# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2005

data_global
_journal_name_full               Chem.Commun.
_journal_coden_cambridge         0182

_publ_contact_author_name        'Dr Kilian Muniz'
_publ_contact_author_address     
;
Kekule-Institut fuer Organische Chemie
Bonn University
Gerhard-Domagk-Str. 1
Bonn
D-53121
GERMANY
;

_publ_contact_author_email       KILIAN.MUNIZ@UNI-BONN.DE

#==============================================================================

# 3. TITLE AND AUTHOR LIST

_publ_section_title              
;
First Direct Osmium-Catalysed Ketamination of Alkenes
;

loop_
_publ_author_name
_publ_author_address
'Villar, Amparo'
; Kekule-Institut fur Organische Chemie
Universitat Bonn
Gerhard-Domagk-Str. 1
D-53121 Bonn
Bundesrepublik Deutschland
;
'Hovelmann, Claas H.'
; Kekule-Institut fur Organische Chemie
Universitat Bonn
Gerhard-Domagk-Str. 1
D-53121 Bonn
Bundesrepublik Deutschland
;
'Nieger, Martin'
; Institut fur Anorganische Chemie
Universitat Bonn
Gerhard-Domagk-Str. 1
D-53121 Bonn
Bundesrepublik Deutschland
;
'Muniz, Kilian'
; Kekule-Institut fur Organische Chemie
Universitat Bonn
Gerhard-Domagk-Str. 1
D-53121 Bonn
Bundesrepublik Deutschland
;

#==============================================================================

data_mun020
_database_code_depnum_ccdc_archive 'CCDC 268052'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
2-(N-Tosyl)-amino-1,2-diphenyl-ethan-2-one
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H19 N O3 S'
_chemical_formula_sum            'C21 H19 N O3 S'
_chemical_formula_weight         365.43

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'
N N 0.0061 0.0033 '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   P2(1)/n
_symmetry_Int_Tables_number      14

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'

_cell_length_a                   12.6115(1)
_cell_length_b                   5.9741(1)
_cell_length_c                   24.2313(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.681(1)
_cell_angle_gamma                90.00
_cell_volume                     1787.83(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    4470
_cell_measurement_theta_min      1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       rods
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             768
_exptl_absorpt_coefficient_mu    0.202
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
dx = 40 mm, 60 sec./deg., 1 deg., 11 sets, 816 frames, mos.= 0.449(1) deg.
;

