# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2007


data_global
_journal_name_full               Chem.Commun.
_journal_coden_Cambridge         0182
_publ_contact_author             'Benjamin Davis'
_publ_contact_author_email       ben.davis@chem.ox.ac.uk

_publ_section_title              
; A trisulfide linked glycoprotein
;
_publ_contact_author_name        'Benjamin Davis'
loop_
_publ_author_name
G.L.Bernandes
J.Marston
'S.I.van Kasteren'
A.S.Batsanov
;
J.A.K.Howard
;
B.G.Davis
#===============================================================

data_(3)
_database_code_depnum_ccdc_archive 'CCDC 645866'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
2,3,4,6-Tetra-O-acetyl-\b-D-glucopyranosyl methanethiosulfonate
;
_chemical_name_common            
;2,3,4,6-Tetra-O-acetyl-beta-D-glucopyranosyl
methanethiosulfonate
;
_chemical_melting_point          423(2)
_chemical_formula_moiety         'C15 H22 O11 S2'
_chemical_formula_sum            'C15 H22 O11 S2'
_chemical_formula_weight         442.45
_chemical_absolute_configuration rmad
_chemical_optical_rotation       '[\a]~D~^27^ = -19 (c 1.24, CHCl~3~)'

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   8.7903(12)
_cell_length_b                   12.7736(17)
_cell_length_c                   9.6066(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.60(2)
_cell_angle_gamma                90.00
_cell_volume                     988.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    108(2)
_cell_measurement_reflns_used    845
_cell_measurement_theta_min      12.0
_cell_measurement_theta_max      25.3

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             464
_exptl_absorpt_coefficient_mu    0.325
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;The data collection nominally covered full sphere of reciprocal
space, by a combination of 4 runs of narrow-frame \w-scans (scan
width 0.3\% \w, 10s exposure), every run at a different \f angle.
Crystal to detector distance 4.53 cm. 2731 unique reflections after
merging Friedel equivalents.
;

_diffrn_ambient_temperature      108(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Siemens SMART 1K CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 8
_diffrn_standards_number         0
_diffrn_reflns_number            12148
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.31
_diffrn_reflns_theta_max         29.05
_reflns_number_total             5179
_reflns_number_gt                5038
_reflns_threshold_expression     I>2\s(I)
_reflns_Friedel_coverage         0.90

