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#$Date: 2016-03-21 14:17:58 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178713 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/24/4082473.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_4082473
loop_
_publ_author_name
'Drinkel, Emma E.'
'Wu, Linglin'
'Linden, Anthony'
'Dorta, Reto'
_publ_section_title
;
 Synthesis, Structure, and Catalytic Studies of Palladium and Platinum
 Bis-Sulfoxide Complexes
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              627
_journal_paper_doi               10.1021/om4000067
_journal_volume                  33
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C38 H26 F6 O6 Pd S2, 2(C4 H10 O)'
_chemical_formula_sum            'C46 H46 F6 O8 Pd S2'
_chemical_formula_weight         1011.37
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      152
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             08-10-10
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   10.9606(1)
_cell_length_b                   10.9606(1)
_cell_length_c                   28.9827(4)
_cell_measurement_reflns_used    41903
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      2.0
_cell_volume                     3015.35(6)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL97 and PLATON (Spek, 2006)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 '65 mm CCD camera on \k goniostat'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Nonius KappaCCD area-detector diffractometer'
_diffrn_measurement_method       'φ and ω scans with κ offsets'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'Nonius FR590 sealed tube generator'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            45433
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.652
_exptl_absorpt_correction_T_max  0.914
_exptl_absorpt_correction_T_min  0.802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1554
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
See _refine_special_details
;
_refine_diff_density_max         0.972
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.165
_refine_ls_abs_structure_details
'Flack & Bernardinelli (2000), ? Friedel pairs'
_refine_ls_abs_structure_Flack   -0.10(4)
_refine_ls_extinction_coef       0.0072(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         5858
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0494
_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)+(0.0801P)²+1.3034P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1336
_refine_ls_wR_factor_ref         0.1399
_reflns_number_gt                4958
_reflns_number_total             5859
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            om4000067_si_001.cif
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      'P 31 2 1     '
_cod_database_code               4082473
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'y, x, -z'
'-x, -x+y, -z+1/3'
'x-y, -y, -z+2/3'
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 0.0000 0.78010(4) 0.1667 0.02967(12) Uani 1 2 d S . .
S3 S 0.07564(11) 0.95340(10) 0.11424(3) 0.0317(2) Uani 1 1 d . . .
F1A F 0.2187(10) 0.5356(6) 0.0984(3) 0.093(2) Uani 0.446(6) 1 d PDU A 1
F2A F 0.4000(5) 0.7373(10) 0.0969(3) 0.097(3) Uani 0.446(6) 1 d PDU A 1
F3A F 0.2343(10) 0.6889(10) 0.0505(2) 0.090(2) Uani 0.446(6) 1 d PDU A 1
F1B F 0.1685(6) 0.5733(8) 0.0649(3) 0.089(2) Uani 0.554(6) 1 d PDU A 2
F2B F 0.3224(9) 0.6083(9) 0.1150(3) 0.098(2) Uani 0.554(6) 1 d PDU A 2
F3B F 0.3571(8) 0.7703(7) 0.0683(3) 0.107(3) Uani 0.554(6) 1 d PDU A 2
O1 O 0.0656(3) 0.6793(3) 0.12235(11) 0.0399(7) Uani 1 1 d . . .
O2 O 0.2745(4) 0.8096(4) 0.15757(13) 0.0536(9) Uani 1 1 d . . .
O3 O 0.1796(3) 0.9547(4) 0.08246(10) 0.0442(7) Uani 1 1 d . . .
C1 C -0.1999(5) 0.8171(6) 0.08511(15) 0.0418(10) Uani 1 1 d . . .
H1 H -0.2159 0.7457 0.1068 0.050 Uiso 1 1 calc R . .
C2 C -0.3058(5) 0.8026(6) 0.05595(15) 0.0506(12) Uani 1 1 d . . .
H2 H -0.3952 0.7191 0.0571 0.061 Uiso 1 1 calc R . .
C3 C -0.2838(5) 0.9087(7) 0.02472(15) 0.0523(13) Uani 1 1 d . . .
C4 C -0.1514(5) 1.0309(7) 0.02374(14) 0.0543(12) Uani 1 1 d . . .
H4 H -0.1355 1.1049 0.0032 0.065 Uiso 1 1 calc R . .
C5 C -0.0444(5) 1.0460(6) 0.05183(15) 0.0476(12) Uani 1 1 d . . .