_diffrn_ambient_temperature      123(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  'Nonius KappaCCD'
_diffrn_measurement_method       'rotation in phi and omega, 1 deg.'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32585
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0209
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         3.30
_diffrn_reflns_theta_max         27.47
_reflns_number_total             4091
_reflns_number_gt                3599
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Collect
_computing_cell_refinement       DENZO-SMN
_computing_data_reduction        DENZO-SMN
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_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^)+(0.0496P)^2^+0.5839P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4091
_refine_ls_number_parameters     239
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0320
_refine_ls_wR_factor_ref         0.0906
_refine_ls_wR_factor_gt          0.0877
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.056
_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
O1 O 0.37546(7) 0.49277(15) 0.48338(4) 0.0244(2) Uani 1 1 d . . .
C1 C 0.31367(9) 0.3550(2) 0.49594(5) 0.0174(2) Uani 1 1 d . . .
C11 C 0.19576(9) 0.3648(2) 0.47053(5) 0.0178(2) Uani 1 1 d . . .
C12 C 0.12559(9) 0.1865(2) 0.47270(5) 0.0212(3) Uani 1 1 d . . .
H12 H 0.1524 0.0510 0.4908 0.025 Uiso 1 1 calc R . .
C13 C 0.01629(10) 0.2064(2) 0.44836(5) 0.0256(3) Uani 1 1 d . . .
H13 H -0.0313 0.0842 0.4496 0.031 Uiso 1 1 calc R . .
C14 C -0.02335(10) 0.4046(2) 0.42223(6) 0.0272(3) Uani 1 1 d . . .
H14 H -0.0984 0.4193 0.4065 0.033 Uiso 1 1 calc R . .
C15 C 0.04641(10) 0.5810(2) 0.41908(6) 0.0277(3) Uani 1 1 d . . .
H15 H 0.0193 0.7157 0.4006 0.033 Uiso 1 1 calc R . .
C16 C 0.15594(10) 0.5618(2) 0.44280(5) 0.0229(3) Uani 1 1 d . . .
H16 H 0.2037 0.6825 0.4402 0.027 Uiso 1 1 calc R . .
C2 C 0.35588(9) 0.17698(19) 0.54078(5) 0.0168(2) Uani 1 1 d . . .
H2 H 0.3303 0.0263 0.5257 0.020 Uiso 1 1 calc R . .
C21 C 0.31183(9) 0.2233(2) 0.59384(5) 0.0172(2) Uani 1 1 d . . .
C22 C 0.33489(10) 0.4251(2) 0.62265(5) 0.0212(3) Uani 1 1 d . . .
H22 H 0.3777 0.5350 0.6091 0.025 Uiso 1 1 calc R . .
C23 C 0.29535(11) 0.4657(2) 0.67110(6) 0.0268(3) Uani 1 1 d . . .
H23 H 0.3120 0.6028 0.6908 0.032 Uiso 1 1 calc R . .
C24 C 0.23159(11) 0.3075(2) 0.69104(6) 0.0290(3) Uani 1 1 d . . .
H24 H 0.2036 0.3374 0.7239 0.035 Uiso 1 1 calc R . .
C25 C 0.20899(10) 0.1057(2) 0.66280(6) 0.0271(3) Uani 1 1 d . . .
H25 H 0.1659 -0.0034 0.6764 0.033 Uiso 1 1 calc R . .
C26 C 0.24945(9) 0.0631(2) 0.61449(5) 0.0212(3) Uani 1 1 d . . .
H26 H 0.2345 -0.0759 0.5955 0.025 Uiso 1 1 calc R . .
