# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1058645'
_audit_update_record             
;
2015-04-09 deposited with the CCDC.
2016-01-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H6 O2 Pd S4'
_chemical_formula_sum            'C4 H6 O2 Pd S4'
_chemical_formula_weight         320.73

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   6.2713(5)
_cell_length_b                   13.5593(11)
_cell_length_c                   10.7931(8)
_cell_angle_alpha                90
_cell_angle_beta                 97.635(9)
_cell_angle_gamma                90
_cell_volume                     909.65(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1052
_cell_measurement_theta_min      1.8999
_cell_measurement_theta_max      27.4982

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.342
_exptl_crystal_F_000             624
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    2.903
_shelx_estimated_absorpt_T_min   0.868
_shelx_estimated_absorpt_T_max   0.868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.69526
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'CrysAlis PRO (Agilent, 2012)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  Mirror
_diffrn_measurement_device_type  
'Agilent Technologies SuperNova Dual diffractometer with Atlas detector'
_diffrn_detector_area_resol_mean 10.4041
_diffrn_measurement_method       'ω scan'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            4854
_diffrn_reflns_av_unetI/netI     0.0687
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.005
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_full        27.500
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2080
_reflns_number_gt                1455
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlis PRO (Agilent, 2012)'
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2012)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2012)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg, 2006)
;
_computing_publication_material  'SHELXL (Sheldrick, 2015)'

_refine_special_details          
;
The (0 1 1) reflection was omitted opwing to poor agreement
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0214P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2080
_refine_ls_number_parameters     102
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0421
_refine_ls_wR_factor_ref         0.0834
_refine_ls_wR_factor_gt          0.0709
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.59290(7) 0.88382(3) 0.09688(4) 0.01212(13) Uani 1 1 d . . . . .
S1 S 0.4128(2) 0.87170(9) -0.10503(13) 0.0143(3) Uani 1 1 d . . . . .
S2 S 0.8672(2) 0.87685(9) -0.02984(13) 0.0141(3) Uani 1 1 d . . . . .
S3 S 0.7711(2) 0.88997(9) 0.30062(13) 0.0141(3) Uani 1 1 d . . . . .
S4 S 0.3171(2) 0.88152(9) 0.22357(13) 0.0131(3) Uani 1 1 d . . . . .
O1 O 0.6825(6) 0.8595(2) -0.2679(3) 0.0148(8) Uani 1 1 d . . . . .
O2 O 0.5013(6) 0.8850(3) 0.4627(3) 0.0162(9) Uani 1 1 d . . . . .
C1 C 0.6631(9) 0.8675(4) -0.1495(5) 0.0141(12) Uani 1 1 d . . . . .
C2 C 0.8982(9) 0.8575(4) -0.3032(5) 0.0189(13) Uani 1 1 d . . . . .
H2A H 0.8896 0.8465 -0.3935 0.028 Uiso 1 1 calc R U . . .
H2B H 0.9808 0.8041 -0.2584 0.028 Uiso 1 1 calc R U . . .
H2C H 0.9697 0.9206 -0.2815 0.028 Uiso 1 1 calc R U . . .
C3 C 0.5203(8) 0.8853(3) 0.3435(5) 0.0128(12) Uani 1 1 d . . . . .
C4 C 0.2866(9) 0.8798(4) 0.5002(5) 0.0199(13) Uani 1 1 d . . . . .
H4A H 0.2981 0.8789 0.5916 0.030 Uiso 1 1 calc R U . . .
H4B H 0.2147 0.8196 0.4663 0.030 Uiso 1 1 calc R U . . .
H4C H 0.2029 0.9375 0.4678 0.030 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 0.0130(2) 0.0163(2) 0.0070(2) -0.00032(18) 0.00098(16) 0.00009(18)
S1 0.0133(7) 0.0204(7) 0.0089(7) 0.0001(6) 0.0009(5) -0.0001(6)
S2 0.0124(7) 0.0213(7) 0.0084(7) -0.0020(6) 0.0011(5) -0.0001(6)
S3 0.0124(7) 0.0201(7) 0.0097(7) -0.0006(6) 0.0008(5) 0.0003(6)
S4 0.0134(7) 0.0184(7) 0.0075(7) 0.0006(6) 0.0015(5) 0.0002(6)
O1 0.016(2) 0.020(2) 0.009(2) 0.0000(17) 0.0026(16) 0.0001(15)
O2 0.013(2) 0.029(2) 0.007(2) 0.0039(17) 0.0034(16) 0.0016(16)
C1 0.017(3) 0.017(3) 0.009(3) 0.002(2) 0.003(2) 0.001(2)
C2 0.017(3) 0.025(3) 0.016(3) 0.000(3) 0.007(2) -0.002(2)
C3 0.016(3) 0.009(3) 0.013(3) 0.001(2) 0.001(2) -0.002(2)
C4 0.014(3) 0.032(3) 0.014(3) 0.000(3) 0.006(2) -0.002(2)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd S1 2.3233(15) . ?
Pd S3 2.3320(15) . ?
Pd S2 2.3376(15) . ?
Pd S4 2.3432(15) . ?
S1 C1 1.702(6) . ?
S2 C1 1.698(6) . ?
S3 C3 1.698(5) . ?
S4 C3 1.693(5) . ?
O1 C1 1.304(6) . ?
O1 C2 1.454(6) . ?
O2 C3 1.307(6) . ?
O2 C4 1.458(6) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?

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
_geom_angle_publ_flag
S1 Pd S3 177.93(5) . . ?
S1 Pd S2 75.66(5) . . ?
S3 Pd S2 104.80(5) . . ?
S1 Pd S4 103.99(5) . . ?
S3 Pd S4 75.44(5) . . ?
S2 Pd S4 176.91(4) . . ?
C1 S1 Pd 85.13(19) . . ?
C1 S2 Pd 84.76(19) . . ?
C3 S3 Pd 84.89(19) . . ?
C3 S4 Pd 84.65(19) . . ?
C1 O1 C2 118.0(4) . . ?
C3 O2 C4 118.8(4) . . ?
O1 C1 S2 126.3(4) . . ?
O1 C1 S1 119.2(4) . . ?
S2 C1 S1 114.4(3) . . ?
O1 C2 H2A 109.5 . . ?
O1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
O1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O2 C3 S4 126.5(4) . . ?
O2 C3 S3 118.5(4) . . ?
S4 C3 S3 115.0(3) . . ?
O2 C4 H4A 109.5 . . ?
O2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
O2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 O1 C1 S2 0.5(7) . . . . ?
C2 O1 C1 S1 179.1(3) . . . . ?
Pd S2 C1 O1 -179.9(5) . . . . ?
Pd S2 C1 S1 1.3(3) . . . . ?
Pd S1 C1 O1 179.8(4) . . . . ?
Pd S1 C1 S2 -1.4(3) . . . . ?
C4 O2 C3 S4 0.9(7) . . . . ?
C4 O2 C3 S3 -179.3(4) . . . . ?
Pd S4 C3 O2 -179.2(4) . . . . ?
Pd S4 C3 S3 1.0(3) . . . . ?
Pd S3 C3 O2 179.2(4) . . . . ?
Pd S3 C3 S4 -1.0(3) . . . . ?

_refine_diff_density_max         0.673
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.187

_shelx_res_file                  
;

    shelx.res created by SHELXL-2014/7

TITL  P2(1)/c
CELL  0.71073 6.2713 13.5593 10.7931 90.000 97.635 90.000
ZERR  4       0.0005  0.0011  0.0008  0.000  0.009  0.000
LATT  1
SYMM -x, y+1/2,-z+1/2
SFAC  C H O S Pd
UNIT  16 24 8 16 4
ACTA  55.0
OMIT  -3 55.0
TEMP -173
SIZE  0.05 0.05 0.05
L.S.  100
OMIT  0   1   1
BOND  $H
CONF
FMAP  2
PLAN -1
SIZE  0.05 0.05 0.05
WGHT    0.021400
FVAR       1.16123
PD    5    0.592904    0.883823    0.096877    11.00000    0.01296    0.01628 =
         0.00703   -0.00032    0.00098    0.00009
S1    4    0.412778    0.871703   -0.105025    11.00000    0.01331    0.02045 =
         0.00887    0.00013    0.00088   -0.00014
S2    4    0.867226    0.876847   -0.029839    11.00000    0.01240    0.02134 =
         0.00837   -0.00204    0.00106   -0.00011
S3    4    0.771059    0.889972    0.300620    11.00000    0.01240    0.02010 =
         0.00967   -0.00064    0.00083    0.00033
S4    4    0.317099    0.881518    0.223566    11.00000    0.01339    0.01839 =
         0.00753    0.00063    0.00147    0.00020
O1    3    0.682451    0.859465   -0.267869    11.00000    0.01589    0.01963 =
         0.00921   -0.00001    0.00265    0.00009
O2    3    0.501327    0.885026    0.462676    11.00000    0.01310    0.02879 =
         0.00723    0.00388    0.00345    0.00161
C1    1    0.663056    0.867484   -0.149472    11.00000    0.01743    0.01677 =
         0.00865    0.00225    0.00338    0.00072
C2    1    0.898234    0.857497   -0.303196    11.00000    0.01691    0.02468 =
         0.01624   -0.00009    0.00659   -0.00209
AFIX 137
H2A   2    0.889648    0.846483   -0.393460    11.00000   -1.50000
H2B   2    0.980796    0.804053   -0.258406    11.00000   -1.50000
H2C   2    0.969685    0.920629   -0.281528    11.00000   -1.50000
AFIX   0
C3    1    0.520347    0.885257    0.343543    11.00000    0.01615    0.00941 =
         0.01270    0.00104    0.00127   -0.00183
C4    1    0.286624    0.879808    0.500167    11.00000    0.01440    0.03242 =
         0.01393    0.00015    0.00586   -0.00250
AFIX 137
H4A   2    0.298060    0.878870    0.591602    11.00000   -1.50000
H4B   2    0.214661    0.819580    0.466292    11.00000   -1.50000
H4C   2    0.202864    0.937465    0.467803    11.00000   -1.50000

AFIX   0
HKLF 4

REM   P2(1)/c
REM R1 =  0.0421 for    1455 Fo > 4sig(Fo)  and  0.0714 for all    2080 data
REM    102 parameters refined using      0 restraints

END

WGHT      0.0216      0.0000

REM Highest difference peak  0.673,  deepest hole -0.880,  1-sigma level  0.187
Q1    1   0.4379  0.7819  0.0485  11.00000  0.05    0.67
;
_shelx_res_checksum              37048
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1058646'
_audit_update_record             
;
2015-04-09 deposited with the CCDC.
2016-01-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H10 O2 Pd S4'
_chemical_formula_sum            'C6 H10 O2 Pd S4'
_chemical_formula_weight         348.78

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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.
;

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'

_cell_length_a                   7.5034(4)
_cell_length_b                   7.2125(4)
_cell_length_c                   20.7854(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1124.87(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4104
_cell_measurement_theta_min      4.2514
_cell_measurement_theta_max      75.0733

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.059
_exptl_crystal_F_000             688
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    19.997
_shelx_estimated_absorpt_T_min   0.108
_shelx_estimated_absorpt_T_max   0.435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.07535
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'CrysAlis PRO (Agilent, 2011)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  Mirror
_diffrn_measurement_device_type  
'Agilent Technologies SuperNova Dual diffractometer with Atlas detector'
_diffrn_detector_area_resol_mean 10.4041
_diffrn_measurement_method       'ω scan'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            9418
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         4.254
_diffrn_reflns_theta_max         74.998
_diffrn_reflns_theta_full        74.998
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1154
_reflns_number_gt                1044
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlis PRO (Agilent, 2012)'
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2012)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2012)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg, 2006)
;
_computing_publication_material  'SHELXL (Sheldrick, 2015)'

_refine_special_details          
;
The maximum and minimum residual electron density peaks of 
0.83 and 1.14 eÅ⁻³, respectively, were located 1.17 Å and 0.71 Å
from the S1 and Pd atoms, resepctively.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0460P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1154
_refine_ls_number_parameters     62
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0251
_refine_ls_wR_factor_ref         0.0721
_refine_ls_wR_factor_gt          0.0691
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_restrained_S_all      1.127
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
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)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
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_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
_geom_angle_publ_flag
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_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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
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) . . . . ?

