#------------------------------------------------------------------------------
#$Date: 2016-02-19 23:18:51 +0100 (vie 19 de feb de 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/25/2012538.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_2012538
loop_
_publ_author_name
'Johansson, Maria H.'
'Oskarsson, Åke'
_publ_section_title
;
 Tetrakis(dimethyl sulfide)palladium(II) bis(tetrafluoroborate) and
 tetrakis(1,4-oxathiane-κS)palladium(II) bis(tetrafluoroborate)
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m102
_journal_page_last               m104
_journal_paper_doi               10.1107/S0108270101019357
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Pd (C4 H8 O S)4] (B F4)2'
_chemical_formula_moiety         'C16 H32 O4 Pd S4 2+ , 2B F4 -'
_chemical_formula_sum            'C16 H32 B2 F8 O4 Pd S4'
_chemical_formula_weight         696.68
_chemical_name_systematic
;
tetrakis(1,4-oxathiane-S)palladium(II) bis(tetrafluoroborate)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                94.11(3)
_cell_angle_beta                 114.12(3)
_cell_angle_gamma                111.79(3)
_cell_formula_units_Z            1
_cell_length_a                   8.8804(18)
_cell_length_b                   9.5397(19)
_cell_length_c                   9.6999(19)
_cell_measurement_reflns_used    2469
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      4
_cell_volume                     671.8(4)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2000)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997b)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full .989
_diffrn_measured_fraction_theta_max .989
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .050
_diffrn_reflns_av_sigmaI/netI    .109
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4856
_diffrn_reflns_theta_full        27.87
_diffrn_reflns_theta_max         27.87
_diffrn_reflns_theta_min         2.38
_diffrn_standards_decay_%        .00
_exptl_absorpt_coefficient_mu    1.079
_exptl_absorpt_correction_T_max  .882
_exptl_absorpt_correction_T_min  .813
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             352
_exptl_crystal_size_max          .20
_exptl_crystal_size_mid          .14
_exptl_crystal_size_min          .12
_refine_diff_density_max         2.56
_refine_diff_density_min         -2.61
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   .960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         3185
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      .960
_refine_ls_R_factor_all          .109
_refine_ls_R_factor_gt           .080
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.1175P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .188
_refine_ls_wR_factor_ref         .203
_reflns_number_gt                2080
_reflns_number_total             3185
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            tr1008.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        671.8(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2012538
_cod_database_fobs_code          2012538
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_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_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Pd .0000 .0000 .0000 .0389(3) Uani d S 1 . . Pd
S1 .1223(3) -.12129(19) .18864(18) .0434(4) Uani d . 1 . . S
S2 -.0004(3) .1677(2) .18654(18) .0453(5) Uani d . 1 . . S