N3 N 0.47377(8) 0.18465(17) 0.54959(4) 0.0182(2) Uani 1 1 d D . .
H3 H 0.5026(11) 0.294(2) 0.5361(6) 0.022 Uiso 1 1 d D . .
S3 S 0.55149(2) 0.02488(5) 0.593418(12) 0.01718(9) Uani 1 1 d . . .
O31 O 0.49434(7) -0.18010(15) 0.59710(4) 0.0243(2) Uani 1 1 d . . .
O32 O 0.65456(7) 0.02185(14) 0.57676(4) 0.02125(19) Uani 1 1 d . . .
C31 C 0.57214(9) 0.1551(2) 0.66020(5) 0.0190(2) Uani 1 1 d . . .
C32 C 0.62688(10) 0.3591(2) 0.66759(5) 0.0237(3) Uani 1 1 d . . .
H32 H 0.6539 0.4246 0.6375 0.028 Uiso 1 1 calc R . .
C33 C 0.64142(11) 0.4653(2) 0.71953(6) 0.0276(3) Uani 1 1 d . . .
H33 H 0.6793 0.6036 0.7249 0.033 Uiso 1 1 calc R . .
C34 C 0.60118(10) 0.3718(3) 0.76392(5) 0.0287(3) Uani 1 1 d . . .
C35 C 0.54760(11) 0.1673(3) 0.75552(6) 0.0306(3) Uani 1 1 d . . .
H35 H 0.5208 0.1010 0.7856 0.037 Uiso 1 1 calc R . .
C36 C 0.53263(10) 0.0582(2) 0.70373(5) 0.0254(3) Uani 1 1 d . . .
H36 H 0.4957 -0.0812 0.6984 0.030 Uiso 1 1 calc R . .
C37 C 0.61568(14) 0.4910(3) 0.81982(7) 0.0450(4) Uani 1 1 d . . .
H37A H 0.6806 0.4340 0.8452 0.068 Uiso 1 1 calc R . .
H37B H 0.5522 0.4643 0.8365 0.068 Uiso 1 1 calc R . .
H37C H 0.6236 0.6520 0.8141 0.068 Uiso 1 1 calc 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
O1 0.0183(4) 0.0256(5) 0.0287(5) 0.0080(4) 0.0031(4) -0.0051(3)
C1 0.0173(5) 0.0186(5) 0.0165(5) -0.0005(4) 0.0040(4) -0.0018(4)
C11 0.0164(5) 0.0215(6) 0.0158(5) 0.0008(4) 0.0037(4) -0.0004(4)
C12 0.0190(6) 0.0234(6) 0.0205(6) 0.0039(5) 0.0022(4) -0.0024(5)
C13 0.0184(6) 0.0318(7) 0.0258(6) 0.0051(5) 0.0025(5) -0.0062(5)
C14 0.0162(6) 0.0385(8) 0.0256(6) 0.0063(6) 0.0013(5) 0.0005(5)
C15 0.0236(6) 0.0287(7) 0.0296(7) 0.0095(5) 0.0026(5) 0.0044(5)
C16 0.0210(6) 0.0219(6) 0.0258(6) 0.0036(5) 0.0045(5) -0.0014(5)
C2 0.0141(5) 0.0181(5) 0.0177(5) 0.0003(4) 0.0019(4) -0.0023(4)
C21 0.0139(5) 0.0202(6) 0.0168(5) 0.0028(4) 0.0014(4) -0.0002(4)
C22 0.0208(6) 0.0199(6) 0.0225(6) 0.0012(5) 0.0030(5) -0.0012(5)
C23 0.0299(7) 0.0274(7) 0.0223(6) -0.0024(5) 0.0033(5) 0.0039(5)
C24 0.0284(6) 0.0405(8) 0.0191(6) 0.0037(5) 0.0075(5) 0.0065(6)
C25 0.0221(6) 0.0360(7) 0.0239(6) 0.0092(6) 0.0063(5) -0.0025(5)
C26 0.0180(5) 0.0233(6) 0.0212(6) 0.0035(5) 0.0012(4) -0.0031(5)
N3 0.0140(4) 0.0203(5) 0.0199(5) 0.0043(4) 0.0027(4) -0.0017(4)
S3 0.01647(15) 0.01668(15) 0.01769(16) 0.00065(10) 0.00176(11) -0.00055(10)
O31 0.0266(4) 0.0178(4) 0.0273(5) 0.0015(3) 0.0029(4) -0.0037(3)
O32 0.0171(4) 0.0243(4) 0.0219(4) -0.0015(3) 0.0029(3) 0.0022(3)
C31 0.0175(5) 0.0204(6) 0.0178(5) 0.0006(5) 0.0009(4) 0.0012(4)
C32 0.0244(6) 0.0240(6) 0.0230(6) -0.0007(5) 0.0057(5) -0.0028(5)
C33 0.0249(6) 0.0289(7) 0.0282(7) -0.0072(5) 0.0033(5) -0.0036(5)
C34 0.0207(6) 0.0429(8) 0.0208(6) -0.0056(6) 0.0001(5) 0.0025(6)