_computing_data_collection       'SMART version 5.060 (Bruker, 1999)'
_computing_cell_refinement       'SMART version 5.060 (Bruker, 1999)'
_computing_data_reduction        'SAINT version 6.02A (Bruker, 2001)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL version 6.14 (Bruker, 2003)'
_computing_publication_material  'SHELXTL version 6.14 (Bruker, 2003)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. Methyl groups
were refined as rigid bodies rotating around C---C bonds, with a common
refined U for three H atoms. Other H atoms: riding model.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0441P)^2^+0.1043P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(4)
_refine_ls_number_reflns         5179
_refine_ls_number_parameters     263
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0264
_refine_ls_wR_factor_ref         0.0688
_refine_ls_wR_factor_gt          0.0680
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
S1 S 0.28414(4) 0.34872(3) 0.81363(3) 0.01923(7) Uani 1 1 d . . .
S2 S 0.06556(4) 0.36922(2) 0.84538(4) 0.01947(8) Uani 1 1 d . . .
O1 O 0.14481(11) 0.37737(7) 0.51842(10) 0.01596(17) Uani 1 1 d . . .
O2 O 0.50028(12) 0.52882(7) 0.76942(11) 0.01781(19) Uani 1 1 d . . .
O3 O 0.54359(11) 0.52743(8) 0.49567(11) 0.01774(19) Uani 1 1 d . . .
O4 O 0.19751(12) 0.54680(8) 0.23579(10) 0.01714(18) Uani 1 1 d . . .
O6 O -0.17649(11) 0.36850(8) 0.25684(11) 0.01892(18) Uani 1 1 d . . .
O11 O 0.10295(15) 0.32162(10) 0.99107(12) 0.0289(2) Uani 1 1 d . . .
O12 O 0.01565(16) 0.47710(9) 0.82085(15) 0.0315(3) Uani 1 1 d . . .
O20 O 0.69179(14) 0.40388(9) 0.88366(13) 0.0269(2) Uani 1 1 d . . .
O30 O 0.51032(14) 0.69845(8) 0.42874(13) 0.0257(2) Uani 1 1 d . . .
O40 O 0.40543(14) 0.50775(9) 0.16276(12) 0.0242(2) Uani 1 1 d . . .
O60 O -0.14949(13) 0.20111(8) 0.33942(13) 0.0243(2) Uani 1 1 d . . .
C1 C 0.24347(16) 0.43350(10) 0.65143(14) 0.0152(2) Uani 1 1 d . . .
H1 H 0.1852 0.4985 0.6608 0.018 Uiso 1 1 d R . .
C2 C 0.41015(16) 0.46021(10) 0.64499(14) 0.0152(2) Uani 1 1 d . . .
H2 H 0.4754 0.3953 0.6496 0.018 Uiso 1 1 d R . .
C3 C 0.38235(16) 0.52245(10) 0.50120(15) 0.0149(2) Uani 1 1 d . . .
H3 H 0.3440 0.5947 0.5107 0.018 Uiso 1 1 d R . .
C4 C 0.25656(16) 0.47036(10) 0.35710(14) 0.0149(2) Uani 1 1 d . . .
H4 H 0.3069 0.4088 0.3274 0.018 Uiso 1 1 d R . .
C5 C 0.10087(16) 0.43812(10) 0.38220(14) 0.0149(2) Uani 1 1 d . . .
H5 H 0.0394 0.5021 0.3897 0.018 Uiso 1 1 d R . .
C6 C -0.01283(15) 0.36910(12) 0.25482(14) 0.0179(2) Uani 1 1 d . . .
H6A H -0.0192 0.3959 0.1560 0.022 Uiso 1 1 d R . .
H6B H 0.0317 0.2970 0.2681 0.022 Uiso 1 1 d R . .
C10 C -0.0851(2) 0.29375(14) 0.70247(18) 0.0281(3) Uani 1 1 d . . .
H10A H -0.1939 0.3050 0.7057 0.040(3) Uiso 1 1 d R . .
H10B H -0.0556 0.2195 0.7195 0.040(3) Uiso 1 1 d R . .
H10C H -0.0895 0.3149 0.6029 0.040(3) Uiso 1 1 d R . .
C20 C 0.64028(17) 0.49088(11) 0.88283(15) 0.0194(2) Uani 1 1 d . . .
C21 C 0.7138(2) 0.57264(13) 1.00338(18) 0.0303(3) Uani 1 1 d . . .
H21A H 0.6545 0.5729 1.0707 0.063(5) Uiso 1 1 d R . .
H21B H 0.7036 0.6415 0.9556 0.063(5) Uiso 1 1 d R . .
H21C H 0.8313 0.5569 1.0626 0.063(5) Uiso 1 1 d R . .
C30 C 0.59393(17) 0.62019(11) 0.45883(15) 0.0185(3) Uani 1 1 d . . .
C31 C 0.76435(18) 0.60824(13) 0.46095(19) 0.0248(3) Uani 1 1 d . . .
H31A H 0.7601 0.5604 0.3798 0.044(4) Uiso 1 1 d R . .
H31B H 0.8393 0.5798 0.5593 0.044(4) Uiso 1 1 d R . .
H31C H 0.8052 0.6767 0.4451 0.044(4) Uiso 1 1 d R . .
C40 C 0.28675(17) 0.56022(11) 0.14824(15) 0.0179(2) Uani 1 1 d . . .
