# Supplementary Material (ESI) for Organic & Biomolecular Chemistry
# This journal is (c) The Royal Society of Chemistry 2009


data_global
_journal_name_full               Org.Biomol.Chem.

_journal_coden_Cambridge         0177
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Xuewei Liu'
_publ_contact_author_email       XUEWEI@NTU.EDU.SG

_publ_section_title              
;
Highly stereoselective synthesis of aminoglycosides
via rhodium-catalyzed and substrate-controlled aziridination of glycals
;
loop_
_publ_author_name
'Xuewei Liu.'
'Jer-Lai Kuo.'
'Rujee Lorpitthaya'
'K. B. Sophy'

# Attachment 'compund10.cif'

data_liu16
_database_code_depnum_ccdc_archive 'CCDC 708553'

_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;

?

;

_chemical_absolute_configuration ad

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         ?

_chemical_formula_sum            'C26 H24 N O5.50 S'

_chemical_formula_weight         470.52

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   C2

loop_

_symmetry_equiv_pos_as_xyz

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

_cell_length_a                   28.5943(12)

_cell_length_b                   9.1264(4)

_cell_length_c                   9.5011(4)

_cell_angle_alpha                90.00

_cell_angle_beta                 90.748(2)

_cell_angle_gamma                90.00

_cell_volume                     2479.22(18)

_cell_formula_units_Z            4

_cell_measurement_temperature    223(2)

_cell_measurement_reflns_used    5484

_cell_measurement_theta_min      2.34

_cell_measurement_theta_max      24.69

_exptl_crystal_description       block

_exptl_crystal_colour            colourless

_exptl_crystal_size_max          0.28

_exptl_crystal_size_mid          0.24

_exptl_crystal_size_min          0.20

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.261

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             988

_exptl_absorpt_coefficient_mu    0.168

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.9543

_exptl_absorpt_correction_T_max  0.9671

_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;

?

;

_diffrn_ambient_temperature      223(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  'CCD area detector'

_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean ?

_diffrn_standards_number         ?

_diffrn_standards_interval_count ?

_diffrn_standards_interval_time  ?

_diffrn_standards_decay_%        ?

_diffrn_reflns_number            14828

_diffrn_reflns_av_R_equivalents  0.0459

_diffrn_reflns_av_sigmaI/netI    0.0532

_diffrn_reflns_limit_h_min       -36

_diffrn_reflns_limit_h_max       36

_diffrn_reflns_limit_k_min       -11

_diffrn_reflns_limit_k_max       11

_diffrn_reflns_limit_l_min       -12

_diffrn_reflns_limit_l_max       12

_diffrn_reflns_theta_min         2.14

_diffrn_reflns_theta_max         27.15

_reflns_number_total             5416

_reflns_number_gt                4479

_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'

_computing_cell_refinement       'Bruker SMART'

_computing_data_reduction        'Bruker SAINT'

_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

_computing_molecular_graphics    'Bruker SHELXTL'

_computing_publication_material  'Bruker SHELXTL'

_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.

Following restraints were used for the refinement of the solvent molecle:

DFIX 1.54 0.01 C27 C26

DFIX 1.45 0.01 C27 O6

ISOR 0.05 C27 C26

;

_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^)+(0.1357P)^2^+0.9935P] 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   0.02(12)