_refine_diff_density_max         0.834
_refine_diff_density_min         -1.139
_refine_diff_density_rms         0.140

_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
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1058647'
_audit_update_record             
;
2015-04-09 deposited with the CCDC.
2016-01-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H14 O2 Pd S4'
_chemical_formula_sum            'C8 H14 O2 Pd S4'
_chemical_formula_weight         376.83

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.4778(4)
_cell_length_b                   9.5272(6)
_cell_length_c                   9.8084(5)
_cell_angle_alpha                74.832(5)
_cell_angle_beta                 86.458(4)
_cell_angle_gamma                76.292(5)
_cell_volume                     655.22(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2199
_cell_measurement_theta_min      3.5220
_cell_measurement_theta_max      27.5340

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.910
_exptl_crystal_F_000             376
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    2.031
_shelx_estimated_absorpt_T_min   0.675
_shelx_estimated_absorpt_T_max   0.871
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.807
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_process_details   'CrysAlis PRO (Agilent, 2012)'
_exptl_absorpt_special_details   ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
2 -1 -13 0.0543 1.9974 -1.0304 -13.0547 -0.6604 -0.7250 0.0780
10 0 -1 0.0235 10.0182 -0.0026 -1.0086 -0.8621 0.4199 0.2073
-4 -13 -2 0.0968 -4.0114 -13.0332 -1.9928 -0.0405 0.0237 -0.9881
8 0 8 0.0165 8.0187 0.0169 8.0302 -0.3699 0.9105 0.0918
-3 0 13 0.0116 -2.9995 0.0282 13.0562 0.7201 0.7033 -0.1691
4 13 4 0.0939 4.0123 13.0375 4.0013 0.1132 0.1069 0.9712
-8 1 -8 0.0542 -8.0185 0.9853 -8.0313 0.3929 -0.9373 -0.0206


_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  Mirror
_diffrn_measurement_device_type  
'Agilent Technologies SuperNova Dual diffractometer with Atlas detector'
_diffrn_detector_area_resol_mean 10.4041
_diffrn_measurement_method       'ω scan'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            5652
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.181
_diffrn_reflns_theta_max         27.492
_diffrn_reflns_theta_full        27.492
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3011
_reflns_number_gt                2414
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlis PRO (Agilent, 2012)'
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2012)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2012)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg, 2006)
;
_computing_publication_material  'SHELXL (Sheldrick, 2015)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0293P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3011
_refine_ls_number_parameters     136
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0334
_refine_ls_wR_factor_ref         0.0775
_refine_ls_wR_factor_gt          0.0694
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.78104(3) 0.69729(3) 0.46038(3) 0.01508(10) Uani 1 1 d . . . . .
S1 S 0.71208(12) 0.60277(10) 0.69613(9) 0.01712(19) Uani 1 1 d . . . . .
S2 S 0.76692(11) 0.45062(10) 0.47628(9) 0.01571(19) Uani 1 1 d . . . . .
S3 S 0.83751(11) 0.79751(10) 0.22172(9) 0.01638(19) Uani 1 1 d . . . . .
S4 S 0.77460(12) 0.94766(10) 0.44382(9) 0.01741(19) Uani 1 1 d . . . . .
O1 O 0.6793(3) 0.3286(3) 0.7434(2) 0.0170(5) Uani 1 1 d . . . . .
O2 O 0.8229(3) 1.0824(3) 0.1722(2) 0.0190(5) Uani 1 1 d . . . . .
C1 C 0.7151(4) 0.4430(4) 0.6486(3) 0.0153(7) Uani 1 1 d . . . . .
C2 C 0.6895(5) 0.1879(4) 0.7042(3) 0.0168(7) Uani 1 1 d . . . . .
H2A H 0.8061 0.1595 0.6540 0.020 Uiso 1 1 calc R U . . .
H2B H 0.5853 0.1982 0.6420 0.020 Uiso 1 1 calc R U . . .
C3 C 0.6804(5) 0.0722(4) 0.8407(4) 0.0201(8) Uani 1 1 d . . . . .
H3A H 0.5668 0.1054 0.8923 0.024 Uiso 1 1 calc R U . . .
H3B H 0.7871 0.0616 0.9006 0.024 Uiso 1 1 calc R U . . .
C4 C 0.6814(5) -0.0780(4) 0.8134(4) 0.0214(8) Uani 1 1 d . . . . .
H4A H 0.6754 -0.1515 0.9036 0.032 Uiso 1 1 calc R U . . .
H4B H 0.5747 -0.0678 0.7554 0.032 Uiso 1 1 calc R U . . .
H4C H 0.7948 -0.1115 0.7637 0.032 Uiso 1 1 calc R U . . .
C5 C 0.8125(4) 0.9608(4) 0.2685(3) 0.0154(7) Uani 1 1 d . . . . .
C6 C 0.7920(4) 1.2249(4) 0.2119(4) 0.0164(7) Uani 1 1 d . . . . .
H6A H 0.8921 1.2229 0.2744 0.020 Uiso 1 1 calc R U . . .
H6B H 0.6735 1.2434 0.2625 0.020 Uiso 1 1 calc R U . . .
C7 C 0.7891(5) 1.3451(4) 0.0768(4) 0.0242(8) Uani 1 1 d . . . . .
H7A H 0.6824 1.3511 0.0190 0.029 Uiso 1 1 calc R U . . .
H7B H 0.9024 1.3189 0.0223 0.029 Uiso 1 1 calc R U . . .
C8 C 0.7766(5) 1.4952(4) 0.1055(4) 0.0243(8) Uani 1 1 d . . . . .
H8A H 0.7750 1.5709 0.0157 0.036 Uiso 1 1 calc R U . . .
H8B H 0.6634 1.5222 0.1580 0.036 Uiso 1 1 calc R U . . .
H8C H 0.8833 1.4901 0.1613 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 0.01753(15) 0.01428(16) 0.01404(16) -0.00458(11) 0.00007(11) -0.00376(11)
S1 0.0232(4) 0.0148(5) 0.0143(4) -0.0060(4) 0.0013(4) -0.0040(4)
S2 0.0198(4) 0.0157(5) 0.0135(4) -0.0062(4) 0.0013(3) -0.0052(3)
S3 0.0206(4) 0.0150(5) 0.0148(4) -0.0063(4) 0.0009(4) -0.0040(4)
S4 0.0244(4) 0.0164(5) 0.0128(4) -0.0054(3) 0.0012(4) -0.0056(4)
O1 0.0217(12) 0.0148(13) 0.0165(13) -0.0082(10) 0.0024(10) -0.0036(10)
O2 0.0291(13) 0.0136(13) 0.0162(13) -0.0067(10) 0.0020(11) -0.0058(11)
C1 0.0141(16) 0.0192(19) 0.0129(18) -0.0036(14) 0.0008(13) -0.0053(14)
C2 0.0221(17) 0.0149(19) 0.0158(18) -0.0070(15) 0.0011(15) -0.0062(15)
C3 0.0243(18) 0.021(2) 0.0171(19) -0.0076(15) 0.0046(15) -0.0070(16)
C4 0.0261(18) 0.019(2) 0.0195(19) -0.0057(15) 0.0002(16) -0.0043(16)
C5 0.0148(16) 0.0153(19) 0.0157(18) -0.0043(15) -0.0006(14) -0.0019(14)
C6 0.0179(16) 0.0107(18) 0.0208(19) -0.0060(14) 0.0011(14) -0.0017(14)
C7 0.038(2) 0.018(2) 0.017(2) -0.0041(16) 0.0034(17) -0.0089(17)
C8 0.039(2) 0.019(2) 0.0155(19) -0.0036(15) 0.0028(17) -0.0106(17)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd S1 2.3253(9) . ?
Pd S4 2.3371(9) . ?
Pd S3 2.3386(9) . ?
Pd S2 2.3414(9) . ?
S1 C1 1.700(3) . ?
S2 C1 1.697(3) . ?
S3 C5 1.700(3) . ?
S4 C5 1.702(3) . ?
O1 C1 1.304(4) . ?
O1 C2 1.473(4) . ?
O2 C5 1.304(4) . ?
O2 C6 1.471(4) . ?
C2 C3 1.505(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.522(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C6 C7 1.505(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.509(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?

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
_geom_angle_publ_flag
S1 Pd S4 103.84(3) . . ?
S1 Pd S3 177.62(3) . . ?
S4 Pd S3 75.53(3) . . ?
S1 Pd S2 75.51(3) . . ?
S4 Pd S2 176.34(3) . . ?
S3 Pd S2 104.97(3) . . ?
C1 S1 Pd 85.20(11) . . ?
C1 S2 Pd 84.76(12) . . ?
C5 S3 Pd 84.91(12) . . ?
C5 S4 Pd 84.91(12) . . ?
C1 O1 C2 119.4(2) . . ?
C5 O2 C6 119.6(3) . . ?
O1 C1 S2 126.3(3) . . ?
O1 C1 S1 119.2(2) . . ?
S2 C1 S1 114.5(2) . . ?
O1 C2 C3 105.9(2) . . ?
O1 C2 H2A 110.6 . . ?
C3 C2 H2A 110.6 . . ?
O1 C2 H2B 110.6 . . ?
C3 C2 H2B 110.6 . . ?
H2A C2 H2B 108.7 . . ?
C2 C3 C4 110.9(3) . . ?
C2 C3 H3A 109.5 . . ?
C4 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 108.1 . . ?
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 . . ?
O2 C5 S3 119.8(2) . . ?
O2 C5 S4 125.6(3) . . ?
S3 C5 S4 114.6(2) . . ?
O2 C6 C7 106.8(3) . . ?
O2 C6 H6A 110.4 . . ?
C7 C6 H6A 110.4 . . ?
O2 C6 H6B 110.4 . . ?
C7 C6 H6B 110.4 . . ?
H6A C6 H6B 108.6 . . ?
C6 C7 C8 111.5(3) . . ?
C6 C7 H7A 109.3 . . ?
C8 C7 H7A 109.3 . . ?
C6 C7 H7B 109.3 . . ?
C8 C7 H7B 109.3 . . ?
H7A C7 H7B 108.0 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 O1 C1 S2 2.4(4) . . . . ?
C2 O1 C1 S1 -177.4(2) . . . . ?
Pd S2 C1 O1 178.8(3) . . . . ?
Pd S2 C1 S1 -1.34(16) . . . . ?
Pd S1 C1 O1 -178.8(3) . . . . ?
Pd S1 C1 S2 1.35(16) . . . . ?
C1 O1 C2 C3 168.5(3) . . . . ?
O1 C2 C3 C4 177.5(3) . . . . ?
C6 O2 C5 S3 177.0(2) . . . . ?
C6 O2 C5 S4 -2.9(4) . . . . ?
Pd S3 C5 O2 -177.7(3) . . . . ?
Pd S3 C5 S4 2.18(16) . . . . ?
Pd S4 C5 O2 177.7(3) . . . . ?
Pd S4 C5 S3 -2.18(16) . . . . ?
C5 O2 C6 C7 -172.9(3) . . . . ?
O2 C6 C7 C8 -174.5(3) . . . . ?

_refine_diff_density_max         0.928
_refine_diff_density_min         -0.967
_refine_diff_density_rms         0.135

_shelx_res_file                  
;

    shelx.res created by SHELXL-2014/7


TITL  3
CELL  0.71073 7.4778 9.5272 9.8084 74.832 86.458 76.292
ZERR  2       0.0004 0.0006 0.0005  0.005  0.004  0.005
LATT  1
SFAC  C H O S Pd
UNIT  16 28 4 8 2
ACTA  55.0
OMIT  -3 55.0
TEMP -173
SIZE  0.20 0.04 0.04
L.S.  100
BOND  $H
CONF
FMAP  2
PLAN -1
SIZE  0.07 0.09 0.21
WGHT    0.029300
FVAR       3.50148
PD    5    0.781036    0.697293    0.460376    11.00000    0.01753    0.01428 =
         0.01404   -0.00458    0.00007   -0.00376
S1    4    0.712082    0.602774    0.696135    11.00000    0.02322    0.01481 =
         0.01434   -0.00603    0.00129   -0.00404
S2    4    0.766916    0.450617    0.476280    11.00000    0.01977    0.01568 =
         0.01351   -0.00618    0.00130   -0.00520
S3    4    0.837507    0.797506    0.221715    11.00000    0.02064    0.01500 =
         0.01475   -0.00628    0.00088   -0.00395
S4    4    0.774595    0.947655    0.443821    11.00000    0.02437    0.01638 =
         0.01281   -0.00543    0.00118   -0.00564
O1    3    0.679295    0.328559    0.743376    11.00000    0.02168    0.01480 =
         0.01647   -0.00822    0.00240   -0.00359
O2    3    0.822855    1.082407    0.172240    11.00000    0.02913    0.01362 =
         0.01624   -0.00669    0.00205   -0.00578
C1    1    0.715093    0.442953    0.648583    11.00000    0.01410    0.01922 =
         0.01291   -0.00364    0.00077   -0.00527
C2    1    0.689470    0.187851    0.704188    11.00000    0.02213    0.01495 =
         0.01583   -0.00704    0.00113   -0.00616
AFIX  23
H2A   2    0.806070    0.159547    0.654018    11.00000   -1.20000
H2B   2    0.585264    0.198229    0.641967    11.00000   -1.20000
AFIX   0
C3    1    0.680390    0.072243    0.840737    11.00000    0.02427    0.02083 =
         0.01705   -0.00759    0.00462   -0.00700
AFIX  23
H3A   2    0.566800    0.105362    0.892286    11.00000   -1.20000
H3B   2    0.787102    0.061564    0.900606    11.00000   -1.20000
AFIX   0
C4    1    0.681419   -0.078023    0.813431    11.00000    0.02613    0.01856 =
         0.01947   -0.00573    0.00017   -0.00435
AFIX  33
H4A   2    0.675435   -0.151472    0.903633    11.00000   -1.50000
H4B   2    0.574732   -0.067805    0.755384    11.00000   -1.50000
H4C   2    0.794753   -0.111547    0.763694    11.00000   -1.50000
AFIX   0
C5    1    0.812536    0.960796    0.268463    11.00000    0.01476    0.01534 =
         0.01572   -0.00433   -0.00060   -0.00186
C6    1    0.792025    1.224906    0.211898    11.00000    0.01786    0.01073 =
         0.02082   -0.00603    0.00113   -0.00167
AFIX  23
H6A   2    0.892126    1.222911    0.274381    11.00000   -1.20000
H6B   2    0.673495    1.243350    0.262481    11.00000   -1.20000
AFIX   0
C7    1    0.789113    1.345130    0.076826    11.00000    0.03809    0.01808 =
         0.01706   -0.00413    0.00336   -0.00893
AFIX  23
H7A   2    0.682379    1.351052    0.018970    11.00000   -1.20000
H7B   2    0.902431    1.318943    0.022284    11.00000   -1.20000
AFIX   0
C8    1    0.776585    1.495235    0.105489    11.00000    0.03938    0.01915 =
         0.01553   -0.00360    0.00279   -0.01062
AFIX  33
H8A   2    0.774967    1.570910    0.015705    11.00000   -1.50000
H8B   2    0.663387    1.522187    0.158034    11.00000   -1.50000
H8C   2    0.883264    1.490103    0.161346    11.00000   -1.50000

AFIX   0
HKLF 4

REM   3
REM R1 =  0.0334 for    2414 Fo > 4sig(Fo)  and  0.0473 for all    3011 data
REM    136 parameters refined using      0 restraints

END

WGHT      0.0294      0.0000

REM Highest difference peak  0.928,  deepest hole -0.967,  1-sigma level  0.135
Q1    1   0.7985  0.7864  0.4208  11.00000  0.05    0.93
;
_shelx_res_checksum              3402
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1058648'
_audit_update_record             
;
2015-04-09 deposited with the CCDC.
2016-01-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H14 O2 Pd S4'
_chemical_formula_sum            'C8 H14 O2 Pd S4'
_chemical_formula_weight         376.83

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.9077(6)
_cell_length_b                   5.8720(3)
_cell_length_c                   11.9621(6)
_cell_angle_alpha                90
_cell_angle_beta                 102.752(5)
_cell_angle_gamma                90
_cell_volume                     678.77(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3211
_cell_measurement_theta_min      4.0360
_cell_measurement_theta_max      27.5440

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.844
_exptl_crystal_F_000             376
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.190
_exptl_absorpt_coefficient_mu    1.961
_shelx_estimated_absorpt_T_min   0.555
_shelx_estimated_absorpt_T_max   0.707
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.591
_exptl_absorpt_correction_T_max  0.748
_exptl_absorpt_process_details   'CrysAlis PRO (Agilent, 2012)'