C41 C 0.2206(2) 0.64938(12) 0.03972(17) 0.0244(3) Uani 1 1 d . . .
H41A H 0.2801 0.7137 0.0862 0.044(4) Uiso 1 1 d R . .
H41B H 0.1020 0.6583 0.0155 0.044(4) Uiso 1 1 d R . .
H41C H 0.2365 0.6346 -0.0537 0.044(4) Uiso 1 1 d R . .
C60 C -0.23138(16) 0.27938(11) 0.29680(14) 0.0169(2) Uani 1 1 d . . .
C61 C -0.40677(18) 0.29307(12) 0.28192(19) 0.0254(3) Uani 1 1 d . . .
H61A H -0.4555 0.2243 0.2838 0.057(4) Uiso 1 1 d R . .
H61B H -0.4719 0.3283 0.1857 0.057(4) Uiso 1 1 d R . .
H61C H -0.4075 0.3356 0.3666 0.057(4) Uiso 1 1 d R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.02178(14) 0.02070(16) 0.01648(13) 0.00348(11) 0.00899(11) -0.00017(12)
S2 0.02392(15) 0.01900(16) 0.01916(14) -0.00294(12) 0.01248(11) -0.00425(12)
O1 0.0185(4) 0.0155(4) 0.0140(4) 0.0009(3) 0.0065(3) -0.0028(3)
O2 0.0182(4) 0.0144(4) 0.0178(4) -0.0009(3) 0.0040(3) -0.0003(3)
O3 0.0141(4) 0.0164(4) 0.0240(4) 0.0026(4) 0.0089(4) -0.0007(3)
O4 0.0194(4) 0.0173(5) 0.0164(4) 0.0040(3) 0.0090(3) 0.0019(3)
O6 0.0150(4) 0.0186(4) 0.0235(4) 0.0028(4) 0.0081(3) 0.0002(4)
O11 0.0323(6) 0.0378(6) 0.0215(5) 0.0004(4) 0.0160(4) -0.0044(5)
O12 0.0335(6) 0.0226(5) 0.0462(7) -0.0025(5) 0.0243(5) -0.0012(5)
O20 0.0252(5) 0.0226(5) 0.0272(5) 0.0014(4) 0.0045(4) 0.0056(4)
O30 0.0271(5) 0.0177(5) 0.0365(6) 0.0042(4) 0.0174(5) 0.0000(4)
O40 0.0263(5) 0.0256(5) 0.0268(5) 0.0026(4) 0.0168(4) 0.0024(4)
O60 0.0241(5) 0.0171(5) 0.0309(5) 0.0013(4) 0.0103(4) 0.0017(4)
C1 0.0175(6) 0.0152(6) 0.0143(5) 0.0012(4) 0.0077(4) -0.0009(4)
C2 0.0161(6) 0.0134(5) 0.0161(5) 0.0004(4) 0.0063(4) -0.0004(4)
C3 0.0148(5) 0.0145(6) 0.0173(5) 0.0011(4) 0.0085(4) 0.0002(4)
C4 0.0158(6) 0.0148(5) 0.0154(5) 0.0020(4) 0.0077(4) 0.0005(4)
C5 0.0146(5) 0.0162(6) 0.0150(5) 0.0009(4) 0.0072(4) 0.0000(4)
C6 0.0154(5) 0.0227(6) 0.0174(5) -0.0008(5) 0.0084(4) -0.0013(5)
C10 0.0286(7) 0.0332(8) 0.0247(7) -0.0082(6) 0.0130(6) -0.0136(6)
C20 0.0184(6) 0.0190(6) 0.0194(6) 0.0029(5) 0.0061(5) -0.0009(5)
C21 0.0309(8) 0.0252(7) 0.0237(7) -0.0025(6) -0.0007(6) -0.0021(6)
C30 0.0193(6) 0.0177(6) 0.0198(6) -0.0006(5) 0.0092(5) -0.0034(5)
C31 0.0183(6) 0.0254(7) 0.0330(7) 0.0024(6) 0.0125(6) -0.0035(5)
C40 0.0221(6) 0.0173(6) 0.0162(5) -0.0011(5) 0.0097(5) -0.0036(5)
C41 0.0355(8) 0.0202(7) 0.0210(6) 0.0044(5) 0.0150(6) 0.0005(6)
C60 0.0172(6) 0.0174(6) 0.0154(5) -0.0018(4) 0.0057(5) -0.0020(5)
C61 0.0180(6) 0.0205(7) 0.0388(8) 0.0025(6) 0.0127(6) -0.0017(5)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C1 1.8118(13) . ?
S1 S2 2.0791(5) . ?
S2 O12 1.4367(12) . ?
S2 O11 1.4381(11) . ?
S2 C10 1.7641(16) . ?
O1 C1 1.4182(16) . ?
O1 C5 1.4350(15) . ?
O2 C20 1.3649(16) . ?
O2 C2 1.4375(15) . ?
O3 C30 1.3603(16) . ?
O3 C3 1.4408(15) . ?
O4 C40 1.3713(15) . ?
O4 C4 1.4480(15) . ?
O6 C60 1.3507(16) . ?
O6 C6 1.4466(15) . ?
O20 C20 1.1989(18) . ?
O30 C30 1.2053(18) . ?
O40 C40 1.2002(18) . ?
O60 C60 1.2038(18) . ?
C1 C2 1.5296(18) . ?
C1 H1 0.9989 . ?
C2 C3 1.5262(17) . ?
C2 H2 0.9989 . ?
C3 C4 1.5350(18) . ?
C3 H3 0.9989 . ?
C4 C5 1.5378(17) . ?
C4 H4 0.9989 . ?
C5 C6 1.5147(18) . ?
C5 H5 0.9989 . ?
C6 H6A 0.9888 . ?
C6 H6B 0.9889 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C20 C21 1.500(2) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C30 C31 1.498(2) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C40 C41 1.4956(19) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C60 C61 1.5005(19) . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?

