# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2009

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Teck-Peng Loh'
_publ_contact_author_email       TECKPENG@NTU.EDU.SG

_publ_section_title              
;
Bio-inspired Polyene Cyclization:
Aziridinyl Polyene Cyclization Catalyzed by InBr3
;
loop_
_publ_author_name
'Teck-Peng Loh.'
'Bin Li.'
'Si-Min Li.'
'Li-Jun Serena Tan.'
'Yu-Jun Zhao.'

# Attachment '4_Cyclization_product_Compound_2.cif'

data_ltp122
_database_code_depnum_ccdc_archive 'CCDC 715056'

_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;

?

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         'C24 H31 N O2 S'

_chemical_formula_sum            'C24 H31 N O2 S'

_chemical_formula_weight         397.56

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           Triclinic

_symmetry_space_group_name_H-M   P-1

loop_

_symmetry_equiv_pos_as_xyz

'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.4457(3)

_cell_length_b                   10.0804(5)

_cell_length_c                   15.3234(7)

_cell_angle_alpha                105.483(2)

_cell_angle_beta                 98.831(2)

_cell_angle_gamma                91.245(2)

_cell_volume                     1092.85(9)

_cell_formula_units_Z            2

_cell_measurement_temperature    296(2)

_cell_measurement_reflns_used    5505

_cell_measurement_theta_min      0.00

_cell_measurement_theta_max      0.00

_exptl_crystal_description       plate

_exptl_crystal_colour            colourless

_exptl_crystal_size_max          0.30

_exptl_crystal_size_mid          0.24

_exptl_crystal_size_min          0.08

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.208

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             428

_exptl_absorpt_coefficient_mu    0.167

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.9516

_exptl_absorpt_correction_T_max  0.9868

_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;

?

;

_diffrn_ambient_temperature      296(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            22664

_diffrn_reflns_av_R_equivalents  0.0384

_diffrn_reflns_av_sigmaI/netI    0.0353

_diffrn_reflns_limit_h_min       -9

_diffrn_reflns_limit_h_max       9

_diffrn_reflns_limit_k_min       -12

_diffrn_reflns_limit_k_max       12

_diffrn_reflns_limit_l_min       -18

_diffrn_reflns_limit_l_max       18

_diffrn_reflns_theta_min         1.40

_diffrn_reflns_theta_max         26.03

_reflns_number_total             4308

_reflns_number_gt                2843

_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.

;

_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^)+(0.0968P)^2^+0.0996P] 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_number_reflns         4308