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
12 1 -12 0.1063 12.0191 1.0490 -11.5002 0.6000 -0.7000 -0.4000
11 1 8 0.1623 10.7132 0.8562 8.3178 -0.5000 -0.9000 0.0000
-13 0 0 0.1415 -12.9786 -0.0313 -0.1090 0.1000 0.9000 0.3000
6 -7 -7 0.1295 5.6018 -7.0901 -6.8029 0.0000 0.0000 -1.0000
3 -6 9 0.1896 2.9028 -5.8734 9.0019 -0.8000 -0.1000 -0.5000
10 -4 6 0.1893 9.5531 -3.8424 6.2557 -0.6000 -0.6000 -0.5000
2 8 0 0.1239 2.4614 8.3541 -0.3878 0.4000 -0.5000 0.8000
13 1 -3 0.1218 13.2710 0.6823 -2.9750 0.1000 -0.9000 -0.3000
7 1 13 0.1792 6.7573 1.0712 12.6272 -0.7000 -0.7000 0.2000
-6 7 7 0.1492 -5.6018 7.0901 6.8029 0.0000 0.0000 1.0000
-8 0 -11 0.1591 -7.8776 0.3469 -11.2666 0.7000 0.7000 0.0000
-2 -1 -17 0.1765 -1.5297 -1.0102 -16.8691 0.9000 0.4000 -0.4000
1 -8 -3 0.1257 0.9344 -7.8601 -3.2413 -0.2000 0.3000 -0.9000
-11 0 12 0.0596 -11.3077 -0.0640 12.2480 -0.6000 0.6000 0.5000

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  Mirror
_diffrn_measurement_device_type  
'Agilent Technologies SuperNova Dual diffractometer with Atlas detector'
_diffrn_detector_area_resol_mean 10.4041
_diffrn_measurement_method       'ω scan'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            5337
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.019
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_full        27.496
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1555
_reflns_number_gt                1452
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlis PRO (Agilent, 2012)'
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2012)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2012)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg, 2006)
;
_computing_publication_material  'SHELXL (Sheldrick, 2015)'

_refine_special_details          
;
The maximum and minimum residual electron density peaks of 
1.68 and 0.85 eÅ⁻³, respectively, were located 1.83 Å and 0.79 Å
from the S2 and Pd atoms, resepctively.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0483P)²+0.2921P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1555
_refine_ls_number_parameters     72
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0277
_refine_ls_wR_factor_ref         0.0741
_refine_ls_wR_factor_gt          0.0718
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.5000 0.5000 0.5000 0.01261(11) Uani 1 2 d S . P . .
S1 S 0.28809(6) 0.33503(10) 0.50421(5) 0.01805(16) Uani 1 1 d . . . . .
S2 S 0.33767(6) 0.71947(10) 0.37361(5) 0.01620(15) Uani 1 1 d . . . . .
O1 O 0.08522(19) 0.5440(3) 0.36852(16) 0.0164(4) Uani 1 1 d . . . . .
C1 C 0.2184(3) 0.5406(4) 0.4079(2) 0.0147(5) Uani 1 1 d . . . . .
C2 C 0.0211(2) 0.7160(4) 0.2815(2) 0.0152(5) Uani 1 1 d . . . . .
H2 H 0.0836 0.7474 0.2282 0.018 Uiso 1 1 calc R U . . .
C3 C -0.0025(3) 0.9316(4) 0.3432(2) 0.0203(5) Uani 1 1 d . . . . .
H3A H 0.0867 0.9926 0.3845 0.030 Uiso 1 1 calc R U . . .
H3B H -0.0604 0.8979 0.3979 0.030 Uiso 1 1 calc R U . . .
H3C H -0.0491 1.0442 0.2874 0.030 Uiso 1 1 calc R U . . .
C4 C -0.1100(3) 0.6053(4) 0.2176(2) 0.0210(5) Uani 1 1 d . . . . .
H4A H -0.0876 0.4616 0.1841 0.032 Uiso 1 1 calc R U . . .
H4B H -0.1572 0.7070 0.1564 0.032 Uiso 1 1 calc R U . . .
H4C H -0.1706 0.5750 0.2705 0.032 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 0.01080(16) 0.01286(16) 0.01284(16) 0.00102(8) -0.00028(11) -0.00071(8)
S1 0.0135(3) 0.0179(3) 0.0206(3) 0.0070(2) -0.0008(2) -0.0023(2)
S2 0.0123(3) 0.0163(3) 0.0188(3) 0.0053(2) 0.0007(2) -0.0015(2)
O1 0.0134(8) 0.0164(8) 0.0177(9) 0.0051(7) 0.0000(7) -0.0005(7)
C1 0.0154(12) 0.0139(10) 0.0144(12) -0.0011(9) 0.0022(9) -0.0003(9)
C2 0.0141(11) 0.0170(11) 0.0127(11) 0.0032(9) -0.0006(9) 0.0003(9)
C3 0.0180(13) 0.0175(11) 0.0245(13) -0.0023(11) 0.0029(10) -0.0011(10)
C4 0.0179(12) 0.0219(13) 0.0202(12) -0.0015(10) -0.0025(10) -0.0014(10)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd S1 2.3229(6) . ?
Pd S1 2.3229(6) 3_666 ?
Pd S2 2.3366(6) . ?
Pd S2 2.3366(6) 3_666 ?
S1 C1 1.706(3) . ?
S2 C1 1.697(3) . ?
O1 C1 1.300(3) . ?
O1 C2 1.488(3) . ?
C2 C4 1.502(3) . ?
C2 C3 1.509(3) . ?
C2 H2 1.0000 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?

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
_geom_angle_publ_flag
S1 Pd S1 180.0 . 3_666 ?
S1 Pd S2 75.39(2) . . ?
S1 Pd S2 104.61(2) 3_666 . ?
S1 Pd S2 104.61(2) . 3_666 ?
S1 Pd S2 75.39(2) 3_666 3_666 ?
S2 Pd S2 180.00(2) . 3_666 ?
C1 S1 Pd 85.60(9) . . ?
C1 S2 Pd 85.34(9) . . ?
C1 O1 C2 120.43(19) . . ?
O1 C1 S2 127.46(19) . . ?
O1 C1 S1 118.86(19) . . ?
S2 C1 S1 113.67(15) . . ?
O1 C2 C4 104.49(18) . . ?
O1 C2 C3 108.40(19) . . ?
C4 C2 C3 113.7(2) . . ?
O1 C2 H2 110.0 . . ?
C4 C2 H2 110.0 . . ?
C3 C2 H2 110.0 . . ?
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 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 O1 C1 S2 1.2(3) . . . . ?
C2 O1 C1 S1 -178.00(16) . . . . ?
Pd S2 C1 O1 -179.1(2) . . . . ?
Pd S2 C1 S1 0.15(13) . . . . ?
Pd S1 C1 O1 179.2(2) . . . . ?
Pd S1 C1 S2 -0.15(13) . . . . ?
C1 O1 C2 C4 153.3(2) . . . . ?
C1 O1 C2 C3 -85.1(3) . . . . ?

_refine_diff_density_max         1.684
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.123

_shelx_res_file                  
;

    shelx.res created by SHELXL-2014/7

TITL 4
CELL  0.71073 9.9077 5.8720 11.9621 90.000 102.752 90.000
ZERR  2       0.0006 0.0003  0.0006  0.000   0.005  0.000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2
SFAC  C H O S Pd
UNIT  16 28 4 8 2
ACTA  55.0
OMIT  -3 55.0
TEMP -173
L.S.  24
BOND  $H
CONF
FMAP  2
PLAN -1
SIZE  0.19 0.27 0.34
WGHT    0.048300    0.292100
FVAR       5.75108
PD    5    0.500000    0.500000    0.500000    10.50000    0.01080    0.01286 =
         0.01284    0.00102   -0.00028   -0.00071
S1    4    0.288087    0.335029    0.504209    11.00000    0.01349    0.01794 =
         0.02058    0.00697   -0.00081   -0.00228
S2    4    0.337675    0.719468    0.373608    11.00000    0.01233    0.01628 =
         0.01876    0.00533    0.00074   -0.00149
O1    3    0.085215    0.544002    0.368517    11.00000    0.01341    0.01644 =
         0.01771    0.00509   -0.00005   -0.00051
C1    1    0.218413    0.540605    0.407889    11.00000    0.01539    0.01393 =
         0.01438   -0.00106    0.00218   -0.00029
C2    1    0.021081    0.715986    0.281546    11.00000    0.01412    0.01702 =
         0.01265    0.00318   -0.00064    0.00032
AFIX  13
H2    2    0.083623    0.747351    0.228182    11.00000   -1.20000
AFIX   0
C3    1   -0.002483    0.931588    0.343239    11.00000    0.01804    0.01753 =
         0.02454   -0.00234    0.00287   -0.00114
AFIX 137
H3A   2    0.086711    0.992601    0.384506    11.00000   -1.50000
H3B   2   -0.060380    0.897938    0.397857    11.00000   -1.50000
H3C   2   -0.049081    1.044216    0.287412    11.00000   -1.50000
AFIX   0
C4    1   -0.109953    0.605287    0.217560    11.00000    0.01794    0.02186 =
         0.02021   -0.00147   -0.00249   -0.00141
AFIX 137
H4A   2   -0.087638    0.461561    0.184102    11.00000   -1.50000
H4B   2   -0.157168    0.707011    0.156359    11.00000   -1.50000
H4C   2   -0.170564    0.575049    0.270464    11.00000   -1.50000
AFIX   0
HKLF  4

REM  4
REM R1 =  0.0277 for    1452 Fo > 4sig(Fo)  and  0.0313 for all    1555 data
REM     72 parameters refined using      0 restraints

END

WGHT      0.0459      0.3406

REM Highest difference peak  1.684,  deepest hole -0.853,  1-sigma level  0.123
Q1    1   0.3994  1.0034  0.4245  11.00000  0.05    1.68
;
_shelx_res_checksum              33568
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1058649'
_audit_update_record             
;
2015-04-09 deposited with the CCDC.
2016-01-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H18 O2 Pd S4'
_chemical_formula_sum            'C10 H18 O2 Pd S4'
_chemical_formula_weight         404.88

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   5.7038(4)
_cell_length_b                   6.7822(4)
_cell_length_c                   10.5967(8)
_cell_angle_alpha                72.420(6)
_cell_angle_beta                 78.467(6)
_cell_angle_gamma                79.852(5)
_cell_volume                     379.94(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2755
_cell_measurement_theta_min      3.1689
_cell_measurement_theta_max      27.4981

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_F_000             204
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.758
_shelx_estimated_absorpt_T_min   0.720
_shelx_estimated_absorpt_T_max   0.917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.58086
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'CrysAlis PRO (Agilent, 2012)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  Mirror
_diffrn_measurement_device_type  
'Agilent Technologies SuperNova Dual diffractometer with Atlas detector'
_diffrn_detector_area_resol_mean 10.4041
_diffrn_measurement_method       'ω scan'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            5606
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.175
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_full        27.496
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1752
_reflns_number_gt                1646
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlis PRO (Agilent, 2012)'
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2012)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2012)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg, 2006)
;
_computing_publication_material  'SHELXL (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0357P)²+0.2633P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1752
_refine_ls_number_parameters     80
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0240
_refine_ls_wR_factor_ref         0.0638
_refine_ls_wR_factor_gt          0.0613
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_restrained_S_all      1.103
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
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)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
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_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
_geom_angle_publ_flag
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_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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
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) . . . . ?

_refine_diff_density_max         0.984
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.102

_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
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1058650'
_audit_update_record             
;
2015-04-09 deposited with the CCDC.
2016-01-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H18 O2 Pd S4'
_chemical_formula_sum            'C10 H18 O2 Pd S4'
_chemical_formula_weight         404.88

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.0243(4)
_cell_length_b                   8.0461(6)
_cell_length_c                   8.9366(7)
_cell_angle_alpha                111.050(7)
_cell_angle_beta                 99.851(6)
_cell_angle_gamma                103.836(6)
_cell_volume                     376.42(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1947
_cell_measurement_theta_min      5.5268
_cell_measurement_theta_max      76.2915

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_F_000             204
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    15.036
_shelx_estimated_absorpt_T_min   0.197
_shelx_estimated_absorpt_T_max   0.466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.28094
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'CrysAlis PRO (Agilent, 2012)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  Mirror
_diffrn_measurement_device_type  
'Agilent Technologies SuperNova Dual diffractometer with Atlas detector'
_diffrn_detector_area_resol_mean 10.4041
_diffrn_measurement_method       'ω scan'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            2501
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_av_R_equivalents  0.0161
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         5.531
_diffrn_reflns_theta_max         74.949
_diffrn_reflns_theta_full        74.949
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.984
_reflns_number_total             1522
_reflns_number_gt                1521
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlis PRO (Agilent, 2012)'
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2012)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2012)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg, 2006)
;
_computing_publication_material  'SHELXL (Sheldrick, 2015)'

_refine_special_details          
;
The maximum and minimum residual electron density peaks of 
0.82 and 1.60 eÅ⁻³, respectively, were located 0.78 Å and 0.83 Å
from the Pd atom.
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0599P)²+0.1867P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1522
_refine_ls_number_parameters     81
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0282
_refine_ls_wR_factor_ref         0.0769
_refine_ls_wR_factor_gt          0.0766
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
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)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
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_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
_geom_angle_publ_flag
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_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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
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) . . . . ?

