#------------------------------------------------------------------------------
#$Date: 2016-05-28 04:36:26 +0300 (Sat, 28 May 2016) $
#$Revision: 183118 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/75/2107562.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2107562
loop_
_publ_author_name
'Tidey, Jeremiah P.'
'Wong, Henry L. S.'
'McMaster, Jonathan'
'Schröder, Martin'
'Blake, Alexander J.'
_publ_section_title
;
 High-pressure studies of three polymorphs of a palladium(II) oxathioether
 macrocyclic complex
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              357
_journal_page_last               371
_journal_paper_doi               10.1107/S2052520616007435
_journal_volume                  72
_journal_year                    2016
_chemical_formula_moiety         'C6 H12 Cl2 O Pd S2'
_chemical_formula_sum            'C6 H12 Cl2 O Pd S2'
_chemical_formula_weight         341.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     isomor
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.06 svn.r3119 for OlexSys, GUI svn.r4979)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.507(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5993(2)
_cell_length_b                   11.8196(6)
_cell_length_c                   8.4004(6)
_cell_measurement_pressure       6540000
_cell_measurement_reflns_used    3202
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.7760
_cell_measurement_theta_min      3.6780
_cell_volume                     851.18(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1592
_diffrn_measured_fraction_theta_full 0.553
_diffrn_measured_fraction_theta_max 0.481
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            7628
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.862
_diffrn_reflns_theta_min         3.692
_exptl_absorpt_coefficient_mu    3.237
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.665
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.118
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.515
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         973
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0286P)²+2.4830P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0674
_reflns_number_gt                842
_reflns_number_total             973
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            xk5029sup1.cif
_cod_data_source_block           bPd_8
_cod_original_cell_volume        851.17(8)
_cod_database_code               2107562
_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'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
Pd Pd1 0.17509(4) 0.51507(4) 0.04998(6) 0.01512(17) Uani d 1
S S4 0.12562(15) 0.53913(12) 0.3050(2) 0.0162(4) Uani d 1
Cl Cl1 0.21662(17) 0.70666(13) 0.0555(2) 0.0271(4) Uani d 1
S S7 0.16243(16) 0.32740(13) 0.0755(2) 0.0208(4) Uani d 1
Cl Cl2 0.22193(16) 0.48766(14) -0.2147(2) 0.0254(4) Uani d 1
O O1 0.4376(4) 0.4087(3) 0.3218(6) 0.0220(11) Uani d 1
C C6 0.0618(7) 0.3114(5) 0.2544(6) 0.0232(17) Uani d 1
H H6A -0.0495 0.3171 0.2262 0.028 Uiso calc 1
H H6B 0.0824 0.2361 0.2970 0.028 Uiso calc 1
C C8 0.3565(5) 0.2719(5) 0.1248(9) 0.0305(18) Uani d 1
H H8A 0.3505 0.2158 0.2084 0.037 Uiso calc 1
H H8B 0.3899 0.2332 0.0316 0.037 Uiso calc 1
C C9 0.4799(6) 0.3565(5) 0.1791(9) 0.0260(18) Uani d 1
