx_res_checksum              88135
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 0.0000 0.5000 0.5000 0.01058(12) Uani 1 2 d S . P
S1 S 0.03940(12) 0.40464(9) 0.23046(8) 0.01465(17) Uani 1 1 d . . .
S2 S 0.37113(12) 0.70203(9) 0.53098(8) 0.01349(17) Uani 1 1 d . . .
O1 O 0.4422(4) 0.6094(3) 0.2267(3) 0.0156(4) Uani 1 1 d . . .
C1 C 0.3071(5) 0.5799(4) 0.3205(3) 0.0132(5) Uani 1 1 d . . .
C2 C 0.6726(5) 0.7607(4) 0.3046(3) 0.0137(5) Uani 1 1 d . . .
H2A H 0.7817 0.7307 0.3796 0.016 Uiso 1 1 calc R U .
H2B H 0.6515 0.8811 0.3713 0.016 Uiso 1 1 calc R U .
C3 C 0.7737(5) 0.7762(4) 0.1646(3) 0.0122(5) Uani 1 1 d . . .
H3 H 0.7803 0.6500 0.0939 0.015 Uiso 1 1 calc R U .
C4 C 1.0264(5) 0.9156(4) 0.2400(4) 0.0168(5) Uani 1 1 d . . .
H4A H 1.1233 0.8737 0.3095 0.025 Uiso 1 1 calc R U .
H4B H 1.0225 1.0404 0.3090 0.025 Uiso 1 1 calc R U .
H4C H 1.0960 0.9224 0.1501 0.025 Uiso 1 1 calc R U .
C5 C 0.6172(5) 0.8367(4) 0.0544(3) 0.0169(5) Uani 1 1 d . . .
H5A H 0.4558 0.7451 0.0073 0.025 Uiso 1 1 calc R U .
H5B H 0.6848 0.8426 -0.0366 0.025 Uiso 1 1 calc R U .
H5C H 0.6109 0.9612 0.1218 0.025 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 0.01315(18) 0.00599(17) 0.01042(17) 0.00228(12) 0.00322(11) 0.00128(11)
S1 0.0156(3) 0.0099(3) 0.0114(3) 0.0009(3) 0.0032(3) -0.0016(3)
S2 0.0163(3) 0.0083(3) 0.0109(3) 0.0015(2) 0.0031(2) 0.0002(3)
O1 0.0158(10) 0.0102(9) 0.0128(9) 0.0012(8) 0.0036(8) -0.0034(7)
C1 0.0174(13) 0.0073(11) 0.0131(12) 0.0032(10) 0.0035(10) 0.0033(10)
C2 0.0146(13) 0.0081(11) 0.0118(12) 0.0013(10) 0.0022(10) -0.0022(10)
C3 0.0147(12) 0.0090(11) 0.0130(12) 0.0050(10) 0.0045(10) 0.0029(10)
C4 0.0170(13) 0.0133(13) 0.0174(13) 0.0067(11) 0.0043(11) 0.0001(10)
C5 0.0184(13) 0.0172(13) 0.0161(13) 0.0096(11) 0.0031(11) 0.0048(10)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 '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_566 .
S1 Pd S2 75.83(3) 2_566 2_566
S1 Pd S2 104.17(2) . 2_566
S1 Pd S2 104.17(2) 2_566 .
S1 Pd S2 75.83(2) . .
S2 Pd S2 180.0 2_566 .
C1 S1 Pd 84.94(10) . .
C1 S2 Pd 84.63(10) . .
C1 O1 C2 119.1(2) . .
O1 C1 S1 119.2(2) . .
O1 C1 S2 126.2(2) . .
S1 C1 S2 114.59(17) . .
O1 C2 C3 107.0(2) . .
O1 C2 H2A 110.3 . .
C3 C2 H2A 110.3 . .
O1 C2 H2B 110.3 . .
C3 C2 H2B 110.3 . .
H2A C2 H2B 108.6 . .
C2 C3 C4 108.9(2) . .
C2 C3 C5 111.3(2) . .
C4 C3 C5 110.9(2) . .
C2 C3 H3 108.6 . .
C4 C3 H3 108.6 . .
C5 C3 H3 108.6 . .
C3 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C3 C5 H5A 109.5 . .
C3 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C3 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 2.3243(7) 2_566
Pd S1 2.3243(7) .
Pd S2 2.3333(7) 2_566
Pd S2 2.3333(7) .
S1 C1 1.700(3) .
S2 C1 1.701(3) .
O1 C1 1.306(4) .
O1 C2 1.465(3) .
C2 C3 1.512(4) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.523(4) .
C3 C5 1.531(4) .
C3 H3 1.0000 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
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 179.89(17)
C2 O1 C1 S2 0.0(4)
Pd S1 C1 O1 -179.7(2)
Pd S1 C1 S2 0.18(13)
Pd S2 C1 O1 179.7(2)
Pd S2 C1 S1 -0.18(13)
C1 O1 C2 C3 -173.4(2)
O1 C2 C3 C4 -173.3(2)
O1 C2 C3 C5 64.1(3)
