# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2004

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Dr Alan Armstrong'
_publ_contact_author_address     
;
Department of Chemistry
Imperial College London
Imperial College London
South Kensington
London
SW7 2AZ
UNITED KINGDOM
;

_publ_contact_author_email       A.ARMSTRONG@IMPERIAL.AC.UK

_publ_section_title              
;
Aminative Rearrangement of
2-Alkoxy-3,4-dihydro-2H-pyrans: A Novel Stereocontrolled Route to
Substituted Pyrrolidines
;
loop_
_publ_author_name
'Alan Armstrong'
'Graham R. Cumming'
'Kurt Pike'

data_AA0304b
_database_code_depnum_ccdc_archive 'CCDC 227678'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H23 N O3 S'
_chemical_formula_weight         309.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   7.224(3)
_cell_length_b                   14.064(6)
_cell_length_c                   32.806(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3333(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    26
_cell_measurement_theta_min      11.13
_cell_measurement_theta_max      24.94

_exptl_crystal_description       platy_needles
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1328
_exptl_absorpt_coefficient_mu    1.802
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.4575
_exptl_absorpt_correction_T_max  0.8224
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2456
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_theta_min         2.69
_diffrn_reflns_theta_max         60.00
_reflns_number_total             2456
_reflns_number_gt                1893
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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.

The S(6) tosyl group is disordered, and three orientations were identified
with occupanices of ca. 88%, 6% and 6%. Only the non-hydrogen atoms of the
major occupoancy orientation were refined anisotropically, the others being
refined isotropically.

;