_refine_ls_number_parameters     257

_refine_ls_number_restraints     0

_refine_ls_R_factor_all          0.0872

_refine_ls_R_factor_gt           0.0506

_refine_ls_wR_factor_ref         0.1759

_refine_ls_wR_factor_gt          0.1420

_refine_ls_goodness_of_fit_ref   1.084

_refine_ls_restrained_S_all      1.084

_refine_ls_shift/su_max          0.000

_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 0.7896(5) 1.0356(3) 0.3479(2) 0.1003(11) Uani 1 1 d . . .
H1A H 0.8036 0.9959 0.2852 0.150 Uiso 1 1 calc R . .
H1B H 0.9067 1.0492 0.3865 0.150 Uiso 1 1 calc R . .
H1C H 0.7362 1.1227 0.3535 0.150 Uiso 1 1 calc R . .
C2 C 0.6676(4) 0.9398(3) 0.37681(18) 0.0666(7) Uani 1 1 d . . .
C3 C 0.4819(4) 0.9489(3) 0.36498(19) 0.0748(8) Uani 1 1 d . . .
H3 H 0.4319 1.0168 0.3398 0.090 Uiso 1 1 calc R . .
C4 C 0.3678(4) 0.8604(3) 0.38932(18) 0.0638(7) Uani 1 1 d . . .
H4 H 0.2426 0.8687 0.3807 0.077 Uiso 1 1 calc R . .
C5 C 0.4407(3) 0.7601(2) 0.42637(15) 0.0493(6) Uani 1 1 d . . .
C6 C 0.6268(3) 0.7485(3) 0.43916(16) 0.0586(6) Uani 1 1 d . . .
H6 H 0.6767 0.6805 0.4643 0.070 Uiso 1 1 calc R . .
C7 C 0.7377(4) 0.8381(3) 0.41452(17) 0.0655(7) Uani 1 1 d . . .
H7 H 0.8629 0.8301 0.4235 0.079 Uiso 1 1 calc R . .
C8 C 0.2490(3) 0.4667(2) 0.28812(15) 0.0473(5) Uani 1 1 d . . .
H8 H 0.1940 0.5494 0.2771 0.057 Uiso 1 1 calc R . .
C9 C 0.1022(3) 0.3459(2) 0.24952(16) 0.0534(6) Uani 1 1 d . . .
C10 C 0.1646(4) 0.2179(3) 0.2807(2) 0.0742(8) Uani 1 1 d . . .
H10A H 0.1548 0.2322 0.3442 0.111 Uiso 1 1 calc R . .
H10B H 0.2889 0.2042 0.2728 0.111 Uiso 1 1 calc R . .
H10C H 0.0888 0.1380 0.2444 0.111 Uiso 1 1 calc R . .
C11 C -0.0707(3) 0.3910(3) 0.28875(19) 0.0729(8) Uani 1 1 d . . .
H11A H -0.1206 0.4627 0.2638 0.109 Uiso 1 1 calc R . .
H11B H -0.0416 0.4250 0.3544 0.109 Uiso 1 1 calc R . .
H11C H -0.1585 0.3137 0.2727 0.109 Uiso 1 1 calc R . .
C12 C 0.0637(3) 0.3211(2) 0.14324(16) 0.0501(6) Uani 1 1 d . . .
H12 H 0.0174 0.4080 0.1350 0.060 Uiso 1 1 calc R . .
C13 C -0.0907(3) 0.2132(3) 0.09217(19) 0.0690(7) Uani 1 1 d . . .
H13A H -0.0460 0.1215 0.0819 0.083 Uiso 1 1 calc R . .
H13B H -0.1872 0.2182 0.1286 0.083 Uiso 1 1 calc R . .
C14 C -0.1635(4) 0.2399(3) 0.00150(19) 0.0708(8) Uani 1 1 d . . .
H14A H -0.2454 0.1623 -0.0354 0.085 Uiso 1 1 calc R . .
H14B H -0.2336 0.3210 0.0126 0.085 Uiso 1 1 calc R . .
C15 C -0.0167(3) 0.2617(2) -0.05185(17) 0.0572(6) Uani 1 1 d . . .
C16 C -0.0629(4) 0.2502(3) -0.14602(19) 0.0702(8) Uani 1 1 d . . .
H16 H -0.1834 0.2271 -0.1744 0.084 Uiso 1 1 calc R . .
C17 C 0.0635(5) 0.2719(3) -0.1969(2) 0.0762(8) Uani 1 1 d . . .
H17 H 0.0291 0.2635 -0.2592 0.091 Uiso 1 1 calc R . .
C18 C 0.2425(4) 0.3062(3) -0.15603(19) 0.0761(8) Uani 1 1 d . . .
H18 H 0.3298 0.3218 -0.1902 0.091 Uiso 1 1 calc R . .
C19 C 0.2903(4) 0.3171(3) -0.06377(17) 0.0681(7) Uani 1 1 d . . .
H19 H 0.4115 0.3396 -0.0366 0.082 Uiso 1 1 calc R . .
C20 C 0.1653(3) 0.2958(2) -0.00968(16) 0.0538(6) Uani 1 1 d . . .
C21 C 0.2295(3) 0.3016(2) 0.09232(16) 0.0492(6) Uani 1 1 d . . .
C22 C 0.3238(4) 0.1658(3) 0.09053(19) 0.0712(8) Uani 1 1 d . . .
H22A H 0.4107 0.1539 0.0493 0.107 Uiso 1 1 calc R . .
H22B H 0.2340 0.0894 0.0701 0.107 Uiso 1 1 calc R . .
H22C H 0.3850 0.1697 0.1511 0.107 Uiso 1 1 calc R . .
C23 C 0.3678(3) 0.4240(3) 0.13844(15) 0.0522(6) Uani 1 1 d . . .
H23A H 0.4777 0.4085 0.1114 0.063 Uiso 1 1 calc R . .
H23B H 0.3182 0.5067 0.1263 0.063 Uiso 1 1 calc R . .
C24 C 0.4167(3) 0.4470(3) 0.24122(15) 0.0539(6) Uani 1 1 d . . .
H24A H 0.5005 0.5279 0.2668 0.065 Uiso 1 1 calc R . .
H24B H 0.4779 0.3683 0.2535 0.065 Uiso 1 1 calc R . .
N1 N 0.3051(3) 0.4939(2) 0.38814(12) 0.0513(5) Uani 1 1 d . . .
H1 H 0.3431 0.4277 0.4103 0.062 Uiso 1 1 calc R . .
O1 O 0.3742(2) 0.63371(19) 0.54644(10) 0.0661(5) Uani 1 1 d . . .
O2 O 0.1164(2) 0.6873(2) 0.44189(12) 0.0714(5) Uani 1 1 d . . .
S1 S 0.29695(8) 0.64410(7) 0.45670(4) 0.0547(2) 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 0.131(3) 0.0598(19) 0.117(3) 0.0204(18) 0.049(2) -0.0025(19)
C2 0.088(2) 0.0473(15) 0.0623(16) 0.0062(13) 0.0207(14) 0.0081(14)
C3 0.097(2) 0.0562(17) 0.0769(19) 0.0305(14) 0.0072(16) 0.0204(15)
C4 0.0633(16) 0.0628(16) 0.0668(17) 0.0247(14) 0.0007(13) 0.0192(13)
C5 0.0534(14) 0.0529(14) 0.0403(12) 0.0114(10) 0.0044(10) 0.0162(11)
C6 0.0581(16) 0.0644(16) 0.0582(15) 0.0231(13) 0.0112(12) 0.0200(12)
C7 0.0614(16) 0.0655(17) 0.0689(17) 0.0133(14) 0.0171(13) 0.0104(13)
C8 0.0443(13) 0.0536(14) 0.0499(13) 0.0226(11) 0.0097(10) 0.0089(10)
C9 0.0436(13) 0.0608(15) 0.0634(15) 0.0298(12) 0.0098(11) 0.0009(11)
C10 0.0811(19) 0.0683(18) 0.086(2) 0.0447(16) 0.0124(15) -0.0011(14)
C11 0.0518(16) 0.097(2) 0.0801(19) 0.0357(17) 0.0224(14) 0.0011(14)
C12 0.0392(12) 0.0528(14) 0.0627(15) 0.0247(12) 0.0069(10) 0.0013(10)
C13 0.0529(15) 0.0689(18) 0.085(2) 0.0248(15) 0.0065(14) -0.0115(13)
C14 0.0532(15) 0.0695(18) 0.0800(19) 0.0144(15) -0.0066(14) -0.0053(13)
C15 0.0538(15) 0.0479(14) 0.0618(16) 0.0074(12) -0.0023(12) 0.0072(11)
C16 0.0698(18) 0.0636(17) 0.0647(18) 0.0066(14) -0.0087(15) 0.0123(14)
C17 0.097(2) 0.0693(19) 0.0550(16) 0.0098(14) 0.0019(16) 0.0182(16)
C18 0.085(2) 0.083(2) 0.0572(17) 0.0123(15) 0.0136(15) 0.0036(16)
C19 0.0615(17) 0.083(2) 0.0554(16) 0.0097(14) 0.0120(13) 0.0012(14)
C20 0.0536(15) 0.0467(13) 0.0561(15) 0.0083(11) 0.0040(12) 0.0076(11)
C21 0.0422(12) 0.0498(13) 0.0560(14) 0.0168(11) 0.0049(10) 0.0030(10)
C22 0.0646(17) 0.0631(17) 0.084(2) 0.0178(15) 0.0082(14) 0.0181(13)
C23 0.0415(13) 0.0639(15) 0.0511(14) 0.0141(12) 0.0114(10) -0.0031(11)
C24 0.0431(13) 0.0657(16) 0.0531(14) 0.0159(12) 0.0097(10) 0.0005(11)
N1 0.0582(12) 0.0561(12) 0.0464(11) 0.0238(9) 0.0109(9) 0.0133(9)
O1 0.0742(12) 0.0870(13) 0.0450(10) 0.0263(9) 0.0159(8) 0.0289(10)
O2 0.0519(10) 0.0888(13) 0.0780(12) 0.0260(10) 0.0157(9) 0.0294(9)
S1 0.0524(4) 0.0696(4) 0.0483(4) 0.0224(3) 0.0133(3) 0.0226(3)

