#------------------------------------------------------------------------------
#$Date: 2016-03-05 11:01:17 +0200 (Sat, 05 Mar 2016) $
#$Revision: 177740 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/38/7223848.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7223848
loop_
_publ_author_name
'Tan, Yee Seng'
'Halim, Siti Nadiah Abdul'
'Molloy, Kieran C.'
'Sudlow, Anna L.'
'Otero-de-la-Roza, A.'
'Tiekink, Edward R. T.'
_publ_section_title
;
 Persistence of C--H⋯π(chelate ring) interactions in the crystal
 structures of Pd(S2COR)2. The utility of Pd(S2COR)2as precursors for
 palladium sulphide materials
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              1105
_journal_paper_doi               10.1039/C5CE02126J
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C14 H26 O2 Pd S4'
_chemical_formula_sum            'C14 H26 O2 Pd S4'
_chemical_formula_weight         460.99
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-04-09 deposited with the CCDC.
2016-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                101.008(6)
_cell_angle_beta                 98.983(6)
_cell_angle_gamma                112.048(6)
_cell_formula_units_Z            1
_cell_length_a                   6.8083(5)
_cell_length_b                   7.5446(4)
_cell_length_c                   10.4837(8)
_cell_measurement_reflns_used    1935
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4997
_cell_measurement_theta_min      3.0216
_cell_volume                     474.33(6)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2012)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2012)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2012)'
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and DIAMOND (Brandenburg, 2006)
;
_computing_publication_material  'SHELXL (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4041
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Agilent Technologies SuperNova Dual diffractometer with Atlas detector'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_monochromator  Mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3938
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.560
_diffrn_reflns_theta_min         3.028
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.419
_exptl_absorpt_correction_T_max  0.9587
_exptl_absorpt_correction_T_min  0.6756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis PRO (Agilent, 2011)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_description       prism
_exptl_crystal_F_000             236
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.914
_refine_diff_density_min         -1.048
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         2192
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0231P)²+0.0817P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0678
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2006
_reflns_number_total             2192
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ce02126j2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7223837--7223848.cif.'
_cod_database_code               7223848
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.676
_shelx_estimated_absorpt_t_max   0.959
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pd Pd 0.5000 0.0000 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_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
S1 Pd S1 180.00(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_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C2 O1 C1 S2 -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)