_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^)+(0.0500P)^2^+2.4836P] 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         2456
_refine_ls_number_parameters     241
_refine_ls_number_restraints     278
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0720
_refine_ls_wR_factor_ref         0.1755
_refine_ls_wR_factor_gt          0.1668
_refine_ls_goodness_of_fit_ref   1.346
_refine_ls_restrained_S_all      1.276
_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
N1 N 0.4633(4) -0.2619(3) 0.12764(9) 0.0534(8) Uani 1 1 d . . .
C2 C 0.4110(6) -0.3448(3) 0.15266(12) 0.0554(10) Uani 1 1 d . A 1
H2A H 0.3199 -0.3834 0.1379 0.066 Uiso 1 1 calc R A 1
C3 C 0.5970(7) -0.4008(3) 0.15623(13) 0.0614(11) Uani 1 1 d . A 1
H3A H 0.6054 -0.4410 0.1319 0.074 Uiso 1 1 calc R A 1
C4 C 0.7423(7) -0.3232(4) 0.15123(15) 0.0734(13) Uani 1 1 d . A 1
H4A H 0.7598 -0.2887 0.1765 0.088 Uiso 1 1 calc R A 1
H4B H 0.8599 -0.3500 0.1428 0.088 Uiso 1 1 calc R A 1
C5 C 0.6655(6) -0.2591(4) 0.11877(14) 0.0660(12) Uani 1 1 d . A 1
H5A H 0.7143 -0.1951 0.1212 0.079 Uiso 1 1 calc R A 1
H5B H 0.6921 -0.2834 0.0917 0.079 Uiso 1 1 calc R A 1
S6 S 0.3168(2) -0.21916(14) 0.09499(4) 0.0494(4) Uani 0.883(3) 1 d PDU A 1
O7 O 0.1387(5) -0.2235(4) 0.11381(12) 0.0633(11) Uani 0.883(3) 1 d PDU A 1
O8 O 0.3910(6) -0.1303(2) 0.08121(10) 0.0724(11) Uani 0.883(3) 1 d PDU A 1
C9 C 0.3131(4) -0.29635(17) 0.05267(6) 0.0418(9) Uani 0.883(3) 1 d PGDU A 1
C10 C 0.4099(4) -0.27342(18) 0.01739(8) 0.0547(12) Uani 0.883(3) 1 d PGDU A 1
H10A H 0.4761 -0.2168 0.0159 0.066 Uiso 0.883(3) 1 calc PR A 1
C11 C 0.4075(4) -0.3351(2) -0.01573(6) 0.0607(12) Uani 0.883(3) 1 d PGDU A 1
H11A H 0.4722 -0.3197 -0.0393 0.073 Uiso 0.883(3) 1 calc PR A 1
C12 C 0.3084(4) -0.41963(19) -0.01356(7) 0.0543(11) Uani 0.883(3) 1 d PGDU A 1
C13 C 0.2117(4) -0.44257(17) 0.02172(8) 0.0540(11) Uani 0.883(3) 1 d PGDU A 1
H13A H 0.1454 -0.4992 0.0232 0.065 Uiso 0.883(3) 1 calc PR A 1
C14 C 0.2140(4) -0.38093(19) 0.05484(6) 0.0503(11) Uani 0.883(3) 1 d PGDU A 1
H14A H 0.1493 -0.3963 0.0784 0.060 Uiso 0.883(3) 1 calc PR A 1
C15 C 0.3037(10) -0.4864(5) -0.04982(17) 0.0814(19) Uani 0.883(3) 1 d PD A 1
H15A H 0.1951 -0.4738 -0.0658 0.122 Uiso 0.883(3) 1 calc PR A 1
H15B H 0.3008 -0.5510 -0.0404 0.122 Uiso 0.883(3) 1 calc PR A 1
H15C H 0.4121 -0.4767 -0.0662 0.122 Uiso 0.883(3) 1 calc PR A 1
S6' S 0.3252(18) -0.3197(10) 0.0938(4) 0.035(4) Uiso 0.061(3) 1 d PDU A 2
O7' O 0.396(6) -0.4077(18) 0.0802(11) 0.060(11) Uiso 0.061(3) 1 d PDU A 2
O8' O 0.154(4) -0.311(3) 0.1151(10) 0.045(9) Uiso 0.061(3) 1 d PDU A 2
C9' C 0.317(5) -0.2408(17) 0.0518(7) 0.020(9) Uiso 0.061(3) 1 d PGDU A 2
C10' C 0.226(5) -0.1539(19) 0.0552(7) 0.042(9) Uiso 0.061(3) 1 d PGDU A 2
H10B H 0.1674 -0.1378 0.0795 0.050 Uiso 0.061(3) 1 calc PR A 2
C11' C 0.224(5) -0.0912(17) 0.0225(8) 0.049(10) Uiso 0.061(3) 1 d PGDU A 2
H11B H 0.1636 -0.0331 0.0248 0.058 Uiso 0.061(3) 1 calc PR A 2
C12' C 0.312(5) -0.1152(19) -0.0137(7) 0.036(10) Uiso 0.061(3) 1 d PGDU A 2
C13' C 0.403(5) -0.202(2) -0.0172(6) 0.042(9) Uiso 0.061(3) 1 d PGDU A 2
H13B H 0.4620 -0.2182 -0.0414 0.051 Uiso 0.061(3) 1 calc PR A 2
C14' C 0.405(5) -0.2648(18) 0.0155(8) 0.055(9) Uiso 0.061(3) 1 d PGDU A 2
H14B H 0.4658 -0.3229 0.0132 0.065 Uiso 0.061(3) 1 calc PR A 2
C15' C 0.311(9) -0.049(3) -0.0504(11) 0.048(14) Uiso 0.061(3) 1 d PDU A 2
H15D H 0.3283 -0.0861 -0.0748 0.072 Uiso 0.061(3) 1 calc PR A 2
H15E H 0.4084 -0.0037 -0.0479 0.072 Uiso 0.061(3) 1 calc PR A 2
H15F H 0.1937 -0.0171 -0.0518 0.072 Uiso 0.061(3) 1 calc PR A 2
S6" S 0.323(3) -0.2527(17) 0.0944(7) 0.048(8) Uiso 0.055(3) 1 d PDU A 3
O7" O 0.409(6) -0.337(2) 0.0795(11) 0.044(10) Uiso 0.055(3) 1 d PDU A 3
O8" O 0.141(6) -0.258(4) 0.1115(19) 0.057(19) Uiso 0.055(3) 1 d PDU A 3
C9" C 0.320(5) -0.1725(18) 0.0530(7) 0.019(9) Uiso 0.055(3) 1 d PGDU A 3
C10" C 0.224(5) -0.087(2) 0.0553(8) 0.047(10) Uiso 0.055(3) 1 d PGDU A 3
H10C H 0.1636 -0.0702 0.0793 0.056 Uiso 0.055(3) 1 calc PR A 3
C11" C 0.217(6) -0.027(2) 0.0217(9) 0.046(11) Uiso 0.055(3) 1 d PGDU A 3
H11C H 0.1526 0.0303 0.0233 0.055 Uiso 0.055(3) 1 calc PR A 3
C12" C 0.307(6) -0.052(2) -0.0142(8) 0.042(13) Uiso 0.055(3) 1 d PGDU A 3
C13" C 0.403(6) -0.137(2) -0.0165(7) 0.042(10) Uiso 0.055(3) 1 d PGDU A 3
H13C H 0.4628 -0.1543 -0.0405 0.050 Uiso 0.055(3) 1 calc PR A 3
C14" C 0.409(5) -0.1977(19) 0.0171(8) 0.042(10) Uiso 0.055(3) 1 d PGDU A 3
H14C H 0.4737 -0.2548 0.0155 0.050 Uiso 0.055(3) 1 calc PR A 3
C15" C 0.306(11) 0.011(4) -0.0517(12) 0.045(17) Uiso 0.055(3) 1 d PDU A 3
H15G H 0.3019 -0.0282 -0.0757 0.068 Uiso 0.055(3) 1 calc PR A 3
H15H H 0.4168 0.0487 -0.0521 0.068 Uiso 0.055(3) 1 calc PR A 3
H15I H 0.1999 0.0517 -0.0511 0.068 Uiso 0.055(3) 1 calc PR A 3
C16 C 0.3286(7) -0.3119(4) 0.19348(14) 0.0681(13) Uani 1 1 d . A 1
O16 O 0.1980(6) -0.3568(4) 0.20684(13) 0.1156(16) Uani 1 1 d . A 1
C17 C 0.4057(8) -0.2318(4) 0.21531(16) 0.0840(15) Uani 1 1 d . A 1
H17A H 0.3805 -0.2385 0.2439 0.126 Uiso 1 1 calc R A 1
H17B H 0.3507 -0.1740 0.2055 0.126 Uiso 1 1 calc R A 1
H17C H 0.5371 -0.2296 0.2110 0.126 Uiso 1 1 calc R A 1
C18 C 0.6163(8) -0.4668(4) 0.19278(14) 0.0750(14) Uani 1 1 d . A 1
H18A H 0.5957 -0.4291 0.2175 0.090 Uiso 1 1 calc R A 1
C19 C 0.4688(11) -0.5454(4) 0.1913(2) 0.110(2) Uani 1 1 d . A 1
H19A H 0.3481 -0.5171 0.1898 0.165 Uiso 1 1 calc R A 1
H19B H 0.4773 -0.5836 0.2155 0.165 Uiso 1 1 calc R A 1
H19C H 0.4889 -0.5846 0.1678 0.165 Uiso 1 1 calc R A 1
C20 C 0.8120(11) -0.5081(5) 0.1948(2) 0.119(3) Uani 1 1 d . A 1
H20A H 0.8215 -0.5498 0.2179 0.178 Uiso 1 1 calc R A 1
H20B H 0.8999 -0.4573 0.1976 0.178 Uiso 1 1 calc R A 1
H20C H 0.8373 -0.5430 0.1703 0.178 Uiso 1 1 calc R A 1