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
_geom_angle_publ_flag
C1 S1 S2 100.09(5) . . ?
O12 S2 O11 120.06(7) . . ?
O12 S2 C10 108.16(9) . . ?
O11 S2 C10 109.52(8) . . ?
O12 S2 S1 109.65(5) . . ?
O11 S2 S1 103.00(5) . . ?
C10 S2 S1 105.48(6) . . ?
C1 O1 C5 113.11(9) . . ?
C20 O2 C2 117.90(10) . . ?
C30 O3 C3 118.38(10) . . ?
C40 O4 C4 117.98(10) . . ?
C60 O6 C6 118.59(11) . . ?
O1 C1 C2 109.06(10) . . ?
O1 C1 S1 108.16(8) . . ?
C2 C1 S1 107.80(9) . . ?
O1 C1 H1 110.5 . . ?
C2 C1 H1 110.6 . . ?
S1 C1 H1 110.6 . . ?
O2 C2 C3 105.68(10) . . ?
O2 C2 C1 108.68(10) . . ?
C3 C2 C1 110.11(10) . . ?
O2 C2 H2 110.7 . . ?
C3 C2 H2 110.7 . . ?
C1 C2 H2 110.8 . . ?
O3 C3 C2 104.65(10) . . ?
O3 C3 C4 110.49(10) . . ?
C2 C3 C4 112.76(10) . . ?
O3 C3 H3 109.6 . . ?
C2 C3 H3 109.6 . . ?
C4 C3 H3 109.6 . . ?
O4 C4 C3 109.28(10) . . ?
O4 C4 C5 104.60(10) . . ?
C3 C4 C5 109.86(10) . . ?
O4 C4 H4 111.0 . . ?
C3 C4 H4 110.9 . . ?
C5 C4 H4 111.0 . . ?
O1 C5 C6 105.76(10) . . ?
O1 C5 C4 110.87(10) . . ?
C6 C5 C4 111.71(10) . . ?
O1 C5 H5 109.4 . . ?
C6 C5 H5 109.5 . . ?
C4 C5 H5 109.5 . . ?
O6 C6 C5 109.29(10) . . ?
O6 C6 H6A 109.9 . . ?
C5 C6 H6A 109.9 . . ?
O6 C6 H6B 109.7 . . ?
C5 C6 H6B 109.8 . . ?
H6A C6 H6B 108.3 . . ?
S2 C10 H10A 109.5 . . ?
S2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
S2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O20 C20 O2 123.50(13) . . ?
O20 C20 C21 126.55(13) . . ?
O2 C20 C21 109.94(12) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O30 C30 O3 123.65(12) . . ?
O30 C30 C31 126.75(13) . . ?
O3 C30 C31 109.60(11) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O40 C40 O4 122.89(13) . . ?
O40 C40 C41 125.69(13) . . ?
O4 C40 C41 111.38(12) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O60 C60 O6 124.31(12) . . ?
O60 C60 C61 125.51(13) . . ?
O6 C60 C61 110.18(12) . . ?
C60 C61 H61A 109.5 . . ?
C60 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C60 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 S1 S2 O12 -39.51(7) . . . . ?
C1 S1 S2 O11 -168.43(7) . . . . ?
C1 S1 S2 C10 76.74(8) . . . . ?
C5 O1 C1 C2 -64.57(13) . . . . ?
C5 O1 C1 S1 178.44(8) . . . . ?
S2 S1 C1 O1 -82.23(8) . . . . ?
S2 S1 C1 C2 159.98(8) . . . . ?
C20 O2 C2 C3 -130.04(11) . . . . ?
C20 O2 C2 C1 111.79(12) . . . . ?
O1 C1 C2 O2 172.36(9) . . . . ?
S1 C1 C2 O2 -70.44(11) . . . . ?
O1 C1 C2 C3 57.03(13) . . . . ?
S1 C1 C2 C3 174.24(8) . . . . ?
C30 O3 C3 C2 -136.56(11) . . . . ?
C30 O3 C3 C4 101.80(13) . . . . ?
O2 C2 C3 O3 72.03(12) . . . . ?
C1 C2 C3 O3 -170.77(10) . . . . ?
O2 C2 C3 C4 -167.84(10) . . . . ?
C1 C2 C3 C4 -50.64(14) . . . . ?
C40 O4 C4 C3 87.36(13) . . . . ?
C40 O4 C4 C5 -155.06(11) . . . . ?
O3 C3 C4 O4 -81.28(12) . . . . ?
C2 C3 C4 O4 162.00(10) . . . . ?
O3 C3 C4 C5 164.50(10) . . . . ?
C2 C3 C4 C5 47.79(14) . . . . ?
C1 O1 C5 C6 -176.13(10) . . . . ?
C1 O1 C5 C4 62.60(13) . . . . ?
O4 C4 C5 O1 -169.04(9) . . . . ?
C3 C4 C5 O1 -51.86(14) . . . . ?
O4 C4 C5 C6 73.26(13) . . . . ?
C3 C4 C5 C6 -169.56(11) . . . . ?
C60 O6 C6 C5 -111.08(13) . . . . ?
O1 C5 C6 O6 77.35(12) . . . . ?
C4 C5 C6 O6 -161.92(10) . . . . ?
C2 O2 C20 O20 0.2(2) . . . . ?
C2 O2 C20 C21 -178.55(12) . . . . ?
C3 O3 C30 O30 -0.9(2) . . . . ?
C3 O3 C30 C31 179.54(11) . . . . ?
C4 O4 C40 O40 4.09(19) . . . . ?
C4 O4 C40 C41 -173.84(11) . . . . ?
C6 O6 C60 O60 4.33(19) . . . . ?
C6 O6 C60 C61 -176.34(11) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        29.05
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.189
_refine_diff_density_rms         0.048

