#------------------------------------------------------------------------------
#$Date: 2016-03-05 11:01:17 +0200 (Sat, 05 Mar 2016) $
#$Revision: 177740 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/38/7223838.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_7223838
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         'C6 H10 O2 Pd S4'
_chemical_formula_sum            'C6 H10 O2 Pd S4'
_chemical_formula_weight         348.78
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.5034(4)
_cell_length_b                   7.2125(4)
_cell_length_c                   20.7854(12)
_cell_measurement_reflns_used    4104
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.0733
_cell_measurement_theta_min      4.2514
_cell_volume                     1124.87(11)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     1.54178
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9418
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        74.998
_diffrn_reflns_theta_max         74.998
_diffrn_reflns_theta_min         4.254
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    19.997
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.07535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis PRO (Agilent, 2011)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.059
_exptl_crystal_description       prism
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.834
_refine_diff_density_min         -1.139
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         1154
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0251
_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)+(0.0460P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0721
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1044
_reflns_number_total             1154
_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               7223838
_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   0.108
_shelx_estimated_absorpt_t_max   0.435
_shelx_res_file
;

    shelx.res created by SHELXL-2014/7

TiTL  2
CELL  1.54178 7.5034 7.2125 20.7854 90.000 90.000 90.000
ZERR  4       0.0004 0.0004  0.0012  0.000  0.000  0.000
LATT  1
SYMM  0.5-X, -Y, 0.5+Z
SYMM -X, 0.5+Y, 0.5-Z
SYMM  0.5+X, 0.5-Y, -Z
SFAC  C H O S PD
UNIT  24 40 8 16 4
ACTA  150
OMIT  -3 150
TEMP -173
SIZE  0.05 0.1 0.2
L.S.  100
BOND  $H
CONF
FMAP  2
PLAN -1
WGHT    0.046000
FVAR       0.09699
PD    5    0.500000    0.500000    0.500000    10.50000    0.01122    0.01627 =
         0.00700   -0.00196    0.00078    0.00076
S1    4    0.614563    0.542898    0.396421    11.00000    0.01515    0.01970 =
         0.00938   -0.00156    0.00266    0.00331
S2    4    0.388464    0.787412    0.467708    11.00000    0.01523    0.01822 =
         0.00980   -0.00251    0.00252    0.00234
O1    3    0.505209    0.857889    0.348224    11.00000    0.01534    0.01889 =
         0.01037   -0.00141    0.00166    0.00266
C1    1    0.501250    0.747651    0.398383    11.00000    0.01100    0.01762 =
         0.01067   -0.00312    0.00001   -0.00186
C2    1    0.410783    1.035049    0.353174    11.00000    0.01843    0.01936 =
         0.01513   -0.00135    0.00116    0.00425
AFIX  23
H2A   2    0.458553    1.108966    0.389414    11.00000   -1.20000
H2B   2    0.282034    1.013839    0.360538    11.00000   -1.20000
AFIX   0
C3    1    0.439653    1.135423    0.290361    11.00000    0.03224    0.02410 =
         0.01606    0.00347    0.00259    0.00680
AFIX 137
H3A   2    0.375327    1.253657    0.291098    11.00000   -1.50000
H3B   2    0.395159    1.059016    0.254835    11.00000   -1.50000
H3C   2    0.567227    1.158805    0.284342    11.00000   -1.50000

AFIX   0
HKLF 4

REM   2
REM R1 =  0.0251 for    1044 Fo > 4sig(Fo)  and  0.0282 for all    1154 data
REM     62 parameters refined using      0 restraints

END

WGHT      0.0461      0.0000

REM Highest difference peak  0.834,  deepest hole -1.139,  1-sigma level  0.140
Q1    1   0.4999  0.4987  0.5683  11.00000  0.05    0.83
;
_shelx_res_checksum              2974
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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 0.01150(14) Uani 1 2 d S . P
S1 S 0.61456(7) 0.54290(9) 0.39642(2) 0.01474(16) Uani 1 1 d . . .
S2 S 0.38846(7) 0.78741(8) 0.46771(2) 0.01442(16) Uani 1 1 d . . .
O1 O 0.5052(2) 0.8579(3) 0.34822(8) 0.0149(4) Uani 1 1 d . . .
C1 C 0.5013(3) 0.7477(4) 0.39838(11) 0.0131(5) Uani 1 1 d . . .
C2 C 0.4108(4) 1.0350(4) 0.35317(11) 0.0176(5) Uani 1 1 d . . .
H2A H 0.4586 1.1090 0.3894 0.021 Uiso 1 1 calc R U .
H2B H 0.2820 1.0138 0.3605 0.021 Uiso 1 1 calc R U .
C3 C 0.4397(4) 1.1354(4) 0.29036(12) 0.0241(6) Uani 1 1 d . . .
H3A H 0.3753 1.2537 0.2911 0.036 Uiso 1 1 calc R U .
H3B H 0.3952 1.0590 0.2548 0.036 Uiso 1 1 calc R U .
H3C H 0.5672 1.1588 0.2843 0.036 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 0.0112(2) 0.0163(2) 0.00700(19) -0.00196(7) 0.00078(6) 0.00076(8)
S1 0.0151(3) 0.0197(3) 0.0094(3) -0.0016(2) 0.00266(17) 0.0033(2)
S2 0.0152(3) 0.0182(3) 0.0098(3) -0.00251(19) 0.00252(17) 0.0023(2)
O1 0.0153(9) 0.0189(10) 0.0104(8) -0.0014(7) 0.0017(5) 0.0027(7)
C1 0.0110(12) 0.0176(14) 0.0107(11) -0.0031(9) 0.0000(6) -0.0019(8)
C2 0.0184(11) 0.0194(12) 0.0151(11) -0.0013(9) 0.0012(8) 0.0042(11)
C3 0.0322(15) 0.0241(14) 0.0161(11) 0.0035(10) 0.0026(10) 0.0068(12)
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
S2 Pd S2 180.00(2) 5_666 .
S2 Pd S1 75.50(2) 5_666 5_666
S2 Pd S1 104.50(2) . 5_666
S2 Pd S1 104.50(2) 5_666 .
S2 Pd S1 75.50(2) . .
S1 Pd S1 180.0 5_666 .
C1 S1 Pd 84.79(8) . .
C1 S2 Pd 85.14(10) . .
C1 O1 C2 117.52(19) . .
O1 C1 S2 125.8(2) . .
O1 C1 S1 119.66(17) . .
S2 C1 S1 114.57(15) . .
O1 C2 C3 106.8(2) . .
O1 C2 H2A 110.4 . .
C3 C2 H2A 110.4 . .
O1 C2 H2B 110.4 . .
C3 C2 H2B 110.4 . .
H2A C2 H2B 108.6 . .
C2 C3 H3A 109.5 . .
C2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C2 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd S2 2.3341(6) 5_666
Pd S2 2.3341(6) .
Pd S1 2.3387(5) 5_666
Pd S1 2.3388(5) .
S1 C1 1.705(3) .
S2 C1 1.695(2) .
O1 C1 1.311(3) .
O1 C2 1.465(3) .
C2 C3 1.509(3) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 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 S2 2.9(3)
C2 O1 C1 S1 -177.93(17)
Pd S2 C1 O1 179.0(2)
Pd S2 C1 S1 -0.20(11)
Pd S1 C1 O1 -179.04(18)
Pd S1 C1 S2 0.20(11)
C1 O1 C2 C3 178.7(2)
