#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/09/4330937.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_4330937
loop_
_publ_author_name
'Tianning Diao'
'Paul White'
'Ilia Guzei'
'Shannon S. Stahl'
_publ_contact_author_address
;
Department of Chemistry
University of Wisconsin-Madison
1101 University Ave
Madison, WI  53706
USA
;
_publ_contact_author_email       iguzei@chem.wisc.edu
_publ_contact_author_fax         608-262-0381
_publ_contact_author_name
;
Guzei, Ilia A. 
;
_publ_contact_author_phone       608-263-4694
_publ_section_title
;
 Characterization of DMSO Coordination to Palladium(II) in Solution and
 Insights into the Aerobic Oxidation Catalyst, Pd(DMSO)2(TFA)2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11898
_journal_page_last               11909
_journal_paper_doi               10.1021/ic301799p
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C8 H12 F6 O7 Pd S'
_chemical_formula_sum            'C8 H12 F6 O7 Pd S'
_chemical_formula_weight         472.64
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 98.79(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.382(4)
_cell_length_b                   7.650(3)
_cell_length_c                   24.478(9)
_cell_measurement_reflns_used    9977
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.5563
_cell_measurement_theta_min      2.4781
_cell_volume                     1551.2(11)
_computing_cell_refinement       'SAINT Ver. 7.68A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 Ver. 2010.11-3 (Bruker-AXS, 2010)'
_computing_data_reduction        'SAINT Ver. 7.68A'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXTL, OLEX2 (Dolomanov et al., 2009)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.50° ω and 0.5° φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0180
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            28411
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.52
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    1.426
_exptl_absorpt_correction_T_max  0.6910
_exptl_absorpt_correction_T_min  0.6134
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS  (Bruker-AXS, 2007)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.024
_exptl_crystal_description       needle
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4710
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0204
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0163P)²+1.2302P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0457
_refine_ls_wR_factor_ref         0.0465
_reflns_number_gt                4408
_reflns_number_total             4710
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic301799p_si_002_2.cif
_cod_data_source_block           stahl138
_cod_original_cell_volume        1551.0(11)
_cod_original_sg_symbol_Hall     '-P 2yn      '
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4330937
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.957765(13) 0.289358(15) 0.731314(4) 0.01319(3) Uani 1 1 d . . .
S1 S 1.14440(4) 0.47634(5) 0.715406(14) 0.01565(7) Uani 1 1 d . . .
F1 F 0.65088(15) 0.47074(18) 0.54628(5) 0.0423(3) Uani 1 1 d . . .
F2 F 0.73829(14) 0.20606(19) 0.54839(4) 0.0405(3) Uani 1 1 d . . .
F3 F 0.50525(13) 0.26299(17) 0.57034(4) 0.0336(3) Uani 1 1 d . . .
F4 F 1.14664(17) 0.18294(16) 0.91630(4) 0.0398(3) Uani 1 1 d . . .
F5 F 0.99191(16) 0.3744(2) 0.94411(4) 0.0449(3) Uani 1 1 d . . .
F6 F 1.20811(16) 0.45541(19) 0.91456(5) 0.0459(3) Uani 1 1 d . . .
O1 O 0.86745(13) 0.28376(15) 0.64993(4) 0.0176(2) Uani 1 1 d . . .
O2 O 0.64680(16) 0.4375(2) 0.66183(5) 0.0398(4) Uani 1 1 d . . .
O3 O 1.05450(13) 0.27390(15) 0.81185(4) 0.0166(2) Uani 1 1 d . . .
O4 O 0.8811(2) 0.4652(3) 0.84041(6) 0.0552(5) Uani 1 1 d . . .
O5 O 0.77845(14) 0.12181(17) 0.74711(5) 0.0232(2) Uani 1 1 d D . .
H5A H 0.808(2) 0.0407(17) 0.7768(5) 0.035 Uiso 1 1 d D . .
H5B H 0.732(2) 0.0508(18) 0.7166(5) 0.035 Uiso 1 1 d D . .
O6 O 1.26051(14) 0.52729(16) 0.76388(4) 0.0216(2) Uani 1 1 d . . .
C1 C 0.72951(19) 0.3503(2) 0.63505(6) 0.0209(3) Uani 1 1 d . . .
C2 C 0.6562(2) 0.3197(3) 0.57388(7) 0.0245(3) Uani 1 1 d . . .