#====================================END

data_(4)
_database_code_depnum_ccdc_archive 'CCDC 645867'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H22 O11 S3'
_chemical_formula_sum            'C15 H22 O11 S3'
_chemical_formula_weight         474.51
_chemical_absolute_configuration rmad
_chemical_optical_rotation       ?

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   5.6609(6)
_cell_length_b                   20.850(2)
_cell_length_c                   9.2785(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.45(3)
_cell_angle_gamma                90.00
_cell_volume                     1055.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    987
_cell_measurement_theta_min      12
_cell_measurement_theta_max      26

_exptl_crystal_description       wedge
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             496
_exptl_absorpt_coefficient_mu    0.405
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7441
_exptl_absorpt_correction_T_max  0.8944
_exptl_absorpt_process_details   
'SADABS (G.M.Sheldrick, 1998), R(int)=0.042 before correction'

_exptl_special_details           
;The data collection nominally covered full sphere of reciprocal
space, by a combination of 4 runs of narrow-frame \w-scans (scan
width 0.3\% \w, 10s exposure), every run at a different \f angle.
Crystal to detector distance 4.41 cm. 2886 unique reflections after
merging Friedel equivalents.
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Siemens SMART 1K CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 8
_diffrn_standards_number         0
_diffrn_reflns_number            11166
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         29.09
_reflns_number_total             5291
_reflns_number_gt                5119
_reflns_threshold_expression     I>2\s(I)
_reflns_Friedel_coverage         0.83