_refine_ls_number_reflns         5416

_refine_ls_number_parameters     316

_refine_ls_number_restraints     15

_refine_ls_R_factor_all          0.0814

_refine_ls_R_factor_gt           0.0700

_refine_ls_wR_factor_ref         0.2216

_refine_ls_wR_factor_gt          0.2025

_refine_ls_goodness_of_fit_ref   1.103

_refine_ls_restrained_S_all      1.108

_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

C1 C 0.6421(2) 0.6653(7) 1.1953(5) 0.0799(16) Uani 1 1 d . . .
H1 H 0.6187 0.6233 1.2511 0.096 Uiso 1 1 calc R . .
C2 C 0.6857(2) 0.6320(7) 1.2281(5) 0.090(2) Uani 1 1 d . . .
H2 H 0.6929 0.5708 1.3049 0.108 Uiso 1 1 calc R . .
C3 C 0.72180(19) 0.6922(5) 1.1425(4) 0.0596(11) Uani 1 1 d . . .
C4 C 0.70536(13) 0.7505(4) 1.0021(3) 0.0428(8) Uani 1 1 d . . .
H4 H 0.6988 0.6684 0.9368 0.051 Uiso 1 1 calc R . .
C5 C 0.66218(14) 0.8428(4) 1.0196(3) 0.0450(8) Uani 1 1 d . . .
H5 H 0.6701 0.9270 1.0811 0.054 Uiso 1 1 calc R . .
C6 C 0.64079(13) 0.9001(4) 0.8848(3) 0.0428(7) Uani 1 1 d . . .
H6A H 0.6108 0.9476 0.9038 0.051 Uiso 1 1 calc R . .
H6B H 0.6616 0.9723 0.8420 0.051 Uiso 1 1 calc R . .
C7 C 0.61028(11) 0.8119(3) 0.6605(3) 0.0355(6) Uani 1 1 d . . .
C8 C 0.64270(12) 0.8955(4) 0.5615(3) 0.0406(7) Uani 1 1 d . . .
C9 C 0.62527(14) 0.9670(4) 0.4420(4) 0.0458(8) Uani 1 1 d . . .
H9 H 0.5929 0.9666 0.4236 0.055 Uiso 1 1 calc R . .
C10 C 0.65485(19) 1.0390(5) 0.3497(4) 0.0625(12) Uani 1 1 d . . .
H10 H 0.6423 1.0887 0.2712 0.075 Uiso 1 1 calc R . .
C11 C 0.7028(2) 1.0373(7) 0.3735(5) 0.0857(19) Uani 1 1 d . . .
H11 H 0.7228 1.0873 0.3123 0.103 Uiso 1 1 calc R . .
C12 C 0.72118(19) 0.9612(9) 0.4884(6) 0.094(2) Uani 1 1 d . . .
H12 H 0.7537 0.9563 0.5028 0.112 Uiso 1 1 calc R . .
C13 C 0.69115(14) 0.8919(7) 0.5826(4) 0.0620(12) Uani 1 1 d . . .
H13 H 0.7037 0.8423 0.6611 0.074 Uiso 1 1 calc R . .
C14 C 0.60215(11) 0.6600(4) 0.5920(3) 0.0366(6) Uani 1 1 d . . .
C15 C 0.63313(14) 0.5446(4) 0.6168(4) 0.0490(8) Uani 1 1 d . . .
H15 H 0.6586 0.5574 0.6792 0.059 Uiso 1 1 calc R . .
C16 C 0.62670(17) 0.4133(5) 0.5508(5) 0.0595(10) Uani 1 1 d . . .