_refine_diff_density_max         0.824
_refine_diff_density_min         -1.602
_refine_diff_density_rms         0.140

_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
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1058651'
_audit_update_record             
;
2015-04-09 deposited with the CCDC.
2016-01-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H26 O2 Pd S4'
_chemical_formula_sum            'C14 H26 O2 Pd S4'
_chemical_formula_weight         460.99

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.0663(5)
_cell_length_b                   8.4457(3)
_cell_length_c                   9.2536(4)
_cell_angle_alpha                63.740(4)
_cell_angle_beta                 73.752(3)
_cell_angle_gamma                83.782(3)
_cell_volume                     475.40(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4745
_cell_measurement_theta_min      2.9971
_cell_measurement_theta_max      27.4937

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_F_000             236
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.416
_shelx_estimated_absorpt_T_min   0.765
_shelx_estimated_absorpt_T_max   0.933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.74644
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'CrysAlis PRO (Agilent, 2011)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  Mirror
_diffrn_measurement_device_type  
'Agilent Technologies SuperNova Dual diffractometer with Atlas detector'
_diffrn_detector_area_resol_mean 10.4041
_diffrn_measurement_method       'ω scan'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7620
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.003
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_full        27.496
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2173
_reflns_number_gt                2069
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlis PRO (Agilent, 2012)'
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2012)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2012)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg, 2006)
;
_computing_publication_material  'SHELXL (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0212P)²+0.2194P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2173
_refine_ls_number_parameters     99
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0181
_refine_ls_R_factor_gt           0.0166
_refine_ls_wR_factor_ref         0.0429
_refine_ls_wR_factor_gt          0.0418
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 1.0000 0.5000 0.5000 0.01188(6) Uani 1 2 d S . P . .
S1 S 0.77367(5) 0.38897(5) 0.76027(4) 0.01574(8) Uani 1 1 d . . . . .
S2 S 0.72124(5) 0.67242(5) 0.45738(4) 0.01474(8) Uani 1 1 d . . . . .
O1 O 0.44900(15) 0.56582(14) 0.75165(12) 0.0158(2) Uani 1 1 d . . . . .
C1 C 0.6232(2) 0.54792(19) 0.66490(17) 0.0137(3) Uani 1 1 d . . . . .
C2 C 0.3183(2) 0.70022(19) 0.66677(17) 0.0149(3) Uani 1 1 d . . . . .
H2A H 0.2877 0.6753 0.5806 0.018 Uiso 1 1 calc R U . . .
H2B H 0.3813 0.8188 0.6123 0.018 Uiso 1 1 calc R U . . .
C3 C 0.1331(2) 0.6917(2) 0.79951(17) 0.0162(3) Uani 1 1 d . . . . .
H3A H 0.1674 0.7110 0.8873 0.019 Uiso 1 1 calc R U . . .
H3B H 0.0717 0.5727 0.8518 0.019 Uiso 1 1 calc R U . . .
C4 C -0.0140(2) 0.82930(19) 0.72828(17) 0.0148(3) Uani 1 1 d . . . . .
H4A H -0.0328 0.8205 0.6300 0.018 Uiso 1 1 calc R U . . .
H4B H 0.0416 0.9482 0.6895 0.018 Uiso 1 1 calc R U . . .
C5 C -0.2151(2) 0.80987(19) 0.85325(18) 0.0145(3) Uani 1 1 d . . . . .
H5 H -0.2649 0.6863 0.8978 0.017 Uiso 1 1 calc R U . . .
C6 C -0.2024(2) 0.8415(2) 1.00089(19) 0.0198(3) Uani 1 1 d . . . . .
H6A H -0.3337 0.8268 1.0778 0.030 Uiso 1 1 calc R U . . .
H6B H -0.1525 0.9616 0.9600 0.030 Uiso 1 1 calc R U . . .
H6C H -0.1128 0.7562 1.0594 0.030 Uiso 1 1 calc R U . . .
C7 C -0.3622(2) 0.9355(2) 0.7662(2) 0.0205(3) Uani 1 1 d . . . . .
H7A H -0.4937 0.9118 0.8441 0.031 Uiso 1 1 calc R U . . .
H7B H -0.3652 0.9178 0.6692 0.031 Uiso 1 1 calc R U . . .
H7C H -0.3221 1.0577 0.7296 0.031 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 0.01076(8) 0.01460(9) 0.01127(8) -0.00703(6) -0.00213(6) 0.00094(5)
S1 0.01457(17) 0.01729(18) 0.01276(17) -0.00514(14) -0.00302(14) 0.00306(13)
S2 0.01327(17) 0.01773(17) 0.01103(16) -0.00544(14) -0.00181(13) 0.00185(13)
O1 0.0133(5) 0.0182(5) 0.0122(5) -0.0047(4) -0.0023(4) 0.0033(4)
C1 0.0142(7) 0.0150(7) 0.0141(6) -0.0081(5) -0.0035(5) -0.0001(5)
C2 0.0131(7) 0.0181(7) 0.0127(6) -0.0061(6) -0.0043(5) 0.0034(5)
C3 0.0146(7) 0.0191(7) 0.0118(6) -0.0053(6) -0.0024(5) 0.0029(6)
C4 0.0151(7) 0.0163(7) 0.0120(6) -0.0054(5) -0.0033(5) 0.0008(5)
C5 0.0134(7) 0.0147(7) 0.0158(7) -0.0074(6) -0.0034(5) 0.0014(5)
C6 0.0210(8) 0.0225(8) 0.0177(7) -0.0113(6) -0.0054(6) 0.0056(6)
C7 0.0176(7) 0.0217(8) 0.0258(8) -0.0127(7) -0.0091(6) 0.0057(6)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd S1 2.3256(4) 2_766 ?
Pd S1 2.3256(4) . ?
Pd S2 2.3370(4) . ?
Pd S2 2.3370(4) 2_766 ?
S1 C1 1.6968(15) . ?
S2 C1 1.7028(15) . ?
O1 C1 1.3025(17) . ?
O1 C2 1.4659(17) . ?
C2 C3 1.5063(19) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.519(2) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.5320(19) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C7 1.526(2) . ?
C5 C6 1.5306(19) . ?
C5 H5 1.0000 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?

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
_geom_angle_publ_flag
S1 Pd S1 180.0 2_766 . ?
S1 Pd S2 104.353(13) 2_766 . ?
S1 Pd S2 75.647(13) . . ?
S1 Pd S2 75.647(13) 2_766 2_766 ?
S1 Pd S2 104.353(13) . 2_766 ?
S2 Pd S2 180.0 . 2_766 ?
C1 S1 Pd 85.16(5) . . ?
C1 S2 Pd 84.67(5) . . ?
C1 O1 C2 118.99(11) . . ?
O1 C1 S1 119.55(11) . . ?
O1 C1 S2 125.95(11) . . ?
S1 C1 S2 114.50(8) . . ?
O1 C2 C3 106.33(11) . . ?
O1 C2 H2A 110.5 . . ?
C3 C2 H2A 110.5 . . ?
O1 C2 H2B 110.5 . . ?
C3 C2 H2B 110.5 . . ?
H2A C2 H2B 108.7 . . ?
C2 C3 C4 111.71(11) . . ?
C2 C3 H3A 109.3 . . ?
C4 C3 H3A 109.3 . . ?
C2 C3 H3B 109.3 . . ?
C4 C3 H3B 109.3 . . ?
H3A C3 H3B 107.9 . . ?
C3 C4 C5 113.60(12) . . ?
C3 C4 H4A 108.8 . . ?
C5 C4 H4A 108.8 . . ?
C3 C4 H4B 108.8 . . ?
C5 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
C7 C5 C6 110.06(12) . . ?
C7 C5 C4 110.33(12) . . ?
C6 C5 C4 112.27(12) . . ?
C7 C5 H5 108.0 . . ?
C6 C5 H5 108.0 . . ?
C4 C5 H5 108.0 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 O1 C1 S1 -178.23(9) . . . . ?
C2 O1 C1 S2 2.03(19) . . . . ?
Pd S1 C1 O1 -178.20(11) . . . . ?
Pd S1 C1 S2 1.57(7) . . . . ?
Pd S2 C1 O1 178.18(13) . . . . ?
Pd S2 C1 S1 -1.57(7) . . . . ?
C1 O1 C2 C3 -178.48(12) . . . . ?
O1 C2 C3 C4 178.36(11) . . . . ?
C2 C3 C4 C5 172.25(12) . . . . ?
C3 C4 C5 C7 -172.20(12) . . . . ?
C3 C4 C5 C6 64.63(16) . . . . ?

_refine_diff_density_max         0.431
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.061

_shelx_res_file                  
;

    shelx.res created by SHELXL-2014/7

TITL  11
CELL  0.71073 7.0663 8.4457 9.2536 63.740 73.752 83.782
ZERR  1       0.0005 0.0003 0.0004  0.004  0.003  0.003
LATT  1
SFAC  C  H  O  S  Pd
UNIT  14 26 2 4 1
L.S.  100
ACTA  55.0
OMIT  -3 55.0
TEMP -173
SIZE  0.05 0.2 0.2
BOND  $H
CONF
FMAP  2
PLAN -1
WGHT    0.021200    0.219400
FVAR       7.43463
PD    5    1.000000    0.500000    0.500000    10.50000    0.01076    0.01460 =
         0.01127   -0.00703   -0.00213    0.00094
S1    4    0.773670    0.388972    0.760266    11.00000    0.01457    0.01729 =
         0.01276   -0.00514   -0.00302    0.00306
S2    4    0.721235    0.672417    0.457379    11.00000    0.01327    0.01773 =
         0.01103   -0.00544   -0.00181    0.00185
O1    3    0.448996    0.565818    0.751648    11.00000    0.01333    0.01820 =
         0.01215   -0.00467   -0.00228    0.00333
C1    1    0.623199    0.547922    0.664898    11.00000    0.01417    0.01497 =
         0.01407   -0.00805   -0.00353   -0.00012
C2    1    0.318257    0.700221    0.666774    11.00000    0.01305    0.01814 =
         0.01272   -0.00614   -0.00429    0.00337
AFIX  23
H2A   2    0.287728    0.675338    0.580649    11.00000   -1.20000
H2B   2    0.381283    0.818831    0.612279    11.00000   -1.20000
AFIX   0
C3    1    0.133078    0.691730    0.799510    11.00000    0.01460    0.01913 =
         0.01181   -0.00526   -0.00245    0.00286
AFIX  23
H3A   2    0.167370    0.711008    0.887253    11.00000   -1.20000
H3B   2    0.071665    0.572663    0.851833    11.00000   -1.20000
AFIX   0
C4    1   -0.013984    0.829298    0.728276    11.00000    0.01506    0.01626 =
         0.01200   -0.00539   -0.00335    0.00083
AFIX  23
H4A   2   -0.032820    0.820453    0.630012    11.00000   -1.20000
H4B   2    0.041640    0.948237    0.689535    11.00000   -1.20000
AFIX   0
C5    1   -0.215118    0.809870    0.853247    11.00000    0.01344    0.01472 =
         0.01577   -0.00745   -0.00340    0.00142
AFIX  13
H5    2   -0.264944    0.686346    0.897811    11.00000   -1.20000
AFIX   0
C6    1   -0.202379    0.841479    1.000888    11.00000    0.02101    0.02252 =
         0.01770   -0.01132   -0.00541    0.00565
AFIX 137
H6A   2   -0.333717    0.826825    1.077789    11.00000   -1.50000
H6B   2   -0.152471    0.961629    0.960014    11.00000   -1.50000
H6C   2   -0.112794    0.756222    1.059394    11.00000   -1.50000
AFIX   0
C7    1   -0.362159    0.935522    0.766246    11.00000    0.01762    0.02174 =
         0.02584   -0.01272   -0.00912    0.00567
AFIX 137
H7A   2   -0.493673    0.911764    0.844051    11.00000   -1.50000
H7B   2   -0.365166    0.917792    0.669159    11.00000   -1.50000
H7C   2   -0.322101    1.057729    0.729636    11.00000   -1.50000

AFIX   0
HKLF 4

REM   11
REM R1 =  0.0166 for    2069 Fo > 4sig(Fo)  and  0.0181 for all    2173 data
REM     99 parameters refined using      0 restraints

END

WGHT      0.0203      0.2181

REM Highest difference peak  0.431,  deepest hole -0.429,  1-sigma level  0.061
Q1    1  -0.1217  0.8142  0.7931  11.00000  0.05    0.43
;
_shelx_res_checksum              97605
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1058652'
_audit_update_record             
;
2015-04-09 deposited with the CCDC.
2016-01-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H26 O2 Pd S4'
_chemical_formula_sum            'C14 H26 O2 Pd S4'
_chemical_formula_weight         460.99

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.1398(6)
_cell_length_b                   6.7176(5)
_cell_length_c                   11.9393(10)
_cell_angle_alpha                90.020(7)
_cell_angle_beta                 99.397(7)
_cell_angle_gamma                95.377(7)
_cell_volume                     483.63(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3530
_cell_measurement_theta_min      3.7499
_cell_measurement_theta_max      76.7014

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_F_000             236
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    11.778
_shelx_estimated_absorpt_T_min   0.202
_shelx_estimated_absorpt_T_max   0.590
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.34731
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'CrysAlis PRO (Agilent, 2012)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  Mirror
_diffrn_measurement_device_type  
'Agilent Technologies SuperNova Dual diffractometer with Atlas detector'
_diffrn_detector_area_resol_mean 10.4041
_diffrn_measurement_method       'ω scan'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7538
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.753
_diffrn_reflns_theta_max         74.970
_diffrn_reflns_theta_full        74.970
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             1979
_reflns_number_gt                1861
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlis PRO (Agilent, 2012)'
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2012)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2012)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg, 2006)
;
_computing_publication_material  'SHELXL (Sheldrick, 2015)'