H H9A 0.5798 0.3189 0.1984 0.031 Uiso calc 1
H H9B 0.4892 0.4133 0.0970 0.031 Uiso calc 1
C C5 0.1064(7) 0.3969(4) 0.3841(7) 0.0209(17) Uani d 1
H H5A 0.2046 0.3745 0.4399 0.025 Uiso calc 1
H H5B 0.0276 0.3971 0.4606 0.025 Uiso calc 1
C C2 0.4482(6) 0.5280(4) 0.3196(9) 0.0209(16) Uani d 1
H H2A 0.4480 0.5541 0.2101 0.025 Uiso calc 1
H H2B 0.5455 0.5515 0.3761 0.025 Uiso calc 1
C C3 0.3132(4) 0.5808(5) 0.3971(7) 0.0168(15) Uani d 1
H H3A 0.3223 0.6625 0.3918 0.020 Uiso calc 1
H H3B 0.3195 0.5595 0.5089 0.020 Uiso calc 1
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'
Cl Cl 0.1484 0.1585 '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_site_symmetry_3
_geom_angle
S4 Pd1 Pd1 3_565 91.17(4)
S4 Pd1 Cl1 . 84.04(6)
S4 Pd1 Cl2 . 178.81(5)
Cl1 Pd1 Pd1 3_565 105.48(4)
Cl1 Pd1 Cl2 . 96.83(6)
S7 Pd1 Pd1 3_565 81.80(4)
S7 Pd1 S4 . 91.14(6)
S7 Pd1 Cl1 . 171.30(6)
S7 Pd1 Cl2 . 88.09(6)
Cl2 Pd1 Pd1 3_565 87.83(4)
C5 S4 Pd1 . 105.2(2)
C3 S4 Pd1 . 102.40(19)
C3 S4 C5 . 101.5(3)
C6 S7 Pd1 . 102.4(2)
C6 S7 C8 . 105.4(3)
C8 S7 Pd1 . 109.32(19)
C2 O1 C9 . 113.7(5)
S7 C6 H6A . 108.6
S7 C6 H6B . 108.6
H6A C6 H6B . 107.5
C5 C6 S7 . 114.8(4)
C5 C6 H6A . 108.6
C5 C6 H6B . 108.6
S7 C8 H8A . 108.2
S7 C8 H8B . 108.2
H8A C8 H8B . 107.3
C9 C8 S7 . 116.4(4)
C9 C8 H8A . 108.2
C9 C8 H8B . 108.2
O1 C9 C8 . 108.9(5)
O1 C9 H9A . 109.9
O1 C9 H9B . 109.9
C8 C9 H9A . 109.9
C8 C9 H9B . 109.9
H9A C9 H9B . 108.3
S4 C5 H5A . 109.1
S4 C5 H5B . 109.1
C6 C5 S4 . 112.3(5)
C6 C5 H5A . 109.1
C6 C5 H5B . 109.1
H5A C5 H5B . 107.9
O1 C2 H2A . 109.5
O1 C2 H2B . 109.5
O1 C2 C3 . 110.7(4)
H2A C2 H2B . 108.1
C3 C2 H2A . 109.5
C3 C2 H2B . 109.5
S4 C3 H3A . 108.9
S4 C3 H3B . 108.9
C2 C3 S4 . 113.3(4)
C2 C3 H3A . 108.9
C2 C3 H3B . 108.9
H3A C3 H3B . 107.7
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Pd1 Pd1 3_565 3.0827(8)
Pd1 S4 . 2.2349(18)
Pd1 Cl1 . 2.2924(16)
Pd1 S7 . 2.2320(16)
Pd1 Cl2 . 2.314(2)
S4 C5 . 1.820(4)
S4 C3 . 1.802(4)
S7 C6 . 1.802(4)
S7 C8 . 1.811(4)
O1 C9 . 1.421(7)
O1 C2 . 1.413(6)
C6 H6A . 0.9700
C6 H6B . 0.9700
C6 C5 . 1.513(4)
C8 H8A . 0.9700
C8 H8B . 0.9700
C8 C9 . 1.502(4)
C9 H9A . 0.9700
C9 H9B . 0.9700
C5 H5A . 0.9700
C5 H5B . 0.9700
C2 H2A . 0.9700
C2 H2B . 0.9700
C2 C3 . 1.509(4)
C3 H3A . 0.9700
C3 H3B . 0.9700
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C6 H6A Cl1 3_565 0.97 2.69 3.402(6) 131.1
C6 H6A Cl2 3_565 0.97 2.74 3.403(7) 126.0
C6 H6B S7 4_566 0.97 2.50 3.217(6) 130.5
C6 H6B Cl2 4_566 0.97 2.91 3.795(7) 152.3
C8 H8A Cl2 4_566 0.97 2.75 3.580(6) 144.6
C8 H8B O1 4_565 0.97 2.49 3.436(8) 164.8
C9 H9A Cl1 3_665 0.97 2.88 3.473(6) 120.4
C9 H9A Cl2 3_665 0.97 2.85 3.152(5) 99.1
C5 H5A S7 4_566 0.97 2.68 3.119(5) 107.9
C5 H5A O1 . 0.97 2.34 2.939(7) 119.3
C5 H5B S4 3_566 0.97 2.57 3.492(6) 159.5
C2 H2B Cl2 3_665 0.97 2.54 3.041(5) 111.8
C2 H2B O1 3_666 0.97 2.57 3.183(9) 121.0
C3 H3A Cl1 4_576 0.97 2.30 2.991(5) 127.2
C3 H3B Cl2 1_556 0.97 2.67 3.587(7) 158.1
C3 H3B O1 3_666 0.97 2.46 3.064(7) 120.0
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
Pd1 S4 C5 C6 -23.7(4)
Pd1 S4 C3 C2 -31.9(5)
Pd1 S7 C6 C5 -38.3(5)
Pd1 S7 C8 C9 14.6(6)
S7 C6 C5 S4 42.1(6)
S7 C8 C9 O1 61.8(8)
O1 C2 C3 S4 -57.4(6)
C6 S7 C8 C9 -94.8(6)
C8 S7 C6 C5 76.0(5)
C9 O1 C2 C3 140.2(5)
C5 S4 C3 C2 76.6(5)
C2 O1 C9 C8 -131.6(5)
C3 S4 C5 C6 -130.1(4)

_cod_database_fobs_code 2107562