_computing_data_collection       'SMART version 5.060 (Bruker, 1999)'
_computing_cell_refinement       'SMART version 5.060 (Bruker, 1999)'
_computing_data_reduction        'SAINT version 6.02A (Bruker, 2001)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL version 6.14 (Bruker, 2003)'
_computing_publication_material  'SHELXTL version 6.14 (Bruker, 2003)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. Methyl groups
were refined as rigid bodies rotating around C---C bonds, with a common
refined U for three H atoms. Other H atoms: riding model.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+0.1885P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.07(4)
_refine_ls_number_reflns         5291
_refine_ls_number_parameters     272
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0275
_refine_ls_wR_factor_ref         0.0701
_refine_ls_wR_factor_gt          0.0693
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
S1 S 0.51131(7) 0.199262(19) 0.59061(4) 0.01954(8) Uani 1 1 d . . .
S2 S 0.12989(8) 0.09608(2) 0.65080(5) 0.02264(9) Uani 1 1 d . . .
S3 S 0.17829(8) 0.16173(2) 0.48987(4) 0.02343(9) Uani 1 1 d . . .
O1 O 0.3072(2) 0.31251(6) 0.55824(12) 0.0188(2) Uani 1 1 d . . .
O2 O 0.7356(2) 0.25950(6) 0.90190(12) 0.0186(2) Uani 1 1 d . . .
O3 O 0.8359(2) 0.39773(6) 0.89019(12) 0.0182(2) Uani 1 1 d . . .
O4 O 0.3772(2) 0.46668(6) 0.74485(13) 0.0199(2) Uani 1 1 d . . .
O6 O -0.1535(2) 0.37404(6) 0.42078(13) 0.0230(2) Uani 1 1 d . . .
O11 O 0.1617(3) 0.12765(8) 0.79233(17) 0.0389(4) Uani 1 1 d . . .
O12 O -0.1032(2) 0.06699(7) 0.57990(18) 0.0333(3) Uani 1 1 d . . .
O20 O 1.1344(2) 0.27922(7) 0.91889(13) 0.0239(2) Uani 1 1 d . . .
O30 O 0.6883(2) 0.44831(7) 1.06209(14) 0.0278(3) Uani 1 1 d . . .
O40 O 0.6935(3) 0.52119(7) 0.69931(17) 0.0342(3) Uani 1 1 d . . .
O60 O -0.0152(2) 0.33375(7) 0.23203(14) 0.0280(3) Uani 1 1 d . . .
C1 C 0.4238(3) 0.27070(7) 0.67608(16) 0.0158(3) Uani 1 1 d . . .
H1 H 0.3093 0.2592 0.7371 0.019 Uiso 1 1 d R . .
C2 C 0.6570(3) 0.30119(7) 0.77514(16) 0.0157(3) Uani 1 1 d . . .
H2 H 0.7857 0.3037 0.7199 0.019 Uiso 1 1 d R . .
C3 C 0.6022(3) 0.36800(8) 0.82529(16) 0.0164(3) Uani 1 1 d . . .
H3 H 0.5081 0.3645 0.9018 0.020 Uiso 1 1 d R . .
C4 C 0.4583(3) 0.40779(8) 0.69325(17) 0.0169(3) Uani 1 1 d . . .
H4 H 0.5611 0.4169 0.6235 0.020 Uiso 1 1 d R . .
C5 C 0.2288(3) 0.37077(8) 0.61262(17) 0.0171(3) Uani 1 1 d . . .
H5 H 0.1288 0.3608 0.6835 0.021 Uiso 1 1 d R . .
C6 C 0.0758(3) 0.40702(9) 0.47955(19) 0.0236(3) Uani 1 1 d . . .
H61 H 0.0445 0.4509 0.5099 0.031 Uiso 1 1 d R . .
H62 H 0.1649 0.4102 0.4017 0.031 Uiso 1 1 d R . .
C10 C 0.3661(3) 0.03996(9) 0.6660(2) 0.0268(4) Uani 1 1 d . . .
H101 H 0.5250 0.0616 0.7003 0.039(4) Uiso 1 1 d R . .
H102 H 0.3523 0.0203 0.5682 0.039(4) Uiso 1 1 d R . .
H103 H 0.3532 0.0067 0.7380 0.039(4) Uiso 1 1 d R . .
C20 C 0.9803(3) 0.25067(8) 0.96106(18) 0.0195(3) Uani 1 1 d . . .
C21 C 1.0271(3) 0.20009(10) 1.07924(19) 0.0271(3) Uani 1 1 d . . .
H211 H 1.0388 0.1582 1.0339 0.063(5) Uiso 1 1 d R . .
H212 H 0.8921 0.1995 1.1269 0.063(5) Uiso 1 1 d R . .
H213 H 1.1810 0.2094 1.1545 0.063(5) Uiso 1 1 d R . .
C30 C 0.8553(3) 0.43716(8) 1.00866(18) 0.0205(3) Uani 1 1 d . . .
C31 C 1.1071(3) 0.46463(11) 1.0594(2) 0.0313(4) Uani 1 1 d . . .
H311 H 1.1110 0.4977 1.1351 0.069(6) Uiso 1 1 d R . .
H312 H 1.1520 0.4838 0.9739 0.069(6) Uiso 1 1 d R . .
H313 H 1.2237 0.4305 1.1024 0.069(6) Uiso 1 1 d R . .
C40 C 0.5099(3) 0.52035(9) 0.74058(19) 0.0242(3) Uani 1 1 d . . .
C41 C 0.3977(4) 0.57709(9) 0.7974(2) 0.0344(4) Uani 1 1 d . . .