_refine_special_details          
;
The maximum and minimum residual electron density peaks of 
4.37 and 2.03 eÅ⁻³, respectively, were located 0.96 Å and 0.89 Å
from the Pd atom.
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1297P)²+0.3746P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1979
_refine_ls_number_parameters     100
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0563
_refine_ls_wR_factor_ref         0.1636
_refine_ls_wR_factor_gt          0.1583
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.5000 0.5000 0.5000 0.0182(2) Uani 1 2 d S . P . .
S1 S 0.33527(19) 0.29465(18) 0.34539(10) 0.0208(3) Uani 1 1 d . . . . .
S2 S 0.74969(19) 0.26455(18) 0.48966(10) 0.0216(3) Uani 1 1 d . . . . .
O1 O 0.5928(6) 0.0181(5) 0.3130(3) 0.0220(7) Uani 1 1 d . . . . .
C1 C 0.5667(8) 0.1700(7) 0.3749(4) 0.0179(9) Uani 1 1 d . . . . .
C2 C 0.7911(8) -0.0887(7) 0.3482(4) 0.0194(9) Uani 1 1 d . . . . .
H2A H 0.8078 -0.1168 0.4304 0.023 Uiso 1 1 calc R U . . .
H2B H 0.9253 -0.0054 0.3338 0.023 Uiso 1 1 calc R U . . .
C3 C 0.7643(8) -0.2834(7) 0.2803(4) 0.0209(9) Uani 1 1 d . . . . .
H3A H 0.6070 -0.3379 0.2725 0.025 Uiso 1 1 calc R U . . .
H3B H 0.8535 -0.3795 0.3257 0.025 Uiso 1 1 calc R U . . .
C4 C 0.8292(8) -0.2777(7) 0.1605(4) 0.0216(9) Uani 1 1 d . . . . .
C5 C 1.0760(9) -0.2133(9) 0.1679(5) 0.0310(11) Uani 1 1 d . . . . .
H5A H 1.1177 -0.2235 0.0924 0.046 Uiso 1 1 calc R U . . .
H5B H 1.1617 -0.3005 0.2202 0.046 Uiso 1 1 calc R U . . .
H5C H 1.1073 -0.0747 0.1957 0.046 Uiso 1 1 calc R U . . .
C6 C 0.7785(9) -0.4908(8) 0.1118(5) 0.0309(11) Uani 1 1 d . . . . .
H6A H 0.8054 -0.4924 0.0331 0.046 Uiso 1 1 calc R U . . .
H6B H 0.6229 -0.5368 0.1138 0.046 Uiso 1 1 calc R U . . .
H6C H 0.8746 -0.5796 0.1572 0.046 Uiso 1 1 calc R U . . .
C7 C 0.6944(9) -0.1344(8) 0.0843(4) 0.0282(11) Uani 1 1 d . . . . .
H7A H 0.7350 -0.1360 0.0083 0.042 Uiso 1 1 calc R U . . .
H7B H 0.7260 0.0014 0.1167 0.042 Uiso 1 1 calc R U . . .
H7C H 0.5358 -0.1767 0.0792 0.042 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 0.0125(3) 0.0189(3) 0.0241(3) 0.00017(19) 0.0039(2) 0.0040(2)
S1 0.0129(6) 0.0239(6) 0.0256(6) -0.0005(5) 0.0014(4) 0.0051(5)
S2 0.0147(6) 0.0241(6) 0.0256(6) -0.0032(4) -0.0006(4) 0.0068(5)
O1 0.0145(16) 0.0251(18) 0.0265(17) 0.0008(13) 0.0005(13) 0.0080(14)
C1 0.013(2) 0.018(2) 0.023(2) 0.0041(16) 0.0039(17) 0.0023(17)
C2 0.014(2) 0.021(2) 0.025(2) -0.0012(17) 0.0049(17) 0.0076(17)
C3 0.015(2) 0.022(2) 0.027(2) 0.0015(17) 0.0068(17) 0.0051(18)
C4 0.015(2) 0.026(2) 0.024(2) -0.0016(17) 0.0044(17) 0.0031(18)
C5 0.018(2) 0.042(3) 0.034(3) -0.006(2) 0.010(2) 0.001(2)
C6 0.024(3) 0.032(3) 0.036(3) -0.009(2) 0.007(2) 0.000(2)
C7 0.027(3) 0.034(3) 0.025(2) 0.0030(19) 0.006(2) 0.008(2)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd S2 2.3201(12) 2_666 ?
Pd S2 2.3202(12) . ?
Pd S1 2.3368(12) . ?
Pd S1 2.3368(12) 2_666 ?
S1 C1 1.704(5) . ?
S2 C1 1.705(5) . ?
O1 C1 1.296(6) . ?
O1 C2 1.473(6) . ?
C2 C3 1.520(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.545(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.525(7) . ?
C4 C6 1.530(7) . ?
C4 C7 1.531(7) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?

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
_geom_angle_publ_flag
S2 Pd S2 180.0 2_666 . ?
S2 Pd S1 104.40(4) 2_666 . ?
S2 Pd S1 75.60(4) . . ?
S2 Pd S1 75.60(4) 2_666 2_666 ?
S2 Pd S1 104.40(4) . 2_666 ?
S1 Pd S1 180.0 . 2_666 ?
C1 S1 Pd 85.08(17) . . ?
C1 S2 Pd 85.59(17) . . ?
C1 O1 C2 117.5(4) . . ?
O1 C1 S1 120.8(4) . . ?
O1 C1 S2 125.4(4) . . ?
S1 C1 S2 113.7(3) . . ?
O1 C2 C3 108.5(4) . . ?
O1 C2 H2A 110.0 . . ?
C3 C2 H2A 110.0 . . ?
O1 C2 H2B 110.0 . . ?
C3 C2 H2B 110.0 . . ?
H2A C2 H2B 108.4 . . ?
C2 C3 C4 118.1(4) . . ?
C2 C3 H3A 107.8 . . ?
C4 C3 H3A 107.8 . . ?
C2 C3 H3B 107.8 . . ?
C4 C3 H3B 107.8 . . ?
H3A C3 H3B 107.1 . . ?
C5 C4 C6 109.5(4) . . ?
C5 C4 C7 109.6(4) . . ?
C6 C4 C7 109.9(4) . . ?
C5 C4 C3 110.4(4) . . ?
C6 C4 C3 106.5(4) . . ?
C7 C4 C3 110.8(4) . . ?
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 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 O1 C1 S1 -176.5(3) . . . . ?
C2 O1 C1 S2 3.5(6) . . . . ?
Pd S1 C1 O1 -178.9(4) . . . . ?
Pd S1 C1 S2 1.1(2) . . . . ?
Pd S2 C1 O1 178.9(4) . . . . ?
Pd S2 C1 S1 -1.1(2) . . . . ?
C1 O1 C2 C3 168.2(4) . . . . ?
O1 C2 C3 C4 83.9(5) . . . . ?
C2 C3 C4 C5 63.0(6) . . . . ?
C2 C3 C4 C6 -178.3(4) . . . . ?
C2 C3 C4 C7 -58.7(6) . . . . ?

_refine_diff_density_max         4.367
_refine_diff_density_min         -2.032
_refine_diff_density_rms         0.222

_shelx_res_file                  
;

    shelx.res created by SHELXL-2014/7

TITL  9
CELL  1.54184 6.1398 6.7176 11.9393 90.020 99.397 95.377
ZERR  1       0.0006 0.0005  0.0010  0.007  0.007  0.007
LATT  1
SFAC  C  H  O  S  Pd
UNIT  14 26 2 4 1
L.S.  24
ACTA  150.0
OMIT  -3 150.0
BOND  $H
FMAP  2
PLAN -1
CONF
SIZE  0.05 0.1 0.2
TEMP -173
WGHT    0.129700    0.374600
FVAR       7.81820
PD    5    0.500000    0.500000    0.500000    10.50000    0.01253    0.01891 =
         0.02405    0.00017    0.00388    0.00399
S1    4    0.335274    0.294649    0.345387    11.00000    0.01286    0.02387 =
         0.02563   -0.00046    0.00142    0.00510
S2    4    0.749688    0.264549    0.489659    11.00000    0.01472    0.02410 =
         0.02558   -0.00320   -0.00062    0.00680
O1    3    0.592849    0.018140    0.313047    11.00000    0.01454    0.02515 =
         0.02647    0.00076    0.00053    0.00796
C1    1    0.566720    0.169991    0.374884    11.00000    0.01250    0.01842 =
         0.02340    0.00414    0.00391    0.00229
C2    1    0.791113   -0.088674    0.348160    11.00000    0.01378    0.02070 =
         0.02543   -0.00117    0.00492    0.00761
AFIX  23
H2A   2    0.807850   -0.116812    0.430352    11.00000   -1.20000
H2B   2    0.925266   -0.005420    0.333849    11.00000   -1.20000
AFIX   0
C3    1    0.764311   -0.283386    0.280308    11.00000    0.01533    0.02228 =
         0.02697    0.00152    0.00676    0.00507
AFIX  23
H3A   2    0.606991   -0.337925    0.272466    11.00000   -1.20000
H3B   2    0.853482   -0.379507    0.325710    11.00000   -1.20000
AFIX   0
C4    1    0.829182   -0.277714    0.160539    11.00000    0.01454    0.02648 =
         0.02436   -0.00162    0.00436    0.00309
C5    1    1.076024   -0.213334    0.167862    11.00000    0.01819    0.04179 =
         0.03438   -0.00631    0.00959    0.00092
AFIX 137
H5A   2    1.117691   -0.223514    0.092399    11.00000   -1.50000
H5B   2    1.161680   -0.300454    0.220217    11.00000   -1.50000
H5C   2    1.107333   -0.074661    0.195678    11.00000   -1.50000
AFIX   0
C6    1    0.778487   -0.490760    0.111794    11.00000    0.02439    0.03225 =
         0.03614   -0.00875    0.00656   -0.00007
AFIX 137
H6A   2    0.805407   -0.492351    0.033135    11.00000   -1.50000
H6B   2    0.622944   -0.536840    0.113779    11.00000   -1.50000
H6C   2    0.874636   -0.579560    0.157243    11.00000   -1.50000
AFIX   0
C7    1    0.694351   -0.134383    0.084310    11.00000    0.02651    0.03421 =
         0.02546    0.00303    0.00607    0.00839
AFIX 137
H7A   2    0.734957   -0.136044    0.008293    11.00000   -1.50000
H7B   2    0.725955    0.001354    0.116661    11.00000   -1.50000
H7C   2    0.535848   -0.176727    0.079188    11.00000   -1.50000

AFIX   0
HKLF  4 1 1 0 0 0 -1 0 0 0 -1

REM   9
REM R1 =  0.0563 for    1861 Fo > 4sig(Fo)  and  0.0590 for all    1979 data
REM    100 parameters refined using      0 restraints

END

WGHT      0.1280      0.4388

REM Highest difference peak  4.367,  deepest hole -2.032,  1-sigma level  0.222
Q1    1   0.4605  0.4866  0.4192  11.00000  0.05    4.37
;
_shelx_res_checksum              3478
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1058653'
_audit_update_record             
;
2015-04-09 deposited with the CCDC.
2016-01-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H22 O2 Pd S4'
_chemical_formula_sum            'C12 H22 O2 Pd S4'
_chemical_formula_weight         432.93

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.8820(11)
_cell_length_b                   7.3531(12)
_cell_length_c                   10.0455(10)
_cell_angle_alpha                70.305(12)
_cell_angle_beta                 70.788(12)
_cell_angle_gamma                67.164(15)
_cell_volume                     429.42(12)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1518
_cell_measurement_theta_min      6.7249
_cell_measurement_theta_max      75.9784

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_F_000             220
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    13.223
_shelx_estimated_absorpt_T_min   0.177
_shelx_estimated_absorpt_T_max   0.558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.50803
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'CrysAlis PRO (Agilent, 2011)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  Mirror
_diffrn_measurement_device_type  
'Agilent Technologies SuperNova Dual diffractometer with Atlas detector'
_diffrn_detector_area_resol_mean 10.4041
_diffrn_measurement_method       'ω scan'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            3253
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         6.730
_diffrn_reflns_theta_max         74.954
_diffrn_reflns_theta_full        74.954
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             1748
_reflns_number_gt                1619
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlis PRO (Agilent, 2012)'
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2012)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2012)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg, 2006)
;
_computing_publication_material  'SHELXL (Sheldrick, 2015)'

_refine_special_details          
;
The maximum and minimum residual electron density peaks of 
1.30 and 3.02 eÅ⁻³, respectively, were located 0.89 Å and 0.85 Å
from the Pd atom.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1188P)²+0.8512P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1748
_refine_ls_number_parameters     89
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0543
_refine_ls_wR_factor_ref         0.1659
_refine_ls_wR_factor_gt          0.1584
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.093
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.5000 0.5000 0.5000 0.0232(3) Uani 1 2 d S . P . .
S1 S 0.6680(2) 0.3824(2) 0.28860(14) 0.0264(4) Uani 1 1 d . . . . .
S2 S 0.2929(2) 0.3108(2) 0.50165(14) 0.0246(3) Uani 1 1 d . . . . .
O1 O 0.4583(7) 0.1760(6) 0.2591(4) 0.0268(9) Uani 1 1 d . . . . .
C1 C 0.4676(10) 0.2765(9) 0.3412(6) 0.0263(11) Uani 1 1 d . . . . .
C2 C 0.2867(10) 0.0818(9) 0.3050(6) 0.0277(12) Uani 1 1 d . . . . .
H2A H 0.1423 0.1856 0.3178 0.033 Uiso 1 1 calc R U . . .
H2B H 0.2976 -0.0217 0.3979 0.033 Uiso 1 1 calc R U . . .
C3 C 0.3204(10) -0.0158(9) 0.1852(6) 0.0280(12) Uani 1 1 d . . . . .
H3A H 0.4679 -0.1145 0.1715 0.034 Uiso 1 1 calc R U . . .
H3B H 0.3101 0.0903 0.0933 0.034 Uiso 1 1 calc R U . . .
C4 C 0.1563(10) -0.1246(9) 0.2170(6) 0.0275(12) Uani 1 1 d . . . . .
H4A H 0.0093 -0.0246 0.2258 0.033 Uiso 1 1 calc R U . . .
H4B H 0.1615 -0.2260 0.3113 0.033 Uiso 1 1 calc R U . . .
C5 C 0.1972(10) -0.2318(9) 0.0997(6) 0.0285(12) Uani 1 1 d . . . . .
H5A H 0.1902 -0.1297 0.0058 0.034 Uiso 1 1 calc R U . . .
H5B H 0.3453 -0.3297 0.0900 0.034 Uiso 1 1 calc R U . . .
C6 C 0.0379(11) -0.3440(10) 0.1299(7) 0.0338(13) Uani 1 1 d . . . . .
H6A H 0.0675 -0.4016 0.0477 0.051 Uiso 1 1 calc R U . . .
H6B H -0.1099 -0.2494 0.1435 0.051 Uiso 1 1 calc R U . . .
H6C H 0.0528 -0.4538 0.2181 0.051 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 0.0321(4) 0.0234(4) 0.0208(3) -0.0051(2) -0.0065(2) -0.0153(2)
S1 0.0332(7) 0.0305(7) 0.0238(7) -0.0086(5) -0.0029(5) -0.0198(6)
S2 0.0323(7) 0.0270(7) 0.0210(6) -0.0068(5) -0.0035(5) -0.0174(6)
O1 0.036(2) 0.032(2) 0.0231(18) -0.0080(16) -0.0028(16) -0.0236(18)
C1 0.035(3) 0.025(3) 0.023(2) -0.006(2) -0.007(2) -0.014(2)
C2 0.040(3) 0.026(3) 0.029(3) -0.004(2) -0.010(2) -0.023(2)
C3 0.038(3) 0.027(3) 0.025(3) -0.006(2) -0.005(2) -0.019(2)
C4 0.039(3) 0.032(3) 0.019(2) -0.007(2) -0.005(2) -0.021(2)
C5 0.039(3) 0.031(3) 0.025(3) -0.008(2) -0.006(2) -0.020(3)
C6 0.048(4) 0.036(3) 0.030(3) -0.009(2) -0.009(3) -0.025(3)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd S1 2.3322(13) . ?
Pd S1 2.3323(14) 2_666 ?
Pd S2 2.3397(13) . ?
Pd S2 2.3397(13) 2_666 ?
S1 C1 1.693(6) . ?
S2 C1 1.694(6) . ?
O1 C1 1.309(7) . ?
O1 C2 1.466(6) . ?
C2 C3 1.512(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.519(7) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.525(7) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.513(8) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?