H16 H 0.6483 0.3372 0.5672 0.071 Uiso 1 1 calc R . .
C17 C 0.58863(16) 0.3891(4) 0.4590(4) 0.0555(10) Uani 1 1 d . . .
H17 H 0.5838 0.2972 0.4167 0.067 Uiso 1 1 calc R . .
C18 C 0.55884(14) 0.5032(5) 0.4330(4) 0.0502(9) Uani 1 1 d . . .
H18 H 0.5335 0.4897 0.3703 0.060 Uiso 1 1 calc R . .
C19 C 0.56511(13) 0.6387(4) 0.4969(3) 0.0444(8) Uani 1 1 d . . .
H19 H 0.5444 0.7161 0.4763 0.053 Uiso 1 1 calc R . .
C20 C 0.56368(12) 0.8901(4) 0.6943(3) 0.0397(7) Uani 1 1 d . . .
C21 C 0.55634(18) 1.0398(5) 0.6751(5) 0.0617(11) Uani 1 1 d . . .
H21 H 0.5792 1.0971 0.6309 0.074 Uiso 1 1 calc R . .
C22 C 0.5155(2) 1.1042(7) 0.7208(6) 0.0827(16) Uani 1 1 d . . .
H22 H 0.5109 1.2054 0.7078 0.099 Uiso 1 1 calc R . .
C23 C 0.48161(19) 1.0233(9) 0.7846(6) 0.0824(18) Uani 1 1 d . . .
H23 H 0.4537 1.0682 0.8130 0.099 Uiso 1 1 calc R . .
C24 C 0.48849(15) 0.8751(8) 0.8075(5) 0.0725(15) Uani 1 1 d . . .
H24 H 0.4656 0.8198 0.8538 0.087 Uiso 1 1 calc R . .
C25 C 0.52958(13) 0.8072(5) 0.7617(4) 0.0489(8) Uani 1 1 d . . .
H25 H 0.5341 0.7063 0.7764 0.059 Uiso 1 1 calc R . .
C26 C 0.5745(3) 0.335(2) 0.964(2) 0.158(9) Uani 0.50 1 d PDU A -1
H26A H 0.5933 0.3202 1.0481 0.238 Uiso 0.50 1 calc PR A -1
H26B H 0.5944 0.3686 0.8881 0.238 Uiso 0.50 1 calc PR A -1
H26C H 0.5596 0.2440 0.9368 0.238 Uiso 0.50 1 calc PR A -1
C27 C 0.5382(5) 0.4479(14) 0.9916(13) 0.142(8) Uani 0.50 1 d PDU A -1
H27A H 0.5289 0.4400 1.0902 0.171 Uiso 0.50 1 calc PR A -1
H27B H 0.5521 0.5451 0.9787 0.171 Uiso 0.50 1 calc PR A -1
O6 O 0.4973(3) 0.4382(13) 0.9055(9) 0.108(4) Uani 0.50 1 d PD A -1
H6 H 0.4779 0.4996 0.9318 0.162 Uiso 0.50 1 calc PR A -1
N1 N 0.76602(16) 0.7009(4) 1.1691(4) 0.0644(10) Uani 1 1 d . . .
O1 O 0.62737(12) 0.7554(4) 1.0879(3) 0.0681(9) Uani 1 1 d . . .
O2 O 0.63405(8) 0.7794(3) 0.7927(2) 0.0395(5) Uani 1 1 d . . .
O3 O 0.74401(10) 0.8363(3) 0.9517(3) 0.0523(7) Uani 1 1 d . . .
O4 O 0.81182(13) 0.9234(4) 1.0880(5) 0.0862(12) Uani 1 1 d . . .
O5 O 0.81816(13) 0.6955(4) 0.9562(4) 0.0693(9) Uani 1 1 d . . .
S1 S 0.79042(4) 0.79078(11) 1.03870(11) 0.0543(3) Uani 1 1 d . . .