H411 H 0.4631 0.5801 0.9062 0.052(5) Uiso 1 1 d R . .
H412 H 0.2194 0.5718 0.7725 0.052(5) Uiso 1 1 d R . .
H413 H 0.4374 0.6163 0.7507 0.052(5) Uiso 1 1 d R . .
C60 C -0.1727(3) 0.33751(8) 0.29660(17) 0.0209(3) Uani 1 1 d . . .
C61 C -0.4138(3) 0.30356(11) 0.2527(2) 0.0315(4) Uani 1 1 d . . .
H611 H -0.4477 0.2896 0.1483 0.067(6) Uiso 1 1 d R . .
H612 H -0.5436 0.3327 0.2638 0.067(6) Uiso 1 1 d R . .
H613 H -0.4084 0.2661 0.3172 0.067(6) Uiso 1 1 d R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
S1 0.02243(17) 0.01496(17) 0.02224(17) -0.00232(15) 0.00770(13) -0.00005(14)
S2 0.02502(19) 0.01821(19) 0.02644(19) -0.00285(16) 0.00992(15) -0.00266(15)
S3 0.0288(2) 0.01582(18) 0.02109(17) -0.00056(15) -0.00133(14) -0.00181(15)
O1 0.0225(5) 0.0150(5) 0.0170(5) -0.0011(4) 0.0020(4) 0.0006(4)
O2 0.0182(5) 0.0195(6) 0.0180(5) 0.0029(4) 0.0044(4) 0.0000(4)
O3 0.0154(5) 0.0206(6) 0.0182(5) -0.0041(4) 0.0037(4) -0.0037(4)
O4 0.0238(5) 0.0136(5) 0.0222(5) -0.0024(4) 0.0061(4) -0.0004(4)
O6 0.0194(5) 0.0259(6) 0.0208(5) -0.0035(5) 0.0003(4) 0.0021(5)
O11 0.0566(10) 0.0341(8) 0.0322(7) -0.0089(6) 0.0227(7) -0.0076(7)
O12 0.0251(6) 0.0234(7) 0.0526(9) -0.0061(6) 0.0127(6) -0.0034(5)
O20 0.0193(5) 0.0303(7) 0.0225(6) -0.0003(5) 0.0063(4) 0.0015(5)
O30 0.0229(6) 0.0336(7) 0.0268(6) -0.0118(5) 0.0062(5) -0.0016(5)
O40 0.0382(8) 0.0245(7) 0.0424(8) 0.0021(6) 0.0149(6) -0.0086(6)
O60 0.0230(6) 0.0361(8) 0.0255(6) -0.0015(5) 0.0076(5) -0.0017(5)
C1 0.0178(6) 0.0133(7) 0.0166(6) -0.0017(6) 0.0048(5) -0.0005(5)
C2 0.0154(6) 0.0157(7) 0.0158(6) -0.0001(5) 0.0038(5) -0.0013(5)
C3 0.0152(6) 0.0172(7) 0.0161(6) -0.0010(5) 0.0029(5) -0.0035(5)
C4 0.0186(7) 0.0146(7) 0.0175(6) -0.0016(6) 0.0049(5) -0.0020(5)
C5 0.0183(7) 0.0149(7) 0.0172(6) -0.0016(6) 0.0032(5) -0.0002(5)
C6 0.0246(8) 0.0174(8) 0.0239(7) 0.0017(6) -0.0020(6) -0.0011(6)
C10 0.0251(8) 0.0247(9) 0.0308(9) 0.0094(7) 0.0076(7) 0.0034(7)
C20 0.0201(7) 0.0201(8) 0.0172(7) -0.0021(6) 0.0031(6) 0.0027(6)
C21 0.0285(8) 0.0269(8) 0.0234(7) 0.0038(7) 0.0023(6) 0.0062(7)
C30 0.0212(7) 0.0200(8) 0.0187(7) -0.0029(6) 0.0027(6) -0.0037(6)
C31 0.0234(8) 0.0396(11) 0.0301(9) -0.0113(8) 0.0057(7) -0.0129(8)
C40 0.0326(9) 0.0158(7) 0.0210(7) 0.0017(6) 0.0018(6) -0.0036(7)
C41 0.0470(11) 0.0159(8) 0.0380(10) -0.0048(8) 0.0073(9) 0.0000(8)
C60 0.0219(7) 0.0211(8) 0.0175(7) 0.0020(6) 0.0017(6) 0.0004(6)
C61 0.0241(8) 0.0467(12) 0.0231(8) -0.0066(8) 0.0052(7) -0.0095(8)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C1 1.8170(15) . ?
S1 S3 2.0252(7) . ?
S2 O11 1.4367(15) . ?
S2 O12 1.4421(14) . ?
S2 C10 1.7542(19) . ?
S2 S3 2.0967(6) . ?
O1 C1 1.4165(19) . ?
O1 C5 1.4306(19) . ?
O2 C20 1.3598(19) . ?
O2 C2 1.4346(19) . ?
O3 C30 1.354(2) . ?
O3 C3 1.4396(18) . ?
O4 C40 1.354(2) . ?
O4 C4 1.4370(19) . ?
O6 C60 1.361(2) . ?
O6 C6 1.442(2) . ?
O20 C20 1.204(2) . ?
O30 C30 1.201(2) . ?
O40 C40 1.199(2) . ?
O60 C60 1.202(2) . ?
C1 C2 1.531(2) . ?
C1 H1 0.9972 . ?
C2 C3 1.527(2) . ?
C2 H2 0.9972 . ?
C3 C4 1.523(2) . ?
C3 H3 0.9972 . ?
C4 C5 1.525(2) . ?
C4 H4 0.9972 . ?
C5 C6 1.509(2) . ?
C5 H5 0.9972 . ?
C6 H61 0.9874 . ?
C6 H62 0.9872 . ?
C10 H101 0.9800 . ?
C10 H102 0.9800 . ?
C10 H103 0.9800 . ?
C20 C21 1.493(2) . ?
C21 H211 0.9800 . ?
C21 H212 0.9800 . ?
C21 H213 0.9800 . ?
C30 C31 1.491(2) . ?
C31 H311 0.9800 . ?
C31 H312 0.9800 . ?
C31 H313 0.9800 . ?
C40 C41 1.503(3) . ?
C41 H411 0.9800 . ?
C41 H412 0.9800 . ?
C41 H413 0.9800 . ?
C60 C61 1.495(2) . ?
C61 H611 0.9800 . ?
C61 H612 0.9800 . ?
C61 H613 0.9800 . ?