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
_geom_angle_publ_flag
S1 Pd S1 180.0 . 2_666 ?
S1 Pd S2 75.50(5) . . ?
S1 Pd S2 104.50(5) 2_666 . ?
S1 Pd S2 104.50(5) . 2_666 ?
S1 Pd S2 75.50(5) 2_666 2_666 ?
S2 Pd S2 180.0 . 2_666 ?
C1 S1 Pd 84.7(2) . . ?
C1 S2 Pd 84.5(2) . . ?
C1 O1 C2 119.8(4) . . ?
O1 C1 S1 119.5(4) . . ?
O1 C1 S2 125.2(4) . . ?
S1 C1 S2 115.2(3) . . ?
O1 C2 C3 105.9(4) . . ?
O1 C2 H2A 110.6 . . ?
C3 C2 H2A 110.6 . . ?
O1 C2 H2B 110.6 . . ?
C3 C2 H2B 110.6 . . ?
H2A C2 H2B 108.7 . . ?
C2 C3 C4 112.7(5) . . ?
C2 C3 H3A 109.0 . . ?
C4 C3 H3A 109.0 . . ?
C2 C3 H3B 109.0 . . ?
C4 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
C3 C4 C5 112.7(5) . . ?
C3 C4 H4A 109.0 . . ?
C5 C4 H4A 109.0 . . ?
C3 C4 H4B 109.0 . . ?
C5 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
C6 C5 C4 113.8(5) . . ?
C6 C5 H5A 108.8 . . ?
C4 C5 H5A 108.8 . . ?
C6 C5 H5B 108.8 . . ?
C4 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 O1 C1 S1 179.3(4) . . . . ?
C2 O1 C1 S2 -0.3(8) . . . . ?
Pd S1 C1 O1 178.4(5) . . . . ?
Pd S1 C1 S2 -2.0(3) . . . . ?
Pd S2 C1 O1 -178.4(5) . . . . ?
Pd S2 C1 S1 2.0(3) . . . . ?
C1 O1 C2 C3 178.7(5) . . . . ?
O1 C2 C3 C4 179.0(5) . . . . ?
C2 C3 C4 C5 -177.2(5) . . . . ?
C3 C4 C5 C6 179.1(5) . . . . ?

_refine_diff_density_max         1.300
_refine_diff_density_min         -3.025
_refine_diff_density_rms         0.198

_shelx_res_file                  
;

    shelx.res created by SHELXL-2014/7

TITL  7
CELL  1.54184 6.8820 7.3531 10.0455 70.305 70.788 67.164
ZERR  1       0.0011 0.0012  0.0010  0.012  0.012  0.015
LATT  1
SFAC  C H O S Pd
UNIT  12 22 2 4 1
ACTA  150
OMIT  -3 150
TEMP -173
SIZE  0.20 0.10 0.05
FMAP  2
PLAN -1
BOND  $H
CONF
L.S.  24
WGHT    0.118800    0.851200
FVAR       6.53561
PD    5    0.500000    0.500000    0.500000    10.50000    0.03215    0.02339 =
         0.02077   -0.00506   -0.00652   -0.01530
S1    4    0.668039    0.382447    0.288601    11.00000    0.03325    0.03045 =
         0.02382   -0.00862   -0.00290   -0.01978
S2    4    0.292942    0.310785    0.501648    11.00000    0.03234    0.02700 =
         0.02102   -0.00677   -0.00347   -0.01735
O1    3    0.458312    0.175967    0.259104    11.00000    0.03587    0.03203 =
         0.02309   -0.00801   -0.00278   -0.02362
C1    1    0.467629    0.276501    0.341164    11.00000    0.03453    0.02536 =
         0.02340   -0.00575   -0.00676   -0.01383
C2    1    0.286662    0.081784    0.304952    11.00000    0.03978    0.02613 =
         0.02911   -0.00429   -0.01023   -0.02262
AFIX  23
H2A   2    0.142259    0.185595    0.317781    11.00000   -1.20000
H2B   2    0.297559   -0.021713    0.397947    11.00000   -1.20000
AFIX   0
C3    1    0.320391   -0.015845    0.185178    11.00000    0.03794    0.02741 =
         0.02522   -0.00577   -0.00481   -0.01934
AFIX  23
H3A   2    0.467948   -0.114542    0.171528    11.00000   -1.20000
H3B   2    0.310084    0.090254    0.093317    11.00000   -1.20000
AFIX   0
C4    1    0.156336   -0.124608    0.217014    11.00000    0.03950    0.03172 =
         0.01945   -0.00667   -0.00480   -0.02061
AFIX  23
H4A   2    0.009285   -0.024588    0.225758    11.00000   -1.20000
H4B   2    0.161501   -0.225997    0.311321    11.00000   -1.20000
AFIX   0
C5    1    0.197154   -0.231784    0.099735    11.00000    0.03901    0.03055 =
         0.02537   -0.00822   -0.00642   -0.01997
AFIX  23
H5A   2    0.190192   -0.129684    0.005841    11.00000   -1.20000
H5B   2    0.345344   -0.329735    0.089998    11.00000   -1.20000
AFIX   0
C6    1    0.037885   -0.344014    0.129940    11.00000    0.04795    0.03602 =
         0.02994   -0.00896   -0.00851   -0.02542
AFIX 137
H6A   2    0.067537   -0.401556    0.047722    11.00000   -1.50000
H6B   2   -0.109895   -0.249405    0.143536    11.00000   -1.50000
H6C   2    0.052844   -0.453779    0.218126    11.00000   -1.50000

AFIX   0
HKLF  4

REM   7
REM R1 =  0.0543 for    1619 Fo > 4sig(Fo)  and  0.0580 for all    1748 data
REM     89 parameters refined using      0 restraints

END

WGHT      0.1131      1.0186

REM Highest difference peak  1.300,  deepest hole -3.025,  1-sigma level  0.198
Q1    1   0.3872  0.4984  0.5762  11.00000  0.05    1.30
;
_shelx_res_checksum              61956
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1058654'
_audit_update_record             
;
2015-04-09 deposited with the CCDC.
2016-01-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H22 O2 Pd S4'
_chemical_formula_sum            'C12 H22 O2 Pd S4'
_chemical_formula_weight         432.93

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.5622(4)
_cell_length_b                   6.8643(5)
_cell_length_c                   9.8385(7)
_cell_angle_alpha                84.811(6)
_cell_angle_beta                 76.424(6)
_cell_angle_gamma                83.388(6)
_cell_volume                     427.00(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3284
_cell_measurement_theta_min      2.9879
_cell_measurement_theta_max      27.4917

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_F_000             220
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.570
_shelx_estimated_absorpt_T_min   0.572
_shelx_estimated_absorpt_T_max   0.859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.73672
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'CrysAlis PRO (Agilent, 2011)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  Mirror
_diffrn_measurement_device_type  
'Agilent Technologies SuperNova Dual diffractometer with Atlas detector'
_diffrn_detector_area_resol_mean 10.4041
_diffrn_measurement_method       'ω scan'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            6326
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.994
_diffrn_reflns_theta_max         27.489
_diffrn_reflns_theta_full        27.489
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1955
_reflns_number_gt                1812
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlis PRO (Agilent, 2012)'
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2012)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2012)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg, 2006)
;
_computing_publication_material  'SHELXL (Sheldrick, 2015)'

_refine_special_details          
;
The maximum and minimum residual electron density peaks of 
1.18 and 1.23 eÅ⁻³, respectively, were located 0.96 Å and 0.87 Å
from the atom.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0462P)²+0.0800P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1955
_refine_ls_number_parameters     90
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0294
_refine_ls_wR_factor_ref         0.0829
_refine_ls_wR_factor_gt          0.0781
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_restrained_S_all      1.129
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.5000 0.5000 0.5000 0.01657(12) Uani 1 2 d S . P . .
S1 S 0.29735(10) 0.69266(9) 0.67578(7) 0.01969(16) Uani 1 1 d . . . . .
S2 S 0.72059(10) 0.73217(9) 0.52350(7) 0.01966(16) Uani 1 1 d . . . . .
O1 O 0.5198(3) 0.9493(3) 0.7370(2) 0.0201(4) Uani 1 1 d . . . . .
C1 C 0.5180(4) 0.8119(4) 0.6545(3) 0.0181(5) Uani 1 1 d . . . . .
C2 C 0.7126(4) 1.0488(4) 0.7160(3) 0.0199(5) Uani 1 1 d . . . . .
H2A H 0.7505 1.1087 0.6192 0.024 Uiso 1 1 calc R U . . .
H2B H 0.8314 0.9543 0.7327 0.024 Uiso 1 1 calc R U . . .
C3 C 0.6644(4) 1.2063(4) 0.8210(3) 0.0198(5) Uani 1 1 d . . . . .
H3A H 0.6322 1.1430 0.9170 0.024 Uiso 1 1 calc R U . . .
H3B H 0.5380 1.2925 0.8076 0.024 Uiso 1 1 calc R U . . .
C4 C 0.8481(4) 1.3317(4) 0.8058(3) 0.0179(5) Uani 1 1 d . . . . .
H4A H 0.8892 1.3825 0.7057 0.022 Uiso 1 1 calc R U . . .
C5 C 0.7793(4) 1.5080(4) 0.8966(3) 0.0196(5) Uani 1 1 d . . . . .
H5A H 0.6587 1.5857 0.8693 0.029 Uiso 1 1 calc R U . . .
H5B H 0.8962 1.5899 0.8834 0.029 Uiso 1 1 calc R U . . .
H5C H 0.7389 1.4611 0.9954 0.029 Uiso 1 1 calc R U . . .
C6 C 1.0403(4) 1.2122(4) 0.8445(3) 0.0220(5) Uani 1 1 d . . . . .
H6A H 1.1559 1.2958 0.8301 0.033 Uiso 1 1 calc R U . . .
H6B H 1.0842 1.1007 0.7852 0.033 Uiso 1 1 calc R U . . .
H6C H 1.0040 1.1634 0.9431 0.033 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 0.01281(16) 0.01684(17) 0.02051(17) -0.00334(11) -0.00355(11) -0.00214(11)
S1 0.0123(3) 0.0211(3) 0.0259(4) -0.0062(3) -0.0022(3) -0.0035(2)
S2 0.0141(3) 0.0209(3) 0.0233(3) -0.0057(3) -0.0004(3) -0.0038(2)
O1 0.0111(9) 0.0222(9) 0.0280(10) -0.0067(7) -0.0036(8) -0.0035(7)
C1 0.0141(12) 0.0180(12) 0.0236(13) -0.0008(10) -0.0072(10) -0.0007(9)
C2 0.0090(11) 0.0225(13) 0.0298(14) -0.0065(10) -0.0042(10) -0.0046(9)
C3 0.0102(11) 0.0225(13) 0.0281(14) -0.0066(10) -0.0053(10) -0.0008(9)
C4 0.0093(11) 0.0221(13) 0.0214(13) -0.0031(10) -0.0013(10) -0.0002(9)
C5 0.0106(12) 0.0217(13) 0.0262(14) -0.0057(10) -0.0025(10) -0.0012(9)
C6 0.0120(12) 0.0230(13) 0.0322(15) -0.0037(11) -0.0075(11) 0.0003(10)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd S1 2.3318(7) 2_666 ?
Pd S1 2.3318(7) . ?
Pd S2 2.3332(6) 2_666 ?
Pd S2 2.3332(6) . ?
S1 C1 1.706(3) . ?
S2 C1 1.698(3) . ?
O1 C1 1.302(3) . ?
O1 C2 1.470(3) . ?
C2 C3 1.518(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.532(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C6 1.530(3) . ?
C4 C5 1.532(3) . ?
C4 H4A 1.0000 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?

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
_geom_angle_publ_flag
S1 Pd S1 180.0 2_666 . ?
S1 Pd S2 75.62(2) 2_666 2_666 ?
S1 Pd S2 104.38(2) . 2_666 ?
S1 Pd S2 104.38(2) 2_666 . ?
S1 Pd S2 75.62(2) . . ?
S2 Pd S2 180.0 2_666 . ?
C1 S1 Pd 84.89(9) . . ?
C1 S2 Pd 85.02(9) . . ?
C1 O1 C2 118.1(2) . . ?
O1 C1 S2 126.2(2) . . ?
O1 C1 S1 119.5(2) . . ?
S2 C1 S1 114.32(15) . . ?
O1 C2 C3 106.2(2) . . ?
O1 C2 H2A 110.5 . . ?
C3 C2 H2A 110.5 . . ?
O1 C2 H2B 110.5 . . ?
C3 C2 H2B 110.5 . . ?
H2A C2 H2B 108.7 . . ?
C2 C3 C4 112.3(2) . . ?
C2 C3 H3A 109.1 . . ?
C4 C3 H3A 109.1 . . ?
C2 C3 H3B 109.1 . . ?
C4 C3 H3B 109.1 . . ?
H3A C3 H3B 107.9 . . ?
C6 C4 C3 111.9(2) . . ?
C6 C4 C5 110.1(2) . . ?
C3 C4 C5 110.2(2) . . ?
C6 C4 H4A 108.2 . . ?
C3 C4 H4A 108.2 . . ?
C5 C4 H4A 108.2 . . ?
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 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 O1 C1 S2 0.8(3) . . . . ?
C2 O1 C1 S1 179.85(17) . . . . ?
Pd S2 C1 O1 175.5(2) . . . . ?
Pd S2 C1 S1 -3.62(12) . . . . ?
Pd S1 C1 O1 -175.6(2) . . . . ?
Pd S1 C1 S2 3.62(12) . . . . ?
C1 O1 C2 C3 177.2(2) . . . . ?
O1 C2 C3 C4 -176.61(19) . . . . ?
C2 C3 C4 C6 -66.5(3) . . . . ?
C2 C3 C4 C5 170.8(2) . . . . ?