_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 1.506(4) . ?
C2 C3 1.375(4) . ?
C2 C7 1.379(4) . ?
C3 C4 1.378(4) . ?
C4 C5 1.370(3) . ?
C5 C6 1.381(3) . ?
C5 S1 1.765(3) . ?
C6 C7 1.373(4) . ?
C8 N1 1.474(3) . ?
C8 C24 1.525(3) . ?
C8 C9 1.545(3) . ?
C9 C11 1.531(3) . ?
C9 C10 1.548(3) . ?
C9 C12 1.560(3) . ?
C12 C13 1.527(3) . ?
C12 C21 1.548(3) . ?
C13 C14 1.507(3) . ?
C14 C15 1.507(4) . ?
C15 C20 1.402(3) . ?
C15 C16 1.404(4) . ?
C16 C17 1.360(4) . ?
C17 C18 1.377(4) . ?
C18 C19 1.378(3) . ?
C19 C20 1.386(3) . ?
C20 C21 1.548(3) . ?
C21 C23 1.529(3) . ?
C21 C22 1.548(3) . ?
C23 C24 1.514(3) . ?
N1 S1 1.6046(19) . ?
O1 S1 1.4385(16) . ?
O2 S1 1.4261(17) . ?

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

C3 C2 C7 117.6(3) . . ?
C3 C2 C1 121.1(3) . . ?
C7 C2 C1 121.3(3) . . ?
C2 C3 C4 122.0(2) . . ?
C5 C4 C3 119.3(2) . . ?
C4 C5 C6 120.0(2) . . ?
C4 C5 S1 120.09(19) . . ?
C6 C5 S1 119.89(18) . . ?
C7 C6 C5 119.6(2) . . ?
C6 C7 C2 121.5(3) . . ?
N1 C8 C24 109.59(17) . . ?
N1 C8 C9 111.73(17) . . ?
C24 C8 C9 113.6(2) . . ?
C11 C9 C8 107.9(2) . . ?
C11 C9 C10 108.1(2) . . ?
C8 C9 C10 110.46(19) . . ?
C11 C9 C12 109.22(19) . . ?
C8 C9 C12 106.88(17) . . ?
C10 C9 C12 114.1(2) . . ?
C13 C12 C21 110.5(2) . . ?
C13 C12 C9 115.25(19) . . ?
C21 C12 C9 117.34(18) . . ?
C14 C13 C12 109.1(2) . . ?
C15 C14 C13 113.4(2) . . ?
C20 C15 C16 118.7(3) . . ?
C20 C15 C14 121.8(2) . . ?
C16 C15 C14 119.4(2) . . ?
C17 C16 C15 121.9(3) . . ?
C16 C17 C18 119.8(3) . . ?
C17 C18 C19 119.0(3) . . ?
C18 C19 C20 122.8(3) . . ?
C19 C20 C15 117.8(2) . . ?
C19 C20 C21 120.3(2) . . ?
C15 C20 C21 121.9(2) . . ?
C23 C21 C12 108.01(19) . . ?
C23 C21 C22 109.21(19) . . ?
C12 C21 C22 114.7(2) . . ?
C23 C21 C20 110.50(18) . . ?
C12 C21 C20 109.15(17) . . ?
C22 C21 C20 105.29(19) . . ?
C24 C23 C21 113.10(19) . . ?
C23 C24 C8 111.91(18) . . ?
C8 N1 S1 121.53(14) . . ?
O2 S1 O1 119.24(10) . . ?
O2 S1 N1 108.65(11) . . ?
O1 S1 N1 105.73(10) . . ?
O2 S1 C5 106.97(11) . . ?
O1 S1 C5 108.00(11) . . ?
N1 S1 C5 107.80(10) . . ?