H5 H 0.0453 1.1291 0.0505 0.057 Uiso 1 1 calc R . .
C6 C -0.0682(5) 0.9397(5) 0.08190(13) 0.0360(9) Uani 1 1 d . . .
C7 C 0.1537(4) 1.1214(4) 0.14182(12) 0.0320(8) Uani 1 1 d . . .
C8 C 0.0802(4) 1.1720(4) 0.16563(13) 0.0322(8) Uani 1 1 d . . .
C9 C 0.1565(5) 1.3023(4) 0.19031(16) 0.0402(9) Uani 1 1 d . . .
C10 C 0.3082(5) 1.3744(5) 0.18967(18) 0.0455(10) Uani 1 1 d . . .
C11 C 0.3764(5) 1.3150(5) 0.16466(17) 0.0483(11) Uani 1 1 d . . .
H11 H 0.4764 1.3621 0.1645 0.058 Uiso 1 1 calc R . .
C12 C 0.3036(4) 1.1931(5) 0.14099(15) 0.0390(9) Uani 1 1 d . . .
H12 H 0.3518 1.1558 0.1240 0.047 Uiso 1 1 calc R . .
C13 C 0.3833(6) 1.5001(6) 0.2141(2) 0.0655(16) Uani 1 1 d . . .
H13 H 0.4834 1.5474 0.2146 0.079 Uiso 1 1 calc R . .
C14 C 0.3126(7) 1.5563(6) 0.2376(3) 0.077(2) Uani 1 1 d . . .
H14 H 0.3644 1.6420 0.2542 0.092 Uiso 1 1 calc R . .
C15 C 0.1668(6) 1.4884(6) 0.2370(3) 0.0692(17) Uani 1 1 d . . .
H15 H 0.1196 1.5303 0.2519 0.083 Uiso 1 1 calc R . .
C16 C 0.0903(5) 1.3619(5) 0.21522(18) 0.0491(11) Uani 1 1 d . . .
H16 H -0.0097 1.3136 0.2170 0.059 Uiso 1 1 calc R . .
C17 C 0.1981(5) 0.7267(5) 0.12884(18) 0.0450(11) Uani 1 1 d . A .
C18 C -0.4011(6) 0.8907(8) -0.00619(17) 0.0702(19) Uani 1 1 d . . .
H181 H -0.4724 0.8982 0.0121 0.105 Uiso 1 1 calc R . .
H182 H -0.4441 0.7979 -0.0210 0.105 Uiso 1 1 calc R . .
H183 H -0.3638 0.9643 -0.0299 0.105 Uiso 1 1 calc R . .
C19 C 0.2600(4) 0.6699(4) 0.0939(2) 0.0709(15) Uani 1 1 d DU . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 138 0.0033 0.0016
; International Tables for Crystallography (1992). 
Vol. C, Tables 4.2.6.8 and 6.1.1.4
;
H H 138 0.0000 0.0000
; International Tables for Crystallography (1992). 
Vol. C, Tables 4.2.6.8 and 6.1.1.4
;
F F 18 0.0171 0.0103
; International Tables for Crystallography (1992). 
Vol. C, Tables 4.2.6.8 and 6.1.1.4
;
O O 24 0.0106 0.0060
; International Tables for Crystallography (1992). 
Vol. C, Tables 4.2.6.8 and 6.1.1.4
;
Pd Pd 3 -0.9988 1.0072
; International Tables for Crystallography (1992). 
Vol. C, Tables 4.2.6.8 and 6.1.1.4
;
S S 6 0.1246 0.1234
; International Tables for Crystallography (1992). 
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_3
O1 Pd1 O1 88.56(18) 5
O1 Pd1 S3 175.72(9) 5
O1 Pd1 S3 87.19(9) .
S3 Pd1 S3 97.07(5) 5
O3 S3 C6 108.88(18) .
O3 S3 C7 107.65(19) .
C6 S3 C7 105.7(2) .
O3 S3 Pd1 113.07(15) .
C6 S3 Pd1 110.48(16) .
C7 S3 Pd1 110.72(12) .
C17 O1 Pd1 108.7(3) .
C2 C1 C6 118.3(5) .
C2 C1 H1 120.8 .
C6 C1 H1 120.8 .
C1 C2 C3 121.1(5) .