C3 C 0.9948(2) 0.3644(2) 0.84710(6) 0.0238(3) Uani 1 1 d . . .
C4 C 1.0859(2) 0.3426(3) 0.90661(7) 0.0266(4) Uani 1 1 d . . .
C5 C 1.0501(2) 0.6661(2) 0.68371(8) 0.0264(3) Uani 1 1 d . . .
H5C H 0.9838 0.6340 0.6486 0.040 Uiso 1 1 calc R . .
H5D H 1.1329 0.7502 0.6767 0.040 Uiso 1 1 calc R . .
H5E H 0.9815 0.7189 0.7083 0.040 Uiso 1 1 calc R . .
C6 C 1.2465(2) 0.3862(2) 0.66398(6) 0.0223(3) Uani 1 1 d . . .
H6A H 1.2922 0.2725 0.6765 0.033 Uiso 1 1 calc R . .
H6B H 1.3335 0.4651 0.6572 0.033 Uiso 1 1 calc R . .
H6C H 1.1703 0.3709 0.6297 0.033 Uiso 1 1 calc R . .
O1S O 0.9959(4) 0.4436(4) 0.43668(11) 0.0382(7) Uani 0.50 1 d P A -1
O2S O 0.9924(10) 0.5401(10) 0.5224(3) 0.0268(12) Uani 0.50 1 d P A -1
C1S C 1.1089(17) 0.271(2) 0.5139(4) 0.037(2) Uani 0.50 1 d P A -1
H1SA H 1.1196 0.1792 0.4869 0.055 Uiso 0.50 1 calc PR A -1
H1SB H 1.0454 0.2276 0.5415 0.055 Uiso 0.50 1 calc PR A -1
H1SC H 1.2163 0.3063 0.5323 0.055 Uiso 0.50 1 calc PR A -1
C2S C 1.0279(13) 0.4213(13) 0.4858(4) 0.0227(15) Uani 0.50 1 d P A -1
C3S C 0.9069(15) 0.7000(18) 0.4986(4) 0.035(2) Uani 0.50 1 d P A -1
H3SA H 0.9703 0.7567 0.4725 0.041 Uiso 0.50 1 calc PR A -1
H3SB H 0.8000 0.6678 0.4780 0.041 Uiso 0.50 1 calc PR A -1
C4S C 0.8864(6) 0.8216(6) 0.54322(19) 0.0385(9) Uani 0.50 1 d P A -1
H4SA H 0.8310 0.9271 0.5275 0.058 Uiso 0.50 1 calc PR A -1
H4SB H 0.9925 0.8533 0.5634 0.058 Uiso 0.50 1 calc PR A -1
H4SC H 0.8221 0.7657 0.5685 0.058 Uiso 0.50 1 calc PR A -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'
F F 0.0171 0.0103 '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'
Pd Pd -0.9988 1.0072 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
O3 Pd1 O1 175.12(5) yes
O3 Pd1 O5 88.62(5) yes
O1 Pd1 O5 89.87(5) yes
O3 Pd1 S1 91.18(4) yes
O1 Pd1 S1 90.50(4) yes
O5 Pd1 S1 177.93(4) yes
O6 S1 C6 110.26(8) ?
O6 S1 C5 109.42(8) ?
C6 S1 C5 103.87(9) ?
O6 S1 Pd1 115.56(5) ?
C6 S1 Pd1 107.91(6) ?
C5 S1 Pd1 109.17(7) ?
C1 O1 Pd1 117.62(10) ?
C3 O3 Pd1 119.45(10) ?
Pd1 O5 H5A 115.8(12) ?
Pd1 O5 H5B 115.5(12) ?
H5A O5 H5B 104.51(16) ?
O2 C1 O1 129.32(15) ?
O2 C1 C2 115.33(15) ?
O1 C1 C2 115.34(14) ?
F2 C2 F3 108.27(15) ?
F2 C2 F1 108.04(15) ?
F3 C2 F1 106.97(15) ?
F2 C2 C1 113.45(14) ?
F3 C2 C1 110.24(14) ?
F1 C2 C1 109.65(15) ?
O4 C3 O3 129.56(15) ?
O4 C3 C4 117.30(15) ?
O3 C3 C4 113.12(14) ?
F5 C4 F4 107.34(16) ?
F5 C4 F6 107.85(16) ?
F4 C4 F6 107.74(15) ?
F5 C4 C3 111.91(14) ?
F4 C4 C3 112.77(14) ?