_diffrn_measured_fraction_theta_max 0.998

_diffrn_reflns_theta_full        26.03

_diffrn_measured_fraction_theta_full 0.998

_refine_diff_density_max         0.290

_refine_diff_density_min         -0.494

_refine_diff_density_rms         0.101

# Attachment '5_Cyclization_product_Compound_4d.cif'

data_ltp127
_database_code_depnum_ccdc_archive 'CCDC 715057'

_audit_creation_method           SHELXL-97

_chemical_name_systematic        
;

?

;

_chemical_name_common            ?

_chemical_melting_point          ?

_chemical_formula_moiety         'C30 H41 N O2 S, C3 H7'

_chemical_formula_sum            'C33 H48 N O2 S'

_chemical_formula_weight         522.78

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

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                   15.9530(10)

_cell_length_b                   10.3665(7)

_cell_length_c                   19.6283(11)

_cell_angle_alpha                90.00

_cell_angle_beta                 112.573(2)

_cell_angle_gamma                90.00

_cell_volume                     2997.4(3)

_cell_formula_units_Z            4

_cell_measurement_temperature    173(2)

_cell_measurement_reflns_used    5150

_cell_measurement_theta_min      2.77

_cell_measurement_theta_max      21.55

_exptl_crystal_description       prism

_exptl_crystal_colour            colourless

_exptl_crystal_size_max          0.32

_exptl_crystal_size_mid          0.24

_exptl_crystal_size_min          0.20

_exptl_crystal_density_meas      ?

_exptl_crystal_density_diffrn    1.158

_exptl_crystal_density_method    'not measured'

_exptl_crystal_F_000             1140

_exptl_absorpt_coefficient_mu    0.137

_exptl_absorpt_correction_type   multi-scan

_exptl_absorpt_correction_T_min  0.9575

_exptl_absorpt_correction_T_max  0.9731

_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;

?

;

_diffrn_ambient_temperature      173(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            33324

_diffrn_reflns_av_R_equivalents  0.0600

_diffrn_reflns_av_sigmaI/netI    0.0518

_diffrn_reflns_limit_h_min       -18

_diffrn_reflns_limit_h_max       19

_diffrn_reflns_limit_k_min       -12

_diffrn_reflns_limit_k_max       12

_diffrn_reflns_limit_l_min       -23

_diffrn_reflns_limit_l_max       22

_diffrn_reflns_theta_min         1.41

_diffrn_reflns_theta_max         25.08

_reflns_number_total             5306

_reflns_number_gt                3505

_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.

;

_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^)+(0.1102P)^2^+0.9855P] 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         5306