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
_geom_angle_publ_flag
C1 S1 S3 100.94(5) . . ?
O11 S2 O12 119.10(9) . . ?
O11 S2 C10 108.95(10) . . ?
O12 S2 C10 109.98(9) . . ?
O11 S2 S3 110.09(7) . . ?
O12 S2 S3 103.12(7) . . ?
C10 S2 S3 104.55(7) . . ?
S1 S3 S2 101.87(3) . . ?
C1 O1 C5 112.02(11) . . ?
C20 O2 C2 118.22(13) . . ?
C30 O3 C3 117.90(12) . . ?
C40 O4 C4 117.86(13) . . ?
C60 O6 C6 116.59(14) . . ?
O1 C1 C2 110.96(12) . . ?
O1 C1 S1 107.02(10) . . ?
C2 C1 S1 108.09(10) . . ?
O1 C1 H1 110.2 . . ?
C2 C1 H1 110.2 . . ?
S1 C1 H1 110.2 . . ?
O2 C2 C3 110.29(12) . . ?
O2 C2 C1 105.66(12) . . ?
C3 C2 C1 110.42(12) . . ?
O2 C2 H2 110.1 . . ?
C3 C2 H2 110.1 . . ?
C1 C2 H2 110.2 . . ?
O3 C3 C4 109.68(13) . . ?
O3 C3 C2 106.36(12) . . ?
C4 C3 C2 111.12(12) . . ?
O3 C3 H3 109.9 . . ?
C4 C3 H3 109.9 . . ?
C2 C3 H3 109.9 . . ?
O4 C4 C3 110.32(12) . . ?
O4 C4 C5 106.84(12) . . ?
C3 C4 C5 108.79(12) . . ?
O4 C4 H4 110.3 . . ?
C3 C4 H4 110.3 . . ?
C5 C4 H4 110.3 . . ?
O1 C5 C6 107.53(13) . . ?
O1 C5 C4 107.39(12) . . ?
C6 C5 C4 112.10(14) . . ?
O1 C5 H5 109.9 . . ?
C6 C5 H5 109.9 . . ?
C4 C5 H5 109.9 . . ?
O6 C6 C5 109.47(14) . . ?
O6 C6 H61 109.8 . . ?
C5 C6 H61 109.8 . . ?
O6 C6 H62 109.8 . . ?
C5 C6 H62 109.8 . . ?
H61 C6 H62 108.2 . . ?
S2 C10 H101 109.5 . . ?
S2 C10 H102 109.5 . . ?
H101 C10 H102 109.5 . . ?
S2 C10 H103 109.5 . . ?
H101 C10 H103 109.5 . . ?
H102 C10 H103 109.5 . . ?
O20 C20 O2 123.39(15) . . ?
O20 C20 C21 125.83(15) . . ?
O2 C20 C21 110.74(14) . . ?
C20 C21 H211 109.5 . . ?
C20 C21 H212 109.5 . . ?
H211 C21 H212 109.5 . . ?
C20 C21 H213 109.5 . . ?
H211 C21 H213 109.5 . . ?
H212 C21 H213 109.5 . . ?
O30 C30 O3 123.38(15) . . ?
O30 C30 C31 125.92(16) . . ?
O3 C30 C31 110.69(15) . . ?
C30 C31 H311 109.5 . . ?
C30 C31 H312 109.5 . . ?
H311 C31 H312 109.5 . . ?
C30 C31 H313 109.5 . . ?
H311 C31 H313 109.5 . . ?
H312 C31 H313 109.5 . . ?
O40 C40 O4 123.77(17) . . ?
O40 C40 C41 125.71(18) . . ?
O4 C40 C41 110.51(16) . . ?
C40 C41 H411 109.5 . . ?
C40 C41 H412 109.5 . . ?
H411 C41 H412 109.5 . . ?
C40 C41 H413 109.5 . . ?
H411 C41 H413 109.5 . . ?
H412 C41 H413 109.5 . . ?
O60 C60 O6 123.80(16) . . ?
O60 C60 C61 125.31(16) . . ?
O6 C60 C61 110.89(14) . . ?
C60 C61 H611 109.5 . . ?
C60 C61 H612 109.5 . . ?
H611 C61 H612 109.5 . . ?
C60 C61 H613 109.5 . . ?
H611 C61 H613 109.5 . . ?
H612 C61 H613 109.5 . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 S1 S3 S2 -94.94(5) . . . . ?
O11 S2 S3 S1 53.69(8) . . . . ?
O12 S2 S3 S1 -178.22(6) . . . . ?
C10 S2 S3 S1 -63.20(7) . . . . ?
C5 O1 C1 C2 -62.53(15) . . . . ?
C5 O1 C1 S1 179.75(10) . . . . ?
S3 S1 C1 O1 -67.51(10) . . . . ?
S3 S1 C1 C2 172.91(9) . . . . ?
C20 O2 C2 C3 -97.26(15) . . . . ?
C20 O2 C2 C1 143.40(13) . . . . ?
O1 C1 C2 O2 170.99(12) . . . . ?
S1 C1 C2 O2 -71.95(13) . . . . ?
O1 C1 C2 C3 51.74(16) . . . . ?
S1 C1 C2 C3 168.80(10) . . . . ?
C30 O3 C3 C4 95.18(16) . . . . ?
C30 O3 C3 C2 -144.57(13) . . . . ?
O2 C2 C3 O3 75.25(14) . . . . ?
C1 C2 C3 O3 -168.35(12) . . . . ?
O2 C2 C3 C4 -165.44(12) . . . . ?
C1 C2 C3 C4 -49.04(16) . . . . ?
C40 O4 C4 C3 98.97(15) . . . . ?
C40 O4 C4 C5 -142.93(13) . . . . ?
O3 C3 C4 O4 -71.20(15) . . . . ?
C2 C3 C4 O4 171.49(12) . . . . ?
O3 C3 C4 C5 171.91(12) . . . . ?
C2 C3 C4 C5 54.60(16) . . . . ?
C1 O1 C5 C6 -171.79(13) . . . . ?
C1 O1 C5 C4 67.39(15) . . . . ?
O4 C4 C5 O1 178.95(12) . . . . ?
C3 C4 C5 O1 -61.96(15) . . . . ?
O4 C4 C5 C6 61.05(16) . . . . ?
C3 C4 C5 C6 -179.86(14) . . . . ?
C60 O6 C6 C5 -101.09(16) . . . . ?
O1 C5 C6 O6 70.10(16) . . . . ?
C4 C5 C6 O6 -172.09(13) . . . . ?
C2 O2 C20 O20 5.0(2) . . . . ?
C2 O2 C20 C21 -173.10(14) . . . . ?
C3 O3 C30 O30 0.2(2) . . . . ?
C3 O3 C30 C31 -178.86(14) . . . . ?
C4 O4 C40 O40 -1.6(2) . . . . ?
C4 O4 C40 C41 179.60(14) . . . . ?
C6 O6 C60 O60 -3.1(2) . . . . ?
C6 O6 C60 C61 177.07(15) . . . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        29.09
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.046