_refine_diff_density_max         1.184
_refine_diff_density_min         -1.227
_refine_diff_density_rms         0.126

_shelx_res_file                  
;

    shelx.res created by SHELXL-2014/7

TITL  8
CELL  0.71073 6.5622 6.8643 9.8385 84.811 76.424 83.388
ZERR  1       0.0004 0.0005 0.0007  0.006  0.006  0.006
LATT  1
SFAC  C H O S Pd
UNIT  12 22 2 4 1
ACTA  55.0
OMIT  -3 55.0
TEMP -173
SIZE  0.4 0.2 0.1
L.S.  24
BOND  $H
CONF
FMAP  2
PLAN -1
WGHT    0.046200    0.080000
FVAR       7.86847
PD    5    0.500000    0.500000    0.500000    10.50000    0.01281    0.01684 =
         0.02051   -0.00334   -0.00355   -0.00214
S1    4    0.297349    0.692665    0.675776    11.00000    0.01232    0.02108 =
         0.02592   -0.00623   -0.00215   -0.00353
S2    4    0.720592    0.732172    0.523495    11.00000    0.01412    0.02090 =
         0.02332   -0.00569   -0.00035   -0.00380
O1    3    0.519752    0.949339    0.737026    11.00000    0.01113    0.02217 =
         0.02802   -0.00667   -0.00356   -0.00345
C1    1    0.518003    0.811911    0.654465    11.00000    0.01407    0.01796 =
         0.02356   -0.00075   -0.00718   -0.00074
C2    1    0.712623    1.048811    0.716040    11.00000    0.00896    0.02248 =
         0.02979   -0.00650   -0.00418   -0.00461
AFIX  23
H2A   2    0.750477    1.108673    0.619187    11.00000   -1.20000
H2B   2    0.831418    0.954254    0.732701    11.00000   -1.20000
AFIX   0
C3    1    0.664443    1.206287    0.820973    11.00000    0.01016    0.02248 =
         0.02809   -0.00664   -0.00532   -0.00078
AFIX  23
H3A   2    0.632195    1.142963    0.917045    11.00000   -1.20000
H3B   2    0.538007    1.292520    0.807610    11.00000   -1.20000
AFIX   0
C4    1    0.848073    1.331659    0.805806    11.00000    0.00928    0.02205 =
         0.02139   -0.00314   -0.00132   -0.00020
AFIX  13
H4A   2    0.889243    1.382525    0.705672    11.00000   -1.20000
AFIX   0
C5    1    0.779258    1.507971    0.896647    11.00000    0.01061    0.02169 =
         0.02622   -0.00569   -0.00251   -0.00122
AFIX 137
H5A   2    0.658678    1.585717    0.869255    11.00000   -1.50000
H5B   2    0.896160    1.589851    0.883355    11.00000   -1.50000
H5C   2    0.738923    1.461110    0.995432    11.00000   -1.50000
AFIX   0
C6    1    1.040285    1.212165    0.844520    11.00000    0.01200    0.02300 =
         0.03225   -0.00368   -0.00751    0.00033
AFIX 137
H6A   2    1.155869    1.295834    0.830132    11.00000   -1.50000
H6B   2    1.084163    1.100723    0.785151    11.00000   -1.50000
H6C   2    1.003971    1.163379    0.943081    11.00000   -1.50000

AFIX   0
HKLF      4

REM   8
REM R1 =  0.0294 for    1812 Fo > 4sig(Fo)  and  0.0327 for all    1955 data
REM     90 parameters refined using      0 restraints

END

WGHT      0.0459      0.0852

REM Highest difference peak  1.184,  deepest hole -1.227,  1-sigma level  0.126
Q1    1   0.4741  0.5146  0.5994  11.00000  0.05    1.18
;
_shelx_res_checksum              37904
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1058655'
_audit_update_record             
;
2015-04-09 deposited with the CCDC.
2016-01-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H22 O2 Pd S4'
_chemical_formula_sum            'C12 H22 O2 Pd S4'
_chemical_formula_weight         432.93

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.2746(3)
_cell_length_b                   6.3302(4)
_cell_length_c                   11.4138(6)
_cell_angle_alpha                79.690(5)
_cell_angle_beta                 88.152(4)
_cell_angle_gamma                86.065(5)
_cell_volume                     444.89(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1761
_cell_measurement_theta_min      3.6310
_cell_measurement_theta_max      27.5120

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_F_000             220
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.507
_shelx_estimated_absorpt_T_min   0.584
_shelx_estimated_absorpt_T_max   0.753
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.611
_exptl_absorpt_correction_T_max  0.832
_exptl_absorpt_process_details   'CrysAlis PRO (Agilent, 2012)'

_exptl_special_details           
;
;

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1 0 -16 0.0649 -0.9661 -0.0242 -16.0403 0.5554 0.5273 0.6684
1 5 15 0.1409 0.9797 5.0093 15.0167 -0.8644 -0.0507 -0.5336
6 6 7 0.1857 5.9944 5.9986 6.9979 -0.9397 -0.0470 0.2477
1 0 16 0.0863 0.9661 0.0242 16.0403 -0.5554 -0.5273 -0.6684
1 -2 15 0.1180 1.2675 -1.7599 14.7997 -0.4103 -0.6705 -0.6181
7 0 -10 0.1055 7.0149 -0.0094 -10.0174 -0.0480 -0.1550 1.0132
9 0 -1 0.1334 8.9947 0.0053 -0.9932 -0.4349 -0.5430 0.7495
6 -6 3 0.2011 6.0273 -5.5730 2.9988 -0.0257 -0.9715 0.2357
0 -5 11 0.1423 -0.0342 -4.9704 11.0482 -0.0058 -0.7665 -0.6014
-6 -1 11 0.1033 -6.0201 -0.9857 11.0251 0.0327 -0.0271 -0.9994
0 9 1 0.1779 0.0186 8.9773 0.9643 -0.6442 0.7768 0.1120
0 -9 1 0.2137 -0.0228 -8.9743 1.0406 0.5813 -0.8347 -0.2053
1 0 16 0.0884 0.9661 0.0242 16.0403 -0.5554 -0.5273 -0.6684

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  Mirror
_diffrn_measurement_device_type  
'Agilent Technologies SuperNova Dual diffractometer with Atlas detector'
_diffrn_detector_area_resol_mean 10.4041
_diffrn_measurement_method       'ω scan'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            3533
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.255
_diffrn_reflns_theta_max         27.489
_diffrn_reflns_theta_full        27.489
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2037
_reflns_number_gt                1872
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlis PRO (Agilent, 2012)'
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2012)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2012)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg, 2006)
;
_computing_publication_material  'SHELXL (Sheldrick, 2015)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0180P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2037
_refine_ls_number_parameters     91
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0234
_refine_ls_wR_factor_ref         0.0492
_refine_ls_wR_factor_gt          0.0472
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.5000 0.5000 0.5000 0.01293(8) Uani 1 2 d S . P . .
S1 S 0.25656(8) 0.68134(8) 0.36237(5) 0.01765(12) Uani 1 1 d . . . . .
S2 S 0.28730(8) 0.23407(8) 0.46139(5) 0.01595(12) Uani 1 1 d . . . . .
O1 O -0.0126(2) 0.4244(2) 0.30734(13) 0.0174(3) Uani 1 1 d . . . . .
C1 C 0.1542(3) 0.4380(3) 0.37015(18) 0.0136(4) Uani 1 1 d . . . . .
C2 C -0.1056(3) 0.2165(3) 0.31149(18) 0.0163(4) Uani 1 1 d . . . . .
H2A H -0.2313 0.2053 0.3665 0.020 Uiso 1 1 calc R U . . .
H2B H 0.0008 0.0976 0.3409 0.020 Uiso 1 1 calc R U . . .
C3 C -0.1727(3) 0.2004(3) 0.18613(18) 0.0149(4) Uani 1 1 d . . . . .
C4 C -0.3349(3) 0.3848(4) 0.1395(2) 0.0224(5) Uani 1 1 d . . . . .
H4A H -0.2685 0.5222 0.1333 0.034 Uiso 1 1 calc R U . . .
H4B H -0.4583 0.3822 0.1945 0.034 Uiso 1 1 calc R U . . .
H4C H -0.3821 0.3685 0.0608 0.034 Uiso 1 1 calc R U . . .
C5 C -0.2754(3) -0.0144(4) 0.1969(2) 0.0231(5) Uani 1 1 d . . . . .
H5A H -0.1718 -0.1319 0.2287 0.035 Uiso 1 1 calc R U . . .
H5B H -0.3200 -0.0334 0.1181 0.035 Uiso 1 1 calc R U . . .
H5C H -0.4004 -0.0156 0.2507 0.035 Uiso 1 1 calc R U . . .
C6 C 0.0256(3) 0.2055(4) 0.1039(2) 0.0263(5) Uani 1 1 d . . . . .
H6A H 0.1275 0.0857 0.1349 0.040 Uiso 1 1 calc R U . . .
H6B H 0.0925 0.3419 0.1006 0.040 Uiso 1 1 calc R U . . .
H6C H -0.0164 0.1920 0.0237 0.040 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 0.01161(12) 0.01070(12) 0.01623(13) -0.00130(9) -0.00169(8) -0.00102(8)
S1 0.0180(3) 0.0101(3) 0.0244(3) -0.0006(2) -0.0070(2) -0.0019(2)
S2 0.0166(3) 0.0116(3) 0.0189(3) 0.0007(2) -0.0044(2) -0.0020(2)
O1 0.0203(7) 0.0108(8) 0.0214(8) -0.0019(6) -0.0074(6) -0.0027(6)
C1 0.0142(10) 0.0131(11) 0.0134(10) -0.0030(8) 0.0028(8) 0.0007(8)
C2 0.0184(10) 0.0113(11) 0.0193(11) -0.0011(9) -0.0024(8) -0.0060(8)
C3 0.0176(10) 0.0122(11) 0.0149(11) -0.0018(9) -0.0018(8) -0.0010(8)
C4 0.0250(11) 0.0173(12) 0.0240(12) -0.0004(10) -0.0084(9) 0.0004(9)
C5 0.0284(12) 0.0169(12) 0.0245(12) -0.0020(10) -0.0076(10) -0.0063(10)
C6 0.0295(12) 0.0255(14) 0.0246(13) -0.0071(11) 0.0070(10) -0.0025(10)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd S1 2.3210(6) 2_666 ?
Pd S1 2.3211(6) . ?
Pd S2 2.3283(5) 2_666 ?
Pd S2 2.3283(5) . ?
S1 C1 1.696(2) . ?
S2 C1 1.696(2) . ?
O1 C1 1.304(2) . ?
O1 C2 1.468(2) . ?
C2 C3 1.527(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.527(3) . ?
C3 C5 1.528(3) . ?
C3 C6 1.533(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?

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
_geom_angle_publ_flag
S1 Pd S1 180.00(2) 2_666 . ?
S1 Pd S2 75.624(19) 2_666 2_666 ?
S1 Pd S2 104.376(19) . 2_666 ?
S1 Pd S2 104.376(19) 2_666 . ?
S1 Pd S2 75.624(19) . . ?
S2 Pd S2 180.0 2_666 . ?
C1 S1 Pd 85.10(7) . . ?
C1 S2 Pd 84.87(7) . . ?
C1 O1 C2 120.39(17) . . ?
O1 C1 S1 118.77(16) . . ?
O1 C1 S2 126.86(16) . . ?
S1 C1 S2 114.37(12) . . ?
O1 C2 C3 108.64(17) . . ?
O1 C2 H2A 110.0 . . ?
C3 C2 H2A 110.0 . . ?
O1 C2 H2B 110.0 . . ?
C3 C2 H2B 110.0 . . ?
H2A C2 H2B 108.3 . . ?
C4 C3 C2 110.31(16) . . ?
C4 C3 C5 109.81(17) . . ?
C2 C3 C5 106.25(17) . . ?
C4 C3 C6 110.56(19) . . ?
C2 C3 C6 109.21(17) . . ?
C5 C3 C6 110.62(16) . . ?
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 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 O1 C1 S1 179.87(12) . . . . ?
C2 O1 C1 S2 0.3(2) . . . . ?
Pd S1 C1 O1 178.59(14) . . . . ?
Pd S1 C1 S2 -1.81(9) . . . . ?
Pd S2 C1 O1 -178.64(16) . . . . ?
Pd S2 C1 S1 1.81(9) . . . . ?
C1 O1 C2 C3 -140.53(16) . . . . ?
O1 C2 C3 C4 -59.0(2) . . . . ?
O1 C2 C3 C5 -177.92(15) . . . . ?
O1 C2 C3 C6 62.7(2) . . . . ?