O1 .1913(9) -.4185(7) .2135(7) .0646(15) Uani d . 1 . . O
O2 .0678(9) .2047(7) .5288(6) .0673(17) Uani d . 1 . . O
C1 .3008(11) -.1557(11) .1718(11) .061(2) Uani d . 1 . . C
H1A .2616 -.1989 .0627 .074 Uiso calc R 1 . . H
H1B .4106 -.0577 .2104 .074 Uiso calc R 1 . . H
C2 .3429(14) -.2699(13) .2665(12) .076(3) Uani d . 1 . . C
H2A .4438 -.2831 .2612 .091 Uiso calc R 1 . . H
H2B .3825 -.2252 .3753 .091 Uiso calc R 1 . . H
C3 -.0429(10) -.3229(8) .1328(8) .0461(16) Uani d . 1 . . C
H3A -.1473 -.3286 .1462 .055 Uiso calc R 1 . . H
H3B -.0868 -.3692 .0233 .055 Uiso calc R 1 . . H
C4 .0455(13) -.4120(9) .2328(9) .057(2) Uani d . 1 . . C
H4A .0908 -.3632 .3419 .069 Uiso calc R 1 . . H
H4B -.0471 -.5179 .2077 .069 Uiso calc R 1 . . H
C5 -.1404(11) .0437(9) .2626(8) .0507(18) Uani d . 1 . . C
H5A -.2687 -.0030 .1842 .061 Uiso calc R 1 . . H
H5B -.1054 -.0400 .2873 .061 Uiso calc R 1 . . H
C6 -.1142(12) .1405(12) .4094(9) .063(2) Uani d . 1 . . C
H6A -.1485 .2244 .3839 .076 Uiso calc R 1 . . H
H6B -.1947 .0749 .4463 .076 Uiso calc R 1 . . H
C7 .2141(12) .2538(10) .3612(9) .060(2) Uani d . 1 . . C
H7A .2585 .1757 .3878 .072 Uiso calc R 1 . . H
H7B .3040 .3369 .3449 .072 Uiso calc R 1 . . H
C8 .1905(13) .3200(10) .4944(9) .066(2) Uani d . 1 . . C
H8A .3092 .3717 .5874 .079 Uiso calc R 1 . . H
H8B .1460 .3979 .4666 .079 Uiso calc R 1 . . H
B1 -.4746(15) .2873(13) .1682(14) .070(3) Uani d . 1 . . B
F1 -.4548(13) .2388(15) .3108(11) .157(4) Uani d . 1 . . F
F2 -.646(2) .251(3) .094(2) .108(8) Uani d P .51(2) . . F
F2' -.543(4) .398(3) .174(2) .134(10) Uani d P .49(2) . . F
F3 -.447(3) .172(3) .0910(16) .121(8) Uani d P .51(2) . . F
F3' -.607(5) .172(3) .069(4) .23(2) Uani d P .49(2) . . F
F4 -.348(4) .412(3) .216(3) .191(18) Uani d P .51(2) . . F
F4' -.325(4) .350(6) .168(6) .24(2) Uani d P .49(2) . . F
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Pd .0707(6) .0420(4) .0305(4) .0368(4) .0350(4) .0191(3)
S1 .0724(12) .0431(9) .0329(8) .0363(9) .0297(8) .0181(7)
S2 .0823(13) .0502(10) .0344(8) .0455(10) .0384(9) .0216(7)
O1 .093(4) .071(4) .067(4) .062(4) .045(3) .031(3)
O2 .118(5) .083(4) .034(3) .066(4) .043(3) .029(3)
C1 .059(5) .079(6) .061(5) .040(4) .029(4) .030(4)
C2 .079(6) .102(8) .074(6) .067(6) .034(5) .039(6)
C3 .069(5) .045(4) .049(4) .034(4) .040(4) .021(3)
C4 .101(6) .053(4) .058(5) .052(4) .054(5) .031(4)
C5 .063(5) .070(5) .038(4) .038(4) .033(3) .016(3)
C6 .090(6) .095(6) .046(4) .059(5) .050(4) .033(4)
C7 .077(5) .050(5) .054(5) .028(4) .032(4) .004(3)
C8 .095(6) .059(5) .039(4) .045(5) .020(4) -.001(4)
B1 .055(7) .059(7) .077(7) .010(6) .031(5) -.004(5)
F1 .179(8) .258(12) .120(7) .149(8) .093(6) .088(7)
F2 .063(10) .16(2) .114(14) .055(14) .045(10) .038(15)
F2' .17(2) .15(2) .112(14) .111(19) .053(13) .038(13)
F3 .183(19) .18(2) .065(8) .128(17) .070(10) .032(9)
F3' .21(4) .12(2) .22(3) -.02(2) .07(2) -.09(2)
F4 .15(2) .119(16) .19(2) -.073(16) .117(18) -.086(15)
F4' .19(3) .32(5) .44(6) .18(3) .26(4) .27(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B .0013 .0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -.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_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S2 Pd S2 2 . 180.00(8) ?
S1 Pd S2 2 . 89.48(6) yes
S1 Pd S2 . . 90.52(6) yes
S1 Pd S2 2 2 90.52(6) ?
S2 Pd S1 . 2 89.48(6) ?
S1 Pd S1 . 2 180.00(9) ?