_refine_ls_number_parameters     409

_refine_ls_number_restraints     321

_refine_ls_R_factor_all          0.1127

_refine_ls_R_factor_gt           0.0642

_refine_ls_wR_factor_ref         0.2122

_refine_ls_wR_factor_gt          0.1680

_refine_ls_goodness_of_fit_ref   1.095

_refine_ls_restrained_S_all      1.089

_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

C24 C -0.083(3) 0.859(4) 0.8515(10) 0.047(4) Uani 0.47(3) 1 d PDU A 1
C25 C -0.130(2) 0.974(3) 0.8451(11) 0.050(4) Uani 0.47(3) 1 d PDU A 1
H25 H -0.1160 1.0283 0.8869 0.060 Uiso 0.47(3) 1 calc PR A 1
C26 C -0.1975(15) 1.010(2) 0.7788(10) 0.057(4) Uani 0.47(3) 1 d PDU A 1
H26 H -0.2313 1.0860 0.7777 0.068 Uiso 0.47(3) 1 calc PR A 1
C27 C -0.2177(11) 0.942(2) 0.7150(9) 0.064(4) Uani 0.47(3) 1 d PDU A 1
C28 C -0.2835(13) 0.985(3) 0.6395(9) 0.095(6) Uani 0.47(3) 1 d PDU A 1
H28A H -0.3458 0.9650 0.6342 0.143 Uiso 0.47(3) 1 calc PR A 1
H28B H -0.2697 0.9402 0.6012 0.143 Uiso 0.47(3) 1 calc PR A 1
H28C H -0.2776 1.0785 0.6345 0.143 Uiso 0.47(3) 1 calc PR A 1
C29 C -0.1705(15) 0.830(2) 0.7200(9) 0.074(5) Uani 0.47(3) 1 d PDU A 1
H29 H -0.1840 0.7782 0.6772 0.088 Uiso 0.47(3) 1 calc PR A 1
C30 C -0.1036(16) 0.790(2) 0.7856(11) 0.063(4) Uani 0.47(3) 1 d PDU A 1
H30 H -0.0710 0.7128 0.7860 0.076 Uiso 0.47(3) 1 calc PR A 1
C24A C -0.080(2) 0.846(4) 0.8491(10) 0.044(3) Uani 0.53(3) 1 d PDU A 2
C25A C -0.1367(18) 0.950(2) 0.8384(10) 0.051(4) Uani 0.53(3) 1 d PDU A 2
H25A H -0.1331 1.0052 0.8781 0.061 Uiso 0.53(3) 1 calc PR A 2
C26A C -0.1997(13) 0.9713(19) 0.7679(8) 0.058(3) Uani 0.53(3) 1 d PDU A 2
H26A H -0.2389 1.0439 0.7587 0.069 Uiso 0.53(3) 1 calc PR A 2
C27A C -0.2069(8) 0.8898(19) 0.7107(6) 0.053(4) Uani 0.53(3) 1 d PDU A 2
C28A C -0.2804(10) 0.914(2) 0.6349(7) 0.087(5) Uani 0.53(3) 1 d PDU A 2
H28D H -0.3145 0.8344 0.6163 0.130 Uiso 0.53(3) 1 calc PR A 2
H28E H -0.2524 0.9425 0.6009 0.130 Uiso 0.53(3) 1 calc PR A 2
H28F H -0.3217 0.9813 0.6386 0.130 Uiso 0.53(3) 1 calc PR A 2
C29A C -0.1507(9) 0.7833(19) 0.7252(8) 0.058(3) Uani 0.53(3) 1 d PDU A 2
H29A H -0.1571 0.7248 0.6862 0.069 Uiso 0.53(3) 1 calc PR A 2
C30A C -0.0855(12) 0.7591(19) 0.7944(9) 0.048(3) Uani 0.53(3) 1 d PDU A 2
H30A H -0.0467 0.6861 0.8038 0.058 Uiso 0.53(3) 1 calc PR A 2
C1 C 0.3668(3) 0.9162(4) 0.54662(18) 0.0577(11) Uani 1 1 d . . .
H1A H 0.3956 0.8663 0.5191 0.087 Uiso 1 1 calc R . .
H1B H 0.3619 1.0067 0.5311 0.087 Uiso 1 1 calc R . .
H1C H 0.3061 0.8815 0.5366 0.087 Uiso 1 1 calc R . .
C2 C 0.4238(3) 0.9069(3) 0.62852(18) 0.0471(9) Uani 1 1 d . . .
C3 C 0.5064(3) 0.8456(4) 0.6523(2) 0.0589(11) Uani 1 1 d . . .
H3 H 0.5271 0.8093 0.6172 0.071 Uiso 1 1 calc R . .
C4 C 0.5594(3) 0.8361(4) 0.7260(2) 0.0668(12) Uani 1 1 d . . .
H4 H 0.6165 0.7938 0.7417 0.080 Uiso 1 1 calc R . .
C5 C 0.5290(2) 0.8887(4) 0.7779(2) 0.0585(11) Uani 1 1 d . . .
H5 H 0.5661 0.8828 0.8289 0.070 Uiso 1 1 calc R . .
C6 C 0.4451(2) 0.9498(3) 0.75573(18) 0.0413(8) Uani 1 1 d . . .
C7 C 0.3933(2) 0.9614(3) 0.68040(17) 0.0413(8) Uani 1 1 d . . .
C8 C 0.3032(3) 1.0316(3) 0.65219(18) 0.0475(9) Uani 1 1 d . . .
H8A H 0.2544 0.9686 0.6272 0.057 Uiso 1 1 calc R . .
H8B H 0.3035 1.0957 0.6149 0.057 Uiso 1 1 calc R . .
C9 C 0.2806(2) 1.1007(3) 0.71123(17) 0.0453(8) Uani 1 1 d . . .
H9A H 0.2146 1.1183 0.6927 0.054 Uiso 1 1 calc R . .
H9B H 0.3131 1.1843 0.7231 0.054 Uiso 1 1 calc R . .
C10 C 0.3086(2) 1.0174(3) 0.78098(15) 0.0358(7) Uani 1 1 d . . .
H10 H 0.2866 0.9289 0.7624 0.043 Uiso 1 1 calc R . .
C11 C 0.4133(2) 1.0050(3) 0.81486(16) 0.0382(8) Uani 1 1 d . . .
C12 C 0.4658(3) 1.1330(4) 0.8419(2) 0.0548(10) Uani 1 1 d . . .
H12A H 0.4464 1.1961 0.8016 0.082 Uiso 1 1 calc R . .
H12B H 0.5311 1.1172 0.8576 0.082 Uiso 1 1 calc R . .
H12C H 0.4530 1.1668 0.8835 0.082 Uiso 1 1 calc R . .
C13 C 0.4384(2) 0.9111(3) 0.88061(17) 0.0430(8) Uani 1 1 d . . .
H13A H 0.4195 0.8229 0.8616 0.052 Uiso 1 1 calc R . .
H13B H 0.5052 0.9105 0.9071 0.052 Uiso 1 1 calc R . .
C14 C 0.3945(2) 0.9457(3) 0.93496(16) 0.0413(8) Uani 1 1 d . . .
H14A H 0.4162 1.0316 0.9566 0.050 Uiso 1 1 calc R . .
H14B H 0.4128 0.8818 0.9756 0.050 Uiso 1 1 calc R . .
C15 C 0.2911(2) 0.9475(3) 0.89670(15) 0.0333(7) Uani 1 1 d . . .
H15 H 0.2757 0.8633 0.8699 0.040 Uiso 1 1 calc R . .
C16 C 0.2600(2) 1.0504(3) 0.83458(16) 0.0360(7) Uani 1 1 d . . .
C17 C 0.2778(3) 1.1909(3) 0.8620(2) 0.0493(9) Uani 1 1 d . . .
H17A H 0.2261 1.2228 0.8723 0.074 Uiso 1 1 calc R . .
H17B H 0.2859 1.2448 0.8239 0.074 Uiso 1 1 calc R . .
H17C H 0.3329 1.1946 0.9072 0.074 Uiso 1 1 calc R . .
C18 C 0.1569(2) 1.0329(3) 0.79258(17) 0.0411(8) Uani 1 1 d . . .
H18A H 0.1338 1.1038 0.7564 0.049 Uiso 1 1 calc R . .
H18B H 0.1459 0.9508 0.7648 0.049 Uiso 1 1 calc R . .
C19 C 0.1038(2) 1.0316(3) 0.84264(18) 0.0431(8) Uani 1 1 d . . .
H19A H 0.1084 1.1174 0.8660 0.052 Uiso 1 1 calc R . .
H19B H 0.0389 1.0150 0.8126 0.052 Uiso 1 1 calc R . .
C20 C 0.1388(2) 0.9295(3) 0.90232(16) 0.0355(7) Uani 1 1 d . . .
H20 H 0.1306 0.8440 0.8770 0.043 Uiso 1 1 calc R . .
C21 C 0.2405(2) 0.9434(3) 0.95077(16) 0.0359(7) Uani 1 1 d . . .
C22 C 0.2575(2) 1.0605(4) 1.00192(18) 0.0492(9) Uani 1 1 d . . .
H22A H 0.3228 1.0781 1.0245 0.074 Uiso 1 1 calc R . .
H22B H 0.2345 1.0425 1.0406 0.074 Uiso 1 1 calc R . .
H22C H 0.2259 1.1358 0.9733 0.074 Uiso 1 1 calc R . .
C23 C 0.2703(2) 0.8226(3) 0.99942(18) 0.0466(9) Uani 1 1 d . . .
H23A H 0.2718 0.7485 0.9689 0.070 Uiso 1 1 calc R . .
H23B H 0.2271 0.8056 1.0229 0.070 Uiso 1 1 calc R . .
H23C H 0.3309 0.8365 1.0375 0.070 Uiso 1 1 calc R . .
C31 C 0.5108(9) 0.4746(19) 0.0372(7) 0.346(11) Uani 1 1 d DU . .
H31A H 0.5432 0.3912 0.0442 0.415 Uiso 1 1 calc R . .
H31B H 0.5482 0.5363 0.0752 0.415 Uiso 1 1 calc R . .
C32 C 0.4256(8) 0.460(2) 0.0393(8) 0.343(10) Uani 1 1 d DU . .
H32A H 0.3875 0.5359 0.0173 0.411 Uiso 1 1 calc R . .
H32B H 0.3955 0.3824 0.0107 0.411 Uiso 1 1 calc R . .
C33 C 0.4356(7) 0.4461(14) 0.1115(6) 0.296(9) Uani 1 1 d DU . .
H33A H 0.4841 0.3839 0.1360 0.444 Uiso 1 1 calc R . .
H33B H 0.3786 0.4151 0.1135 0.444 Uiso 1 1 calc R . .
H33C H 0.4514 0.5297 0.1365 0.444 Uiso 1 1 calc R . .
N1 N 0.08470(18) 0.9269(3) 0.94891(14) 0.0386(7) Uani 1 1 d . A .
H1N H 0.071(2) 1.003(3) 0.9681(17) 0.046 Uiso 1 1 d . . .
O1 O -0.02922(16) 0.8465(2) 0.99206(12) 0.0486(6) Uani 1 1 d . A .
O2 O 0.04310(19) 0.6975(2) 0.93309(16) 0.0652(8) Uani 1 1 d . A .
S1 S 0.00634(6) 0.82121(8) 0.93633(5) 0.0434(3) Uani 1 1 d 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