_refine_diff_density_max         0.696
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.090

_shelx_res_file                  
;

    shelx.res created by SHELXL-2014/7

TITL  9
CELL  0.71073 6.2746 6.3302 11.4138 79.690 88.152 86.065
ZERR  1       0.0003 0.0004  0.0006  0.005  0.004  0.005
LATT  1
SFAC  C H O S Pd
UNIT  12 22 2 4 1
ACTA  55.0
OMIT  -3 55.0
TEMP -173
SIZE  0.4 0.3 0.2
BOND  $H
CONF
FMAP  2
PLAN -1
L.S.  24
WGHT    0.018000
FVAR       8.51772
PD    5    0.500000    0.500000    0.500000    10.50000    0.01161    0.01070 =
         0.01623   -0.00130   -0.00169   -0.00102
S1    4    0.256563    0.681345    0.362367    11.00000    0.01804    0.01015 =
         0.02442   -0.00062   -0.00697   -0.00191
S2    4    0.287303    0.234066    0.461390    11.00000    0.01655    0.01155 =
         0.01890    0.00074   -0.00443   -0.00203
O1    3   -0.012649    0.424354    0.307341    11.00000    0.02032    0.01079 =
         0.02145   -0.00188   -0.00736   -0.00268
C1    1    0.154207    0.438012    0.370153    11.00000    0.01424    0.01310 =
         0.01338   -0.00298    0.00283    0.00066
C2    1   -0.105597    0.216531    0.311492    11.00000    0.01844    0.01131 =
         0.01927   -0.00113   -0.00236   -0.00603
AFIX  23
H2A   2   -0.231255    0.205267    0.366455    11.00000   -1.20000
H2B   2    0.000798    0.097607    0.340901    11.00000   -1.20000
AFIX   0
C3    1   -0.172701    0.200400    0.186125    11.00000    0.01755    0.01219 =
         0.01495   -0.00176   -0.00182   -0.00099
C4    1   -0.334927    0.384825    0.139488    11.00000    0.02497    0.01734 =
         0.02395   -0.00043   -0.00840    0.00045
AFIX 137
H4A   2   -0.268512    0.522177    0.133266    11.00000   -1.50000
H4B   2   -0.458286    0.382198    0.194505    11.00000   -1.50000
H4C   2   -0.382095    0.368457    0.060764    11.00000   -1.50000
AFIX   0
C5    1   -0.275446   -0.014379    0.196852    11.00000    0.02845    0.01691 =
         0.02451   -0.00201   -0.00755   -0.00627
AFIX 137
H5A   2   -0.171784   -0.131896    0.228656    11.00000   -1.50000
H5B   2   -0.320045   -0.033397    0.118097    11.00000   -1.50000
H5C   2   -0.400407   -0.015597    0.250682    11.00000   -1.50000
AFIX   0
C6    1    0.025614    0.205455    0.103905    11.00000    0.02952    0.02551 =
         0.02459   -0.00707    0.00697   -0.00246
AFIX 137
H6A   2    0.127521    0.085715    0.134856    11.00000   -1.50000
H6B   2    0.092469    0.341907    0.100550    11.00000   -1.50000
H6C   2   -0.016356    0.191974    0.023740    11.00000   -1.50000

AFIX   0
HKLF  4

REM   9
REM R1 =  0.0234 for    1872 Fo > 4sig(Fo)  and  0.0276 for all    2037 data
REM     91 parameters refined using      0 restraints

END

WGHT      0.0178      0.0000

REM Highest difference peak  0.696,  deepest hole -0.393,  1-sigma level  0.090
Q1    1   0.4233  0.5575  0.5553  11.00000  0.05    0.70
;
_shelx_res_checksum              29879
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1058656'
_audit_update_record             
;
2015-04-09 deposited with the CCDC.
2016-01-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H26 O2 Pd S4'
_chemical_formula_sum            'C14 H26 O2 Pd S4'
_chemical_formula_weight         460.99

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.8083(5)
_cell_length_b                   7.5446(4)
_cell_length_c                   10.4837(8)
_cell_angle_alpha                101.008(6)
_cell_angle_beta                 98.983(6)
_cell_angle_gamma                112.048(6)
_cell_volume                     474.33(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1935
_cell_measurement_theta_min      3.0216
_cell_measurement_theta_max      27.4997

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_F_000             236
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    1.419
_shelx_estimated_absorpt_T_min   0.676
_shelx_estimated_absorpt_T_max   0.959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6756
_exptl_absorpt_correction_T_max  0.9587
_exptl_absorpt_process_details   'CrysAlis PRO (Agilent, 2011)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  Mirror
_diffrn_measurement_device_type  
'Agilent Technologies SuperNova Dual diffractometer with Atlas detector'
_diffrn_detector_area_resol_mean 10.4041
_diffrn_measurement_method       'ω scan'
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            3938
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.028
_diffrn_reflns_theta_max         27.560
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2192
_reflns_number_gt                2006
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlis PRO (Agilent, 2012)'
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2012)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2012)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg, 2006)
;
_computing_publication_material  'SHELXL (Sheldrick, 2015)'

_refine_special_details          
;
The maximum and minimum residual electron density peaks of 
0.91 and 1.05 eÅ⁻³, respectively, were located 1.00 Å and 0.94 Å
from the Pd atom.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0231P)²+0.0817P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2192
_refine_ls_number_parameters     98
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0291
_refine_ls_wR_factor_ref         0.0678
_refine_ls_wR_factor_gt          0.0644
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.5000 0.0000 0.5000 0.01620(9) Uani 1 2 d S . P . .
S1 S 0.69147(9) 0.27275(9) 0.68632(6) 0.01994(14) Uani 1 1 d . . . . .
S2 S 0.29121(9) 0.18487(8) 0.50028(6) 0.01844(14) Uani 1 1 d . . . . .
O1 O 0.4830(3) 0.4981(2) 0.71669(17) 0.0190(4) Uani 1 1 d . . . . .
C1 C 0.4842(4) 0.3402(3) 0.6421(2) 0.0177(5) Uani 1 1 d . . . . .
C2 C 0.3040(4) 0.5560(3) 0.6783(2) 0.0193(5) Uani 1 1 d . . . . .
H2A H 0.1621 0.4508 0.6771 0.023 Uiso 1 1 calc R U . . .
H2B H 0.2969 0.5784 0.5880 0.023 Uiso 1 1 calc R U . . .
C3 C 0.3536(4) 0.7455(3) 0.7824(2) 0.0193(5) Uani 1 1 d . . . . .
H3A H 0.4982 0.8471 0.7840 0.023 Uiso 1 1 calc R U . . .
H3B H 0.3623 0.7202 0.8719 0.023 Uiso 1 1 calc R U . . .
C4 C 0.1829(4) 0.8259(3) 0.7558(2) 0.0188(5) Uani 1 1 d . . . . .
H4A H 0.0378 0.7243 0.7533 0.023 Uiso 1 1 calc R U . . .
H4B H 0.1755 0.8537 0.6671 0.023 Uiso 1 1 calc R U . . .
C5 C 0.2352(4) 1.0156(3) 0.8634(3) 0.0192(5) Uani 1 1 d . . . . .
H5A H 0.2403 0.9853 0.9514 0.023 Uiso 1 1 calc R U . . .
H5B H 0.3829 1.1140 0.8673 0.023 Uiso 1 1 calc R U . . .
C6 C 0.0765(4) 1.1091(3) 0.8432(2) 0.0201(5) Uani 1 1 d . . . . .
H6A H -0.0708 1.0132 0.8426 0.024 Uiso 1 1 calc R U . . .
H6B H 0.0680 1.1372 0.7546 0.024 Uiso 1 1 calc R U . . .
C7 C 0.1397(4) 1.3010(4) 0.9511(3) 0.0255(5) Uani 1 1 d . . . . .
H7A H 0.0294 1.3534 0.9338 0.038 Uiso 1 1 calc R U . . .
H7B H 0.2826 1.3988 0.9499 0.038 Uiso 1 1 calc R U . . .
H7C H 0.1477 1.2745 1.0393 0.038 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 0.01424(14) 0.01404(14) 0.02242(16) 0.00290(11) 0.00548(10) 0.00879(10)
S1 0.0160(3) 0.0184(3) 0.0262(3) 0.0017(3) 0.0030(2) 0.0109(2)
S2 0.0166(3) 0.0170(3) 0.0225(3) 0.0016(2) 0.0033(2) 0.0104(2)
O1 0.0167(8) 0.0182(8) 0.0239(9) 0.0025(7) 0.0026(7) 0.0118(7)
C1 0.0163(11) 0.0161(11) 0.0235(13) 0.0056(10) 0.0089(10) 0.0079(9)
C2 0.0164(12) 0.0195(12) 0.0275(14) 0.0059(11) 0.0061(10) 0.0132(10)
C3 0.0182(12) 0.0176(11) 0.0229(13) 0.0031(10) 0.0042(10) 0.0100(9)
C4 0.0187(12) 0.0160(11) 0.0237(13) 0.0035(10) 0.0069(10) 0.0098(9)
C5 0.0187(12) 0.0172(11) 0.0260(13) 0.0048(10) 0.0082(10) 0.0115(9)
C6 0.0222(12) 0.0187(12) 0.0219(13) 0.0045(10) 0.0056(10) 0.0116(10)
C7 0.0296(14) 0.0222(13) 0.0271(14) 0.0004(11) 0.0058(11) 0.0170(11)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd S1 2.3249(7) 2_656 ?
Pd S1 2.3249(7) . ?
Pd S2 2.3354(6) 2_656 ?
Pd S2 2.3354(6) . ?
S1 C1 1.700(2) . ?
S2 C1 1.697(3) . ?
O1 C1 1.298(3) . ?
O1 C2 1.467(3) . ?
C2 C3 1.509(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.513(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.523(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.506(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.522(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?

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
_geom_angle_publ_flag
S1 Pd S1 180.00(3) 2_656 . ?
S1 Pd S2 75.60(2) 2_656 2_656 ?
S1 Pd S2 104.40(2) . 2_656 ?
S1 Pd S2 104.40(2) 2_656 . ?
S1 Pd S2 75.60(2) . . ?
S2 Pd S2 180.0 2_656 . ?
C1 S1 Pd 85.06(9) . . ?
C1 S2 Pd 84.79(8) . . ?
C1 O1 C2 119.49(19) . . ?
O1 C1 S2 125.91(18) . . ?
O1 C1 S1 119.58(18) . . ?
S2 C1 S1 114.50(14) . . ?
O1 C2 C3 106.29(18) . . ?
O1 C2 H2A 110.5 . . ?
C3 C2 H2A 110.5 . . ?
O1 C2 H2B 110.5 . . ?
C3 C2 H2B 110.5 . . ?
H2A C2 H2B 108.7 . . ?
C2 C3 C4 112.69(19) . . ?
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 111.6(2) . . ?
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 . . ?
C6 C5 C4 115.3(2) . . ?
C6 C5 H5A 108.4 . . ?
C4 C5 H5A 108.4 . . ?
C6 C5 H5B 108.4 . . ?
C4 C5 H5B 108.4 . . ?
H5A C5 H5B 107.5 . . ?
C5 C6 C7 113.2(2) . . ?
C5 C6 H6A 108.9 . . ?
C7 C6 H6A 108.9 . . ?
C5 C6 H6B 108.9 . . ?
C7 C6 H6B 108.9 . . ?
H6A C6 H6B 107.8 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 O1 C1 S2 -1.0(3) . . . . ?
C2 O1 C1 S1 179.98(14) . . . . ?
Pd S2 C1 O1 -177.19(19) . . . . ?
Pd S2 C1 S1 1.84(11) . . . . ?
Pd S1 C1 O1 177.25(17) . . . . ?
Pd S1 C1 S2 -1.84(11) . . . . ?
C1 O1 C2 C3 -178.65(18) . . . . ?
O1 C2 C3 C4 179.52(17) . . . . ?
C2 C3 C4 C5 179.21(19) . . . . ?
C3 C4 C5 C6 178.59(18) . . . . ?
C4 C5 C6 C7 -178.4(2) . . . . ?

_refine_diff_density_max         0.914
_refine_diff_density_min         -1.048
_refine_diff_density_rms         0.105

_shelx_res_file                  
;

    shelx.res created by SHELXL-2014/7


TITL  10
CELL  0.71073 6.8083 7.5446 10.4837 101.008 98.983 112.048
ZERR  1       0.0005 0.0004  0.0008   0.006  0.006   0.006
LATT  1
SFAC  C H O S Pd
UNIT  14 26 2 4 1
ACTA
TEMP -173
SIZE  0.30 0.20 0.03
FMAP  2
PLAN -1
L.S.  24
BOND  $H
CONF
WGHT    0.023100    0.081700
FVAR       6.15203
PD    5    0.500000    0.000000    0.500000    10.50000    0.01424    0.01404 =
         0.02242    0.00290    0.00548    0.00879
S1    4    0.691470    0.272748    0.686316    11.00000    0.01598    0.01837 =
         0.02616    0.00174    0.00295    0.01091
S2    4    0.291214    0.184867    0.500282    11.00000    0.01657    0.01704 =
         0.02254    0.00157    0.00325    0.01037
O1    3    0.482962    0.498096    0.716694    11.00000    0.01672    0.01821 =
         0.02392    0.00245    0.00256    0.01179
C1    1    0.484222    0.340157    0.642087    11.00000    0.01625    0.01610 =
         0.02345    0.00562    0.00887    0.00791
C2    1    0.304021    0.556013    0.678329    11.00000    0.01637    0.01950 =
         0.02750    0.00591    0.00606    0.01322
AFIX  23
H2A   2    0.162108    0.450767    0.677051    11.00000   -1.20000
H2B   2    0.296860    0.578358    0.588010    11.00000   -1.20000
AFIX   0
C3    1    0.353585    0.745512    0.782418    11.00000    0.01819    0.01761 =
         0.02288    0.00307    0.00419    0.00998
AFIX  23
H3A   2    0.498166    0.847066    0.783998    11.00000   -1.20000
H3B   2    0.362307    0.720215    0.871931    11.00000   -1.20000
AFIX   0
C4    1    0.182871    0.825947    0.755849    11.00000    0.01872    0.01600 =
         0.02368    0.00354    0.00686    0.00982
AFIX  23
H4A   2    0.037758    0.724274    0.753288    11.00000   -1.20000
H4B   2    0.175549    0.853737    0.667094    11.00000   -1.20000
AFIX   0
C5    1    0.235164    1.015568    0.863382    11.00000    0.01872    0.01719 =
         0.02602    0.00478    0.00820    0.01155
AFIX  23
H5A   2    0.240269    0.985325    0.951351    11.00000   -1.20000
H5B   2    0.382924    1.114050    0.867290    11.00000   -1.20000
AFIX   0
C6    1    0.076451    1.109126    0.843238    11.00000    0.02216    0.01871 =
         0.02190    0.00446    0.00562    0.01163
AFIX  23
H6A   2   -0.070816    1.013244    0.842592    11.00000   -1.20000
H6B   2    0.068001    1.137171    0.754552    11.00000   -1.20000
AFIX   0
C7    1    0.139650    1.301049    0.951138    11.00000    0.02961    0.02219 =
         0.02708    0.00036    0.00577    0.01701
AFIX 137
H7A   2    0.029391    1.353429    0.933757    11.00000   -1.50000
H7B   2    0.282586    1.398847    0.949857    11.00000   -1.50000
H7C   2    0.147672    1.274459    1.039282    11.00000   -1.50000

AFIX   0
HKLF  4 1

REM   10
REM R1 =  0.0291 for    2006 Fo > 4sig(Fo)  and  0.0329 for all    2192 data
REM     98 parameters refined using      0 restraints

END

WGHT      0.0235      0.0737

REM Highest difference peak  0.914,  deepest hole -1.048,  1-sigma level  0.105
Q1    1   0.5013  0.0005  0.5959  11.00000  0.05    0.91
;
_shelx_res_checksum              68431