C35 0.0296(7) 0.0435(8) 0.0190(6) 0.0033(6) 0.0054(5) -0.0026(6)
C36 0.0244(6) 0.0285(7) 0.0230(6) 0.0038(5) 0.0042(5) -0.0027(5)
C37 0.0398(8) 0.0686(12) 0.0264(8) -0.0186(8) 0.0063(6) -0.0085(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
O1 C1 1.2136(14) . ?
C1 C11 1.4909(15) . ?
C1 C2 1.5366(16) . ?
C11 C12 1.3925(16) . ?
C11 C16 1.3972(17) . ?
C12 C13 1.3902(16) . ?
C12 H12 0.9500 . ?
C13 C14 1.3871(19) . ?
C13 H13 0.9500 . ?
C14 C15 1.3848(19) . ?
C14 H14 0.9500 . ?
C15 C16 1.3893(17) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C2 N3 1.4593(14) . ?
C2 C21 1.5258(16) . ?
C2 H2 1.0000 . ?
C21 C22 1.3939(17) . ?
C21 C26 1.3946(16) . ?
C22 C23 1.3866(19) . ?
C22 H22 0.9500 . ?
C23 C24 1.390(2) . ?
C23 H23 0.9500 . ?
C24 C25 1.387(2) . ?
C24 H24 0.9500 . ?
C25 C26 1.3918(19) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
N3 S3 1.6056(10) . ?
N3 H3 0.845(13) . ?
S3 O31 1.4329(9) . ?
S3 O32 1.4371(9) . ?
S3 C31 1.7668(12) . ?
C31 C36 1.3817(18) . ?
C31 C32 1.3940(17) . ?
C32 C33 1.3881(18) . ?
C32 H32 0.9500 . ?
C33 C34 1.395(2) . ?
C33 H33 0.9500 . ?
C34 C35 1.391(2) . ?
C34 C37 1.508(2) . ?
C35 C36 1.3926(19) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 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
O1 C1 C11 120.49(11) . . ?
O1 C1 C2 119.90(10) . . ?
C11 C1 C2 119.52(10) . . ?
C12 C11 C16 119.54(11) . . ?
C12 C11 C1 122.89(11) . . ?
C16 C11 C1 117.57(10) . . ?
C13 C12 C11 120.10(11) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C14 C13 C12 120.10(12) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C15 C14 C13 120.02(11) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C16 120.25(12) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C15 C16 C11 119.94(12) . . ?
C15 C16 H16 120.0 . . ?
C11 C16 H16 120.0 . . ?
N3 C2 C21 113.88(9) . . ?
N3 C2 C1 106.18(9) . . ?
C21 C2 C1 109.70(9) . . ?
N3 C2 H2 109.0 . . ?
C21 C2 H2 109.0 . . ?
C1 C2 H2 109.0 . . ?
C22 C21 C26 119.31(11) . . ?
C22 C21 C2 120.29(10) . . ?
C26 C21 C2 120.39(11) . . ?
C23 C22 C21 120.06(12) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C24 120.54(13) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 H23 119.7 . . ?
C25 C24 C23 119.68(12) . . ?
C25 C24 H24 120.2 . . ?
C23 C24 H24 120.2 . . ?
C24 C25 C26 120.02(12) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C25 C26 C21 120.38(12) . . ?
C25 C26 H26 119.8 . . ?
C21 C26 H26 119.8 . . ?
C2 N3 S3 123.07(8) . . ?
C2 N3 H3 118.2(10) . . ?
S3 N3 H3 117.6(10) . . ?
O31 S3 O32 120.11(5) . . ?
O31 S3 N3 107.57(5) . . ?
O32 S3 N3 106.71(5) . . ?
O31 S3 C31 107.58(6) . . ?
O32 S3 C31 106.78(5) . . ?
N3 S3 C31 107.52(6) . . ?
C36 C31 C32 120.94(12) . . ?
C36 C31 S3 120.36(10) . . ?
C32 C31 S3 118.68(9) . . ?