F6 C4 C3 109.04(16) ?
S1 C5 H5C 109.5 ?
S1 C5 H5D 109.5 ?
H5C C5 H5D 109.5 ?
S1 C5 H5E 109.5 ?
H5C C5 H5E 109.5 ?
H5D C5 H5E 109.5 ?
S1 C6 H6A 109.5 ?
S1 C6 H6B 109.5 ?
H6A C6 H6B 109.5 ?
S1 C6 H6C 109.5 ?
H6A C6 H6C 109.5 ?
H6B C6 H6C 109.5 ?
C2S O2S C3S 115.9(6) ?
O1S C2S O2S 122.2(6) ?
O1S C2S C1S 127.1(11) ?
O2S C2S C1S 110.7(8) ?
C4S C3S O2S 109.5(6) ?
C4S C3S H3SA 109.8 ?
O2S C3S H3SA 109.8 ?
C4S C3S H3SB 109.8 ?
O2S C3S H3SB 109.8 ?
H3SA C3S H3SB 108.2 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 O3 2.0171(13) yes
Pd1 O1 2.0205(13) yes
Pd1 O5 2.0564(13) yes
Pd1 S1 2.1979(8) yes
S1 O6 1.4677(13) ?
S1 C6 1.7666(17) ?
S1 C5 1.7737(18) ?
F1 C2 1.336(2) ?
F2 C2 1.323(2) ?
F3 C2 1.328(2) ?
F4 C4 1.330(2) ?
F5 C4 1.321(2) ?
F6 C4 1.331(2) ?
O1 C1 1.265(2) ?
O2 C1 1.222(2) ?
O3 C3 1.2673(19) ?
O4 C3 1.217(2) ?
O5 H5A 0.9580(11) ?
O5 H5B 0.9580(11) ?
C1 C2 1.547(2) ?
C3 C4 1.547(2) ?
C5 H5C 0.9800 ?
C5 H5D 0.9800 ?
C5 H5E 0.9800 ?
C6 H6A 0.9800 ?
C6 H6B 0.9800 ?
C6 H6C 0.9800 ?
O1S C2S 1.203(10) ?
O2S C2S 1.342(5) ?
O2S C3S 1.491(13) ?
C1S C2S 1.451(14) ?
C1S H1SA 0.9800 ?
C1S H1SB 0.9800 ?
C1S H1SC 0.9800 ?
C3S C4S 1.464(15) ?
C3S H3SA 0.9900 ?
C3S H3SB 0.9900 ?
C4S H4SA 0.9800 ?
C4S H4SB 0.9800 ?
C4S H4SC 0.9800 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H5A O2 0.9580(11) 1.689(4) 2.6312(19) 166.9(17) 2_646
O5 H5B O4 0.9580(11) 1.692(5) 2.634(2) 166.6(18) 2_646
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
O3 Pd1 S1 O6 -2.14(7)
O1 Pd1 S1 O6 -177.55(7)
O3 Pd1 S1 C6 121.78(7)
O1 Pd1 S1 C6 -53.63(7)
O3 Pd1 S1 C5 -125.94(8)
O1 Pd1 S1 C5 58.64(8)
O3 Pd1 O1 C1 138.3(5)
O5 Pd1 O1 C1 66.31(13)
S1 Pd1 O1 C1 -111.65(12)
O1 Pd1 O3 C3 -151.9(5)
O5 Pd1 O3 C3 -79.95(14)
S1 Pd1 O3 C3 97.99(13)
Pd1 O1 C1 O2 9.3(3)
Pd1 O1 C1 C2 -171.81(11)
O2 C1 C2 F2 -171.36(17)
O1 C1 C2 F2 9.6(2)
O2 C1 C2 F3 -49.8(2)
O1 C1 C2 F3 131.24(17)
O2 C1 C2 F1 67.8(2)
O1 C1 C2 F1 -111.25(17)
Pd1 O3 C3 O4 0.4(3)
Pd1 O3 C3 C4 -178.06(12)
O4 C3 C4 F5 27.3(3)
O3 C3 C4 F5 -154.05(17)
O4 C3 C4 F4 148.4(2)
O3 C3 C4 F4 -32.9(2)
O4 C3 C4 F6 -91.9(2)
O3 C3 C4 F6 86.72(19)
C3S O2S C2S O1S 1.5(8)
C3S O2S C2S C1S -179.4(13)
C2S O2S C3S C4S -176.2(5)