C24 0.047(7) 0.065(9) 0.043(6) -0.014(6) 0.034(5) -0.019(6)
C25 0.045(6) 0.068(8) 0.041(6) -0.008(5) 0.021(5) -0.006(6)
C26 0.053(5) 0.075(9) 0.043(6) -0.013(5) 0.020(5) -0.012(6)
C27 0.056(6) 0.087(9) 0.051(6) -0.009(7) 0.022(5) -0.008(6)
C28 0.082(9) 0.131(15) 0.049(7) 0.002(9) -0.002(6) -0.016(11)
C29 0.074(10) 0.087(11) 0.056(6) -0.030(8) 0.020(7) -0.008(8)
C30 0.059(8) 0.072(9) 0.064(6) -0.019(6) 0.030(6) -0.006(6)
C24A 0.043(5) 0.052(7) 0.051(6) -0.016(5) 0.033(5) -0.011(5)
C25A 0.045(6) 0.068(8) 0.040(5) -0.019(4) 0.015(4) -0.009(6)
C26A 0.048(5) 0.086(8) 0.042(5) -0.019(5) 0.021(4) 0.006(6)
C27A 0.040(5) 0.087(10) 0.041(4) -0.017(6) 0.027(4) 0.003(6)
C28A 0.060(6) 0.150(14) 0.054(6) -0.017(8) 0.026(5) -0.015(8)
C29A 0.048(5) 0.085(8) 0.050(5) -0.038(5) 0.030(4) -0.007(5)
C30A 0.042(6) 0.059(7) 0.054(5) -0.022(5) 0.031(4) -0.004(4)
C1 0.090(3) 0.052(2) 0.042(2) -0.0103(17) 0.038(2) -0.017(2)
C2 0.062(2) 0.047(2) 0.043(2) -0.0088(16) 0.0313(18) -0.0214(19)
C3 0.063(3) 0.072(3) 0.059(3) -0.017(2) 0.042(2) -0.017(2)
C4 0.050(2) 0.097(3) 0.065(3) -0.016(2) 0.035(2) 0.000(2)
C5 0.043(2) 0.091(3) 0.049(2) -0.012(2) 0.0256(18) -0.002(2)
C6 0.043(2) 0.048(2) 0.0414(19) -0.0085(15) 0.0249(16) -0.0114(16)
C7 0.055(2) 0.0408(19) 0.0358(18) -0.0053(15) 0.0258(17) -0.0166(16)
C8 0.066(2) 0.0415(19) 0.0365(18) 0.0043(15) 0.0207(18) -0.0021(18)
C9 0.055(2) 0.042(2) 0.0414(19) 0.0035(15) 0.0212(17) -0.0007(17)
C10 0.0421(19) 0.0364(18) 0.0297(16) -0.0019(13) 0.0145(14) -0.0025(15)
C11 0.0399(19) 0.048(2) 0.0306(17) -0.0082(14) 0.0181(15) -0.0078(15)
C12 0.053(2) 0.063(2) 0.054(2) -0.0181(19) 0.0267(19) -0.021(2)
C13 0.0355(18) 0.060(2) 0.0340(17) -0.0048(16) 0.0145(15) 0.0044(17)
C14 0.0366(18) 0.058(2) 0.0307(17) -0.0023(15) 0.0144(15) 0.0023(16)
C15 0.0322(17) 0.0398(18) 0.0267(15) -0.0032(13) 0.0101(13) 0.0028(14)
C16 0.0384(18) 0.0385(18) 0.0331(16) -0.0001(14) 0.0159(14) 0.0020(14)
C17 0.063(2) 0.039(2) 0.054(2) -0.0060(16) 0.0320(19) -0.0024(17)
C18 0.0387(19) 0.047(2) 0.0353(17) 0.0103(15) 0.0119(15) 0.0068(16)
C19 0.0371(19) 0.049(2) 0.0447(19) 0.0064(16) 0.0178(16) 0.0087(16)
C20 0.0373(18) 0.0406(18) 0.0337(17) -0.0017(14) 0.0194(15) 0.0034(14)
C21 0.0352(18) 0.0453(19) 0.0281(16) -0.0009(14) 0.0132(14) 0.0045(15)
C22 0.049(2) 0.064(2) 0.0412(19) -0.0159(17) 0.0246(17) -0.0060(18)
C23 0.046(2) 0.062(2) 0.0341(18) 0.0073(16) 0.0182(16) 0.0082(17)
C31 0.228(15) 0.292(17) 0.40(2) 0.138(15) -0.015(18) 0.012(16)
C32 0.238(17) 0.38(2) 0.264(15) 0.045(15) -0.061(14) 0.064(18)
C33 0.178(10) 0.398(19) 0.194(10) -0.111(12) -0.060(8) 0.163(12)
N1 0.0381(16) 0.0444(17) 0.0395(15) -0.0043(12) 0.0217(13) 0.0018(13)
O1 0.0624(16) 0.0496(14) 0.0477(14) 0.0003(11) 0.0366(13) 0.0006(12)
O2 0.084(2) 0.0399(15) 0.094(2) -0.0025(13) 0.0589(18) 0.0063(13)
S1 0.0520(6) 0.0409(5) 0.0491(5) -0.0031(4) 0.0327(4) -0.0003(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