C33 C32 C31 119.14(12) . . ?
C33 C32 H32 120.4 . . ?
C31 C32 H32 120.4 . . ?
C32 C33 C34 120.94(13) . . ?
C32 C33 H33 119.5 . . ?
C34 C33 H33 119.5 . . ?
C35 C34 C33 118.71(12) . . ?
C35 C34 C37 120.86(14) . . ?
C33 C34 C37 120.43(14) . . ?
C34 C35 C36 121.07(13) . . ?
C34 C35 H35 119.5 . . ?
C36 C35 H35 119.5 . . ?
C31 C36 C35 119.19(13) . . ?
C31 C36 H36 120.4 . . ?
C35 C36 H36 120.4 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 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
O1 C1 C11 C12 164.62(12) . . . . ?
C2 C1 C11 C12 -18.78(17) . . . . ?
O1 C1 C11 C16 -14.39(18) . . . . ?
C2 C1 C11 C16 162.21(11) . . . . ?
C16 C11 C12 C13 -1.26(19) . . . . ?
C1 C11 C12 C13 179.75(12) . . . . ?
C11 C12 C13 C14 -0.5(2) . . . . ?
C12 C13 C14 C15 1.7(2) . . . . ?
C13 C14 C15 C16 -1.0(2) . . . . ?
C14 C15 C16 C11 -0.8(2) . . . . ?
C12 C11 C16 C15 1.89(19) . . . . ?
C1 C11 C16 C15 -179.06(12) . . . . ?
O1 C1 C2 N3 -13.26(15) . . . . ?
C11 C1 C2 N3 170.12(10) . . . . ?
O1 C1 C2 C21 110.22(12) . . . . ?
C11 C1 C2 C21 -66.40(13) . . . . ?
N3 C2 C21 C22 58.91(14) . . . . ?
C1 C2 C21 C22 -59.92(13) . . . . ?
N3 C2 C21 C26 -120.16(11) . . . . ?
C1 C2 C21 C26 121.01(11) . . . . ?
C26 C21 C22 C23 -0.43(17) . . . . ?
C2 C21 C22 C23 -179.50(11) . . . . ?
C21 C22 C23 C24 -0.73(19) . . . . ?
C22 C23 C24 C25 1.2(2) . . . . ?
C23 C24 C25 C26 -0.47(19) . . . . ?
C24 C25 C26 C21 -0.68(18) . . . . ?
C22 C21 C26 C25 1.12(17) . . . . ?
C2 C21 C26 C25 -179.80(11) . . . . ?
C21 C2 N3 S3 59.17(13) . . . . ?
C1 C2 N3 S3 179.99(8) . . . . ?
C2 N3 S3 O31 29.87(11) . . . . ?
C2 N3 S3 O32 160.00(9) . . . . ?
C2 N3 S3 C31 -85.74(10) . . . . ?
O31 S3 C31 C36 -1.52(12) . . . . ?
O32 S3 C31 C36 -131.71(10) . . . . ?
N3 S3 C31 C36 114.08(10) . . . . ?
O31 S3 C31 C32 179.82(9) . . . . ?
O32 S3 C31 C32 49.63(11) . . . . ?
N3 S3 C31 C32 -64.58(11) . . . . ?
C36 C31 C32 C33 -0.07(19) . . . . ?
S3 C31 C32 C33 178.58(10) . . . . ?
C31 C32 C33 C34 -0.6(2) . . . . ?
C32 C33 C34 C35 1.1(2) . . . . ?
C32 C33 C34 C37 -178.84(13) . . . . ?
C33 C34 C35 C36 -0.9(2) . . . . ?
C37 C34 C35 C36 179.05(14) . . . . ?
C32 C31 C36 C35 0.28(19) . . . . ?
S3 C31 C36 C35 -178.35(10) . . . . ?
C34 C35 C36 C31 0.2(2) . . . . ?

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
N3 H3 O1 0.845(13) 2.123(13) 2.9297(13) 159.7(13) 3_666
C22 H22 O31 0.95 2.31 3.2392(15) 167.2 1_565
C2 H2 O32 1.00 2.55 3.0640(14) 112.0 3_656
C37 H37A O32 0.98 2.57 3.4307(18) 147.2 2_656
C16 H16 O32 0.95 2.60 3.5472(15) 172.0 3_666
N3 H3 O1 0.845(13) 2.187(14) 2.5873(13) 108.9(11) .

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.044
#==============================================================================