Pd S1 C1 . . 111.3(3) yes
Pd S1 C3 . . 108.4(2) yes
Pd S2 C5 . . 106.2(3) yes
Pd S2 C7 . . 111.7(3) yes
C1 S1 C3 . . 97.7(4) yes
C5 S2 C7 . . 98.7(4) yes
C2 O1 C4 . . 112.6(7) yes
C6 O2 C8 . . 113.0(6) yes
C2 C1 S1 . . 109.7(6) ?
O1 C2 C1 . . 113.4(7) ?
C4 C3 S1 . . 109.6(6) ?
O1 C4 C3 . . 113.8(6) ?
C6 C5 S2 . . 109.6(6) ?
O2 C6 C5 . . 111.8(7) ?
C8 C7 S2 . . 109.7(6) ?
O2 C8 C7 . . 112.7(7) ?
F4 B1 F3' . . 156(2) ?
F4 B1 F4' . . 42(2) ?
F3' B1 F4' . . 124(3) ?
F4 B1 F2 . . 129(2) ?
F3' B1 F2 . . 47(2) ?
F4' B1 F2 . . 145(2) ?
F4 B1 F2' . . 73(2) ?
F3' B1 F2' . . 104(2) ?
F4' B1 F2' . . 110(2) ?
F2 B1 F2' . . 58.1(13) ?
F4 B1 F3 . . 111.8(18) ?
F3' B1 F3 . . 61(2) ?
F4' B1 F3 . . 70(2) ?
F2 B1 F3 . . 106.2(16) ?
F2' B1 F3 . . 154.8(14) ?
F4 B1 F1 . . 102.6(16) ?
F3' B1 F1 . . 102(2) ?
F4' B1 F1 . . 112(2) ?
F2 B1 F1 . . 103.2(11) ?
F2' B1 F1 . . 102.6(12) ?
F3 B1 F1 . . 100.3(12) ?
F3' F2 B1 . . 64(2) ?
F3' F2 F2' . . 128(3) ?
B1 F2 F2' . . 65.9(13) ?
F2 F2' B1 . . 56.0(11) ?
F2 F2' F4 . . 101.1(16) ?
B1 F2' F4 . . 46.6(11) ?
F3' F3 B1 . . 51.7(11) ?
F3' F3 F4' . . 96.8(17) ?
B1 F3 F4' . . 48.9(11) ?
F2 F3' B1 . . 69.9(17) ?
F2 F3' F3 . . 136(3) ?
B1 F3' F3 . . 68(2) ?
F4' F4 B1 . . 73(3) ?
F4' F4 F2' . . 126(4) ?
B1 F4 F2' . . 60.0(14) ?
F4 F4' B1 . . 65.5(19) ?
F4 F4' F3 . . 126(3) ?
B1 F4' F3 . . 60.8(18) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd S1 . 2.3406(17) yes
Pd S1 2 2.3406(17) ?
Pd S2 2 2.3293(17) ?
Pd S2 . 2.3293(17) yes
S1 C1 . 1.799(9) yes
S1 C3 . 1.803(7) yes
S2 C5 . 1.809(7) yes
S2 C7 . 1.782(8) yes
O1 C2 . 1.414(12) yes
O1 C4 . 1.403(10) yes
O2 C6 . 1.401(10) yes
O2 C8 . 1.403(11) yes
C1 C2 . 1.529(12) ?
C3 C4 . 1.507(10) ?
C5 C6 . 1.523(10) ?
C7 C8 . 1.522(11) ?
B1 F4 . 1.180(19) ?
B1 F3' . 1.22(2) ?
B1 F4' . 1.24(2) ?
B1 F2 . 1.278(18) ?
B1 F2' . 1.41(2) ?
B1 F3 . 1.436(19) ?
B1 F1 . 1.453(14) ?
F2 F3' . .99(4) ?
F2 F2' . 1.31(3) ?
F2' F4 . 1.56(3) ?
F3 F3' . 1.35(4) ?
F3 F4' . 1.55(5) ?
F4 F4' . .86(4) ?
