#------------------------------------------------------------------------------
#$Date: 2016-03-05 11:01:17 +0200 (Sat, 05 Mar 2016) $
#$Revision: 177740 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/38/7223844.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_7223844
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                90.020(7)
_cell_angle_beta                 99.397(7)
_cell_angle_gamma                95.377(7)
_cell_formula_units_Z            1
_cell_length_a                   6.1398(6)
_cell_length_b                   6.7176(5)
_cell_length_c                   11.9393(10)
_cell_measurement_reflns_used    3530
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.7014
_cell_measurement_theta_min      3.7499
_cell_volume                     483.63(7)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
'Agilent Technologies SuperNova Dual diffractometer with Atlas detector'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_monochromator  Mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_laue_measured_fraction_full 0.995
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7538
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        74.970
_diffrn_reflns_theta_max         74.970
_diffrn_reflns_theta_min         3.753
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.778
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.34731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis PRO (Agilent, 2012)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_description       prism
_exptl_crystal_F_000             236
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         4.367
_refine_diff_density_min         -2.032
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1979
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0563
_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)+(0.1297P)²+0.3746P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1583
_refine_ls_wR_factor_ref         0.1636
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1861
_reflns_number_total             1979
_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               7223844
_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   0.202
_shelx_estimated_absorpt_t_max   0.590
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pd Pd 0.5000 0.5000 0.5000 0.0182(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_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
S2 Pd S2 180.0 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_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C2 O1 C1 S1 -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)