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

C1 0.106(4) 0.081(3) 0.053(2) 0.026(3) 0.032(3) 0.009(3)
C2 0.133(5) 0.093(4) 0.045(2) 0.036(3) 0.025(3) 0.031(4)
C3 0.096(3) 0.052(2) 0.0317(17) 0.0089(16) -0.0028(18) 0.021(2)
C4 0.068(2) 0.0360(17) 0.0249(14) 0.0013(12) 0.0008(13) 0.0020(15)
C5 0.064(2) 0.0423(18) 0.0289(14) -0.0031(13) 0.0001(14) 0.0024(16)
C6 0.0579(19) 0.0371(17) 0.0330(15) -0.0042(14) -0.0092(13) 0.0024(15)
C7 0.0450(15) 0.0320(16) 0.0293(13) 0.0010(12) -0.0040(11) -0.0023(12)
C8 0.0511(17) 0.0391(17) 0.0315(15) -0.0083(13) 0.0021(13) -0.0103(14)
C9 0.062(2) 0.0381(18) 0.0376(17) -0.0012(14) 0.0038(15) 0.0017(16)
C10 0.098(3) 0.050(2) 0.040(2) -0.0023(17) 0.020(2) -0.011(2)
C11 0.119(4) 0.091(4) 0.047(2) -0.015(3) 0.030(3) -0.054(4)
C12 0.067(3) 0.154(6) 0.060(3) -0.019(3) 0.007(2) -0.053(4)
C13 0.054(2) 0.090(3) 0.0420(18) -0.009(2) -0.0022(15) -0.017(2)
C14 0.0470(16) 0.0315(15) 0.0313(14) 0.0013(12) 0.0006(12) -0.0046(13)
C15 0.056(2) 0.044(2) 0.0457(19) -0.0044(16) -0.0104(16) 0.0017(16)
C16 0.078(3) 0.039(2) 0.062(2) -0.0039(18) -0.003(2) 0.008(2)
C17 0.083(3) 0.0360(18) 0.0482(19) -0.0097(16) 0.0079(18) -0.0179(19)
C18 0.057(2) 0.055(2) 0.0389(17) -0.0102(16) -0.0020(15) -0.0147(17)
C19 0.0495(18) 0.049(2) 0.0350(16) 0.0001(14) -0.0022(13) -0.0054(15)
C20 0.0485(16) 0.0434(18) 0.0272(14) -0.0012(13) -0.0032(12) 0.0016(15)
C21 0.080(3) 0.055(2) 0.050(2) -0.0039(19) 0.010(2) 0.023(2)
C22 0.103(4) 0.072(3) 0.073(3) -0.008(3) 0.001(3) 0.041(3)
C23 0.063(3) 0.121(5) 0.063(3) -0.034(3) -0.007(2) 0.036(3)
C24 0.047(2) 0.117(5) 0.054(2) -0.028(3) 0.0037(17) -0.005(3)
C25 0.0500(18) 0.058(2) 0.0391(16) -0.0072(17) 0.0004(14) -0.0028(17)
C26 0.038(5) 0.26(3) 0.176(15) -0.064(17) 0.036(7) -0.044(9)
C27 0.32(2) 0.057(7) 0.055(6) 0.005(5) 0.011(11) -0.012(10)
O6 0.084(5) 0.162(10) 0.078(5) -0.047(6) 0.002(4) -0.015(6)
N1 0.095(3) 0.057(2) 0.0411(17) 0.0023(15) -0.0167(17) 0.026(2)
O1 0.0773(19) 0.080(2) 0.0479(15) 0.0118(15) 0.0201(14) -0.0039(17)
O2 0.0500(12) 0.0371(12) 0.0311(10) -0.0026(10) -0.0091(8) 0.0030(10)
O3 0.0579(15) 0.0539(16) 0.0449(13) 0.0132(12) -0.0091(11) -0.0018(12)
O4 0.087(2) 0.059(2) 0.112(3) -0.027(2) -0.046(2) 0.0171(18)
O5 0.081(2) 0.0499(17) 0.078(2) -0.0120(16) 0.0066(17) 0.0194(15)
S1 0.0667(6) 0.0395(5) 0.0562(5) -0.0085(4) -0.0197(4) 0.0149(4)

_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

C1 C2 1.317(8) . ?
C1 O1 1.372(6) . ?
C2 C3 1.432(7) . ?
C3 N1 1.289(7) . ?
C3 C4 1.506(5) . ?
C4 O3 1.442(5) . ?
C4 C5 1.505(5) . ?
C5 O1 1.436(5) . ?
C5 C6 1.506(5) . ?
C6 O2 1.419(4) . ?
C7 O2 1.451(4) . ?
C7 C8 1.532(4) . ?
C7 C14 1.548(4) . ?
C7 C20 1.549(5) . ?
C8 C9 1.396(5) . ?
C8 C13 1.398(5) . ?
C9 C10 1.391(5) . ?
C10 C11 1.388(8) . ?
C11 C12 1.391(10) . ?
C12 C13 1.400(7) . ?
C14 C15 1.394(5) . ?
C14 C19 1.396(5) . ?
C15 C16 1.364(6) . ?
C16 C17 1.403(7) . ?
C17 C18 1.366(6) . ?
C18 C19 1.388(5) . ?
C20 C21 1.394(6) . ?
C20 C25 1.397(5) . ?
C21 C22 1.384(7) . ?
C22 C23 1.366(9) . ?
C23 C24 1.383(10) . ?
C24 C25 1.402(6) . ?
C26 C27 1.488(9) . ?
C27 O6 1.420(9) . ?
N1 S1 1.648(4) . ?
O3 S1 1.609(3) . ?
O4 S1 1.432(4) . ?
O5 S1 1.420(3) . ?