C24 C25 1.392(13) . ?
C24 C30 1.402(12) . ?
C24 S1 1.768(7) . ?
C25 C26 1.384(12) . ?
C26 C27 1.364(13) . ?
C27 C29 1.366(14) . ?
C27 C28 1.519(13) . ?
C29 C30 1.384(13) . ?
C24A C25A 1.373(11) . ?
C24A C30A 1.379(11) . ?
C24A S1 1.754(6) . ?
C25A C26A 1.381(11) . ?
C26A C27A 1.374(12) . ?
C27A C29A 1.382(13) . ?
C27A C28A 1.521(11) . ?
C29A C30A 1.380(12) . ?
C1 C2 1.516(5) . ?
C2 C3 1.373(5) . ?
C2 C7 1.404(4) . ?
C3 C4 1.370(6) . ?
C4 C5 1.395(5) . ?
C5 C6 1.392(5) . ?
C6 C7 1.395(5) . ?
C6 C11 1.544(4) . ?
C7 C8 1.515(5) . ?
C8 C9 1.518(5) . ?
C9 C10 1.533(4) . ?
C10 C11 1.548(4) . ?
C10 C16 1.566(4) . ?
C11 C13 1.542(4) . ?
C11 C12 1.550(5) . ?
C13 C14 1.527(4) . ?
C14 C15 1.529(4) . ?
C15 C16 1.551(4) . ?
C15 C21 1.560(4) . ?
C16 C17 1.541(4) . ?
C16 C18 1.542(4) . ?
C18 C19 1.525(4) . ?
C19 C20 1.518(4) . ?
C20 N1 1.479(4) . ?
C20 C21 1.541(4) . ?
C21 C22 1.531(4) . ?
C21 C23 1.536(4) . ?
C31 C32 1.385(15) . ?
C31 C31 1.464(16) 3_665 ?
C32 C33 1.369(12) . ?
N1 S1 1.609(3) . ?
O1 S1 1.436(2) . ?
O2 S1 1.422(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

