#------------------------------------------------------------------------------
#$Date: 2016-03-05 10:01:17 +0100 (Sat 05 de Mar de 2016) $
#$Revision: 177740 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/38/7223846.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_7223846
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         'C12 H22 O2 Pd S4'
_chemical_formula_sum            'C12 H22 O2 Pd S4'
_chemical_formula_weight         432.93
_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                84.811(6)
_cell_angle_beta                 76.424(6)
_cell_angle_gamma                83.388(6)
_cell_formula_units_Z            1
_cell_length_a                   6.5622(4)
_cell_length_b                   6.8643(5)
_cell_length_c                   9.8385(7)
_cell_measurement_reflns_used    3284
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.4917
_cell_measurement_theta_min      2.9879
_cell_volume                     427.00(5)
_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  0.0400
_diffrn_reflns_av_unetI/netI     0.0352
_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       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6326
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.489
_diffrn_reflns_theta_max         27.489
_diffrn_reflns_theta_min         2.994
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.570
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis PRO (Agilent, 2011)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_description       prism
_exptl_crystal_F_000             220
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.184
_refine_diff_density_min         -1.227
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         1955
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0294
_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)+(0.0462P)²+0.0800P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1812
_reflns_number_total             1955
_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               7223846
_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   0.572
_shelx_estimated_absorpt_t_max   0.859
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 0.01657(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_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 180.0 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_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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_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 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)