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

C2 C1 O1 126.4(4) . . ?
C1 C2 C3 117.7(4) . . ?
N1 C3 C2 128.7(4) . . ?
N1 C3 C4 116.5(4) . . ?
C2 C3 C4 114.8(4) . . ?
O3 C4 C5 111.5(3) . . ?
O3 C4 C3 104.7(3) . . ?
C5 C4 C3 110.3(3) . . ?
O1 C5 C4 108.3(3) . . ?
O1 C5 C6 107.5(3) . . ?
C4 C5 C6 115.2(3) . . ?
O2 C6 C5 107.8(3) . . ?
O2 C7 C8 110.6(3) . . ?
O2 C7 C14 104.3(2) . . ?
C8 C7 C14 106.1(2) . . ?
O2 C7 C20 108.0(2) . . ?
C8 C7 C20 115.2(3) . . ?
C14 C7 C20 112.0(3) . . ?
C9 C8 C13 118.1(3) . . ?
C9 C8 C7 121.3(3) . . ?
C13 C8 C7 120.4(3) . . ?
C10 C9 C8 121.3(4) . . ?
C11 C10 C9 120.0(5) . . ?
C10 C11 C12 119.7(4) . . ?
C11 C12 C13 120.0(5) . . ?
C8 C13 C12 120.9(5) . . ?
C15 C14 C19 118.6(3) . . ?
C15 C14 C7 120.9(3) . . ?
C19 C14 C7 120.3(3) . . ?
C16 C15 C14 120.3(4) . . ?
C15 C16 C17 121.5(4) . . ?
C18 C17 C16 118.0(4) . . ?
C17 C18 C19 121.5(4) . . ?
C18 C19 C14 120.0(4) . . ?
C21 C20 C25 119.1(4) . . ?
C21 C20 C7 123.6(3) . . ?
C25 C20 C7 116.9(3) . . ?
C22 C21 C20 120.1(5) . . ?
C23 C22 C21 121.1(5) . . ?
C22 C23 C24 119.9(4) . . ?
C23 C24 C25 120.1(5) . . ?
C20 C25 C24 119.7(5) . . ?
O6 C27 C26 115.2(11) . . ?
C3 N1 S1 107.9(3) . . ?
C1 O1 C5 117.5(4) . . ?
C6 O2 C7 115.7(3) . . ?
C4 O3 S1 108.7(2) . . ?
O5 S1 O4 117.3(2) . . ?
O5 S1 O3 109.71(19) . . ?
O4 S1 O3 107.22(18) . . ?
O5 S1 N1 110.8(2) . . ?
O4 S1 N1 111.0(3) . . ?
O3 S1 N1 99.24(18) . . ?