C1 C2 H2 119.5 .
C3 C2 H2 119.5 .
C2 C3 C4 118.4(5) .
C2 C3 C18 119.9(5) .
C4 C3 C18 121.7(5) .
C5 C4 C3 121.3(5) .
C5 C4 H4 119.3 .
C3 C4 H4 119.3 .
C4 C5 C6 119.3(5) .
C4 C5 H5 120.4 .
C6 C5 H5 120.4 .
C5 C6 C1 121.6(4) .
C5 C6 S3 118.7(4) .
C1 C6 S3 119.5(4) .
C8 C7 C12 122.3(4) .
C8 C7 S3 124.6(3) .
C12 C7 S3 112.8(3) .
C7 C8 C9 119.1(4) .
C7 C8 C8 121.9(3) 5
C9 C8 C8 119.0(3) 5
C16 C9 C8 122.9(4) .
C16 C9 C10 118.5(4) .
C8 C9 C10 118.6(4) .
C13 C10 C11 121.9(4) .
C13 C10 C9 119.1(5) .
C11 C10 C9 119.0(4) .
C12 C11 C10 122.0(4) .
C12 C11 H11 119.0 .
C10 C11 H11 119.0 .
C11 C12 C7 119.0(4) .
C11 C12 H12 120.5 .
C7 C12 H12 120.5 .
C14 C13 C10 120.2(5) .
C14 C13 H13 119.9 .
C10 C13 H13 119.9 .
C15 C14 C13 120.5(5) .
C15 C14 H14 119.8 .
C13 C14 H14 119.8 .
C16 C15 C14 120.6(5) .
C16 C15 H15 119.7 .
C14 C15 H15 119.7 .
C15 C16 C9 121.1(5) .
C15 C16 H16 119.5 .
C9 C16 H16 119.5 .
O2 C17 O1 128.4(4) .
O2 C17 C19 119.1(4) .
O1 C17 C19 112.5(4) .
C3 C18 H181 109.5 .
C3 C18 H182 109.5 .
H181 C18 H182 109.5 .
C3 C18 H183 109.5 .
H181 C18 H183 109.5 .
H182 C18 H183 109.5 .
F3B C19 F1A 132.7(7) .
F3B C19 F2B 106.2(4) .
F1A C19 F2B 50.2(4) .
F3B C19 F3A 58.7(4) .
F1A C19 F3A 106.8(4) .
F2B C19 F3A 136.2(7) .
F3B C19 F1B 106.6(4) .
F1A C19 F1B 58.0(4) .
F2B C19 F1B 105.2(4) .
F3A C19 F1B 52.6(4) .
F3B C19 F2A 49.1(4) .
F1A C19 F2A 105.8(4) .
F2B C19 F2A 60.6(4) .
F3A C19 F2A 104.6(4) .
F1B C19 F2A 133.3(7) .
F3B C19 C17 112.0(5) .
F1A C19 C17 114.8(5) .
F2B C19 C17 110.5(5) .
F3A C19 C17 113.2(5) .
F1B C19 C17 115.7(5) .
F2A C19 C17 110.8(5) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 O1 2.045(3) .
Pd1 S3 2.2427(10) .
S3 O3 1.460(3) .
S3 C6 1.775(4) .
S3 C7 1.785(4) .
F1A C19 1.312(5) .
F2A C19 1.331(5) .
F3A C19 1.326(5) .
F1B C19 1.329(5) .
F2B C19 1.326(5) .
F3B C19 1.312(5) .
O1 C17 1.289(5) .
O2 C17 1.208(6) .
C1 C2 1.380(6) .
C1 C6 1.400(7) .
C1 H1 0.9500 .
C2 C3 1.396(8) .
C2 H2 0.9500 .
C3 C4 1.399(8) .
C3 C18 1.497(7) .
C4 C5 1.368(7) .
C4 H4 0.9500 .
C5 C6 1.371(6) .
C5 H5 0.9500 .
C7 C8 1.371(6) .
C7 C12 1.423(6) .
C8 C9 1.433(6) .
C8 C8 1.525(7) 5
C9 C16 1.396(6) .
C9 C10 1.441(6) .
C10 C13 1.393(7) .
C10 C11 1.413(7) .
C11 C12 1.351(7) .
C11 H11 0.9500 .
C12 H12 0.9500 .