C25 C24 C30 115.2(11) . . ?
C25 C24 S1 119.0(15) . . ?
C30 C24 S1 125.2(15) . . ?
C26 C25 C24 121.1(13) . . ?
C27 C26 C25 123.2(13) . . ?
C26 C27 C29 116.4(12) . . ?
C26 C27 C28 125.0(13) . . ?
C29 C27 C28 118.5(13) . . ?
C27 C29 C30 122.0(13) . . ?
C29 C30 C24 121.9(12) . . ?
C25A C24A C30A 123.4(9) . . ?
C25A C24A S1 119.3(12) . . ?
C30A C24A S1 117.3(12) . . ?
C24A C25A C26A 117.6(12) . . ?
C27A C26A C25A 121.4(11) . . ?
C26A C27A C29A 118.6(9) . . ?
C26A C27A C28A 119.3(11) . . ?
C29A C27A C28A 122.0(11) . . ?
C30A C29A C27A 122.1(10) . . ?
C24A C30A C29A 116.7(10) . . ?
C3 C2 C7 119.5(3) . . ?
C3 C2 C1 119.8(3) . . ?
C7 C2 C1 120.7(3) . . ?
C4 C3 C2 121.0(3) . . ?
C3 C4 C5 119.7(4) . . ?
C6 C5 C4 120.8(4) . . ?
C5 C6 C7 118.5(3) . . ?
C5 C6 C11 119.2(3) . . ?
C7 C6 C11 122.3(3) . . ?
C6 C7 C2 120.4(3) . . ?
C6 C7 C8 121.4(3) . . ?
C2 C7 C8 118.2(3) . . ?
C7 C8 C9 114.7(3) . . ?
C8 C9 C10 110.1(3) . . ?
C9 C10 C11 109.1(3) . . ?
C9 C10 C16 115.3(3) . . ?
C11 C10 C16 117.4(2) . . ?
C13 C11 C6 109.9(3) . . ?
C13 C11 C10 107.7(2) . . ?
C6 C11 C10 108.6(2) . . ?
C13 C11 C12 108.8(3) . . ?
C6 C11 C12 106.5(2) . . ?
C10 C11 C12 115.3(3) . . ?
C14 C13 C11 113.2(3) . . ?
C13 C14 C15 111.0(2) . . ?
C14 C15 C16 110.7(3) . . ?
C14 C15 C21 114.1(2) . . ?
C16 C15 C21 117.5(2) . . ?
C17 C16 C18 108.3(3) . . ?
C17 C16 C15 114.5(3) . . ?
C18 C16 C15 107.0(2) . . ?
C17 C16 C10 111.6(3) . . ?
C18 C16 C10 108.5(2) . . ?
C15 C16 C10 106.7(2) . . ?
C19 C18 C16 113.5(3) . . ?
C20 C19 C18 111.8(3) . . ?
N1 C20 C19 111.1(2) . . ?
N1 C20 C21 110.3(2) . . ?
C19 C20 C21 113.6(3) . . ?
C22 C21 C23 107.7(3) . . ?
C22 C21 C20 110.9(3) . . ?
C23 C21 C20 108.0(3) . . ?
C22 C21 C15 114.7(3) . . ?
C23 C21 C15 109.2(2) . . ?
C20 C21 C15 106.2(2) . . ?
C32 C31 C31 102.3(14) . 3_665 ?
C33 C32 C31 108.4(11) . . ?
C20 N1 S1 121.4(2) . . ?
O2 S1 O1 119.25(15) . . ?
O2 S1 N1 108.18(16) . . ?
O1 S1 N1 105.65(14) . . ?
O2 S1 C24A 105.7(7) . . ?
O1 S1 C24A 109.1(14) . . ?
N1 S1 C24A 108.6(19) . . ?
O2 S1 C24 110.6(9) . . ?
O1 S1 C24 105.5(15) . . ?
N1 S1 C24 107(2) . . ?
C24A S1 C24 4.9(14) . . ?

_diffrn_measured_fraction_theta_max 0.995

_diffrn_reflns_theta_full        25.08

_diffrn_measured_fraction_theta_full 0.995

_refine_diff_density_max         0.695

_refine_diff_density_min         -0.461

_refine_diff_density_rms         0.136