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 C2 C3 -1.4(10) . . . . ?
C1 C2 C3 N1 164.3(6) . . . . ?
C1 C2 C3 C4 -16.8(8) . . . . ?
N1 C3 C4 O3 -14.9(5) . . . . ?
C2 C3 C4 O3 166.1(4) . . . . ?
N1 C3 C4 C5 -135.0(4) . . . . ?
C2 C3 C4 C5 46.0(5) . . . . ?
O3 C4 C5 O1 -172.2(3) . . . . ?
C3 C4 C5 O1 -56.3(4) . . . . ?
O3 C4 C5 C6 67.5(4) . . . . ?
C3 C4 C5 C6 -176.6(4) . . . . ?
O1 C5 C6 O2 -68.5(3) . . . . ?
C4 C5 C6 O2 52.3(4) . . . . ?
O2 C7 C8 C9 -165.6(3) . . . . ?
C14 C7 C8 C9 81.8(4) . . . . ?
C20 C7 C8 C9 -42.7(4) . . . . ?
O2 C7 C8 C13 19.6(4) . . . . ?
C14 C7 C8 C13 -92.9(4) . . . . ?
C20 C7 C8 C13 142.5(4) . . . . ?
C13 C8 C9 C10 -3.0(6) . . . . ?
C7 C8 C9 C10 -177.9(3) . . . . ?
C8 C9 C10 C11 1.7(6) . . . . ?
C9 C10 C11 C12 1.2(8) . . . . ?
C10 C11 C12 C13 -2.7(10) . . . . ?
C9 C8 C13 C12 1.5(7) . . . . ?
C7 C8 C13 C12 176.5(5) . . . . ?
C11 C12 C13 C8 1.3(9) . . . . ?
O2 C7 C14 C15 -30.4(4) . . . . ?
C8 C7 C14 C15 86.5(4) . . . . ?
C20 C7 C14 C15 -147.0(3) . . . . ?
O2 C7 C14 C19 153.7(3) . . . . ?
C8 C7 C14 C19 -89.5(3) . . . . ?
C20 C7 C14 C19 37.1(4) . . . . ?
C19 C14 C15 C16 -1.1(6) . . . . ?
C7 C14 C15 C16 -177.1(3) . . . . ?
C14 C15 C16 C17 -1.3(7) . . . . ?
C15 C16 C17 C18 2.4(6) . . . . ?
C16 C17 C18 C19 -1.3(6) . . . . ?
C17 C18 C19 C14 -1.0(6) . . . . ?
C15 C14 C19 C18 2.2(5) . . . . ?
C7 C14 C19 C18 178.2(3) . . . . ?
O2 C7 C20 C21 105.4(4) . . . . ?
C8 C7 C20 C21 -18.9(5) . . . . ?
C14 C7 C20 C21 -140.3(4) . . . . ?
O2 C7 C20 C25 -67.4(4) . . . . ?
C8 C7 C20 C25 168.3(3) . . . . ?
C14 C7 C20 C25 46.9(4) . . . . ?
C25 C20 C21 C22 -0.9(6) . . . . ?
C7 C20 C21 C22 -173.5(4) . . . . ?
C20 C21 C22 C23 -0.3(8) . . . . ?
C21 C22 C23 C24 1.6(8) . . . . ?
C22 C23 C24 C25 -1.8(7) . . . . ?
C21 C20 C25 C24 0.7(5) . . . . ?
C7 C20 C25 C24 173.8(3) . . . . ?
C23 C24 C25 C20 0.6(6) . . . . ?
C2 C3 N1 S1 -176.1(5) . . . . ?
C4 C3 N1 S1 5.0(5) . . . . ?
C2 C1 O1 C5 -11.9(9) . . . . ?
C4 C5 O1 C1 40.5(5) . . . . ?
C6 C5 O1 C1 165.5(4) . . . . ?
C5 C6 O2 C7 175.4(3) . . . . ?
C8 C7 O2 C6 73.5(3) . . . . ?
C14 C7 O2 C6 -172.8(3) . . . . ?
C20 C7 O2 C6 -53.5(3) . . . . ?
C5 C4 O3 S1 136.8(2) . . . . ?
C3 C4 O3 S1 17.5(3) . . . . ?
C4 O3 S1 O5 101.6(3) . . . . ?
C4 O3 S1 O4 -130.0(3) . . . . ?
C4 O3 S1 N1 -14.5(3) . . . . ?
C3 N1 S1 O5 -109.6(3) . . . . ?
C3 N1 S1 O4 118.2(3) . . . . ?
C3 N1 S1 O3 5.7(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        27.15

_diffrn_measured_fraction_theta_full 0.999

_refine_diff_density_max         0.779

_refine_diff_density_min         -0.321

_refine_diff_density_rms         0.085