C13 C14 1.387(8) .
C13 H13 0.9500 .
C14 C15 1.385(9) .
C14 H14 0.9500 .
C15 C16 1.365(7) .
C15 H15 0.9500 .
C16 H16 0.9500 .
C17 C19 1.516(7) .
C18 H181 0.9800 .
C18 H182 0.9800 .
C18 H183 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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O1 Pd1 S3 O3 -21.41(17) . .
S3 Pd1 S3 O3 158.20(16) 5 .
O1 Pd1 S3 C6 100.90(17) . .
S3 Pd1 S3 C6 -79.49(15) 5 .
O1 Pd1 S3 C7 -142.31(17) . .
S3 Pd1 S3 C7 37.30(14) 5 .
O1 Pd1 O1 C17 -96.0(3) 5 .
S3 Pd1 O1 C17 84.4(3) . .
C6 C1 C2 C3 -1.5(7) . .
C1 C2 C3 C4 -0.2(8) . .
C1 C2 C3 C18 -179.4(5) . .
C2 C3 C4 C5 1.4(8) . .
C18 C3 C4 C5 -179.4(5) . .
C3 C4 C5 C6 -0.8(8) . .
C4 C5 C6 C1 -1.0(7) . .
C4 C5 C6 S3 174.2(4) . .
C2 C1 C6 C5 2.2(7) . .
C2 C1 C6 S3 -173.0(3) . .
O3 S3 C6 C5 -62.7(4) . .
C7 S3 C6 C5 52.7(4) . .
Pd1 S3 C6 C5 172.6(3) . .
O3 S3 C6 C1 112.7(4) . .
C7 S3 C6 C1 -131.9(4) . .
Pd1 S3 C6 C1 -12.1(4) . .
O3 S3 C7 C8 164.3(3) . .
C6 S3 C7 C8 48.0(4) . .
Pd1 S3 C7 C8 -71.7(4) . .
O3 S3 C7 C12 -22.2(3) . .
C6 S3 C7 C12 -138.4(3) . .
Pd1 S3 C7 C12 101.9(3) . .
C12 C7 C8 C9 0.5(6) . .
S3 C7 C8 C9 173.5(3) . .
C12 C7 C8 C8 -177.8(4) . 5
S3 C7 C8 C8 -4.8(6) . 5
C7 C8 C9 C16 179.6(4) . .
C8 C8 C9 C16 -2.1(7) 5 .
C7 C8 C9 C10 -0.8(6) . .
C8 C8 C9 C10 177.5(4) 5 .
C16 C9 C10 C13 0.5(7) . .
C8 C9 C10 C13 -179.1(5) . .
C16 C9 C10 C11 179.9(5) . .
C8 C9 C10 C11 0.3(7) . .
C13 C10 C11 C12 180.0(5) . .
C9 C10 C11 C12 0.6(8) . .
C10 C11 C12 C7 -0.9(7) . .
C8 C7 C12 C11 0.4(6) . .
S3 C7 C12 C11 -173.4(4) . .
C11 C10 C13 C14 178.9(6) . .
C9 C10 C13 C14 -1.7(9) . .
C10 C13 C14 C15 -0.1(11) . .
C13 C14 C15 C16 3.1(12) . .
C14 C15 C16 C9 -4.4(10) . .
C8 C9 C16 C15 -177.8(6) . .
C10 C9 C16 C15 2.6(8) . .
Pd1 O1 C17 O2 4.5(6) . .
Pd1 O1 C17 C19 -173.7(3) . .
O2 C17 C19 F3B -61.2(7) . .
O1 C17 C19 F3B 117.1(5) . .
O2 C17 C19 F1A 111.6(6) . .
O1 C17 C19 F1A -70.1(7) . .
O2 C17 C19 F2B 57.0(6) . .
O1 C17 C19 F2B -124.7(5) . .
O2 C17 C19 F3A -125.3(6) . .
O1 C17 C19 F3A 53.0(6) . .
O2 C17 C19 F1B 176.4(5) . .
O1 C17 C19 F1B -5.3(6) . .
O2 C17 C19 F2A -8.2(7) . .
O1 C17 C19 F2A 170.1(6) . .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.363 0.363 -0.000 170 91 ' '
2 -0.363 -0.000 0.333 170 91 ' '
3 -0.000 0.637 0.667 170 91 ' '