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
N1 0.0494(18) 0.071(2) 0.0401(16) 0.0107(15) -0.0048(14) -0.0067(17)
C2 0.057(2) 0.063(3) 0.047(2) 0.0066(18) -0.0063(19) -0.009(2)
C3 0.074(3) 0.059(3) 0.052(2) -0.003(2) -0.002(2) 0.005(2)
C4 0.055(2) 0.091(4) 0.074(3) 0.010(3) -0.002(2) 0.004(3)
C5 0.049(2) 0.089(3) 0.060(2) 0.014(2) 0.0000(19) -0.012(2)
S6 0.0580(8) 0.0489(9) 0.0411(6) 0.0024(6) -0.0043(5) 0.0052(7)
O7 0.055(2) 0.083(3) 0.052(2) -0.008(2) 0.0005(14) 0.017(2)
O8 0.105(3) 0.0454(18) 0.066(2) 0.0115(15) -0.011(2) -0.0056(19)
C9 0.040(2) 0.049(3) 0.0358(19) 0.0073(17) -0.0030(16) -0.0006(19)
C10 0.050(2) 0.068(3) 0.046(2) 0.009(2) 0.003(2) -0.010(2)
C11 0.053(3) 0.086(3) 0.043(2) 0.002(2) 0.009(2) -0.004(3)
C12 0.049(2) 0.066(3) 0.048(2) -0.007(2) -0.011(2) 0.015(2)
C13 0.056(3) 0.057(3) 0.049(2) 0.005(2) -0.011(2) -0.003(2)
C14 0.049(2) 0.062(3) 0.040(2) 0.0106(19) -0.0039(18) -0.011(2)
C15 0.081(4) 0.098(5) 0.065(3) -0.028(3) -0.021(3) 0.025(4)
C16 0.060(3) 0.086(3) 0.058(2) 0.016(2) 0.009(2) -0.001(3)
O16 0.102(3) 0.140(4) 0.105(3) 0.017(3) 0.041(3) -0.028(3)
C17 0.088(4) 0.090(4) 0.074(3) -0.016(3) 0.013(3) 0.006(3)
C18 0.107(4) 0.062(3) 0.057(2) -0.002(2) -0.012(3) 0.011(3)
C19 0.163(7) 0.071(4) 0.097(4) 0.020(3) -0.023(4) -0.022(4)
C20 0.159(7) 0.099(5) 0.098(4) 0.013(4) -0.030(4) 0.047(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
N1 C2 1.475(5) . ?
N1 C5 1.490(5) . ?
N1 S6" 1.49(2) . ?
N1 S6 1.621(3) . ?
N1 S6' 1.699(13) . ?
C2 C16 1.537(6) . ?
C2 C3 1.561(6) . ?
C3 C18 1.522(6) . ?
C3 C4 1.523(7) . ?
C4 C5 1.501(6) . ?
S6 O7 1.428(4) . ?
S6 O8 1.432(4) . ?
S6 C9 1.762(2) . ?
C9 C10 1.3900 . ?
C9 C14 1.3900 . ?
C10 C11 1.3900 . ?
C11 C12 1.3900 . ?
C12 C13 1.3900 . ?
C12 C15 1.516(6) . ?
C13 C14 1.3900 . ?
S6' O7' 1.411(18) . ?
S6' O8' 1.430(17) . ?
S6' C9' 1.771(13) . ?
C9' C10' 1.3900 . ?
C9' C14' 1.3900 . ?
C10' C11' 1.3900 . ?
C11' C12' 1.3900 . ?
C12' C13' 1.3900 . ?
C12' C15' 1.520(17) . ?
C13' C14' 1.3900 . ?
S6" O7" 1.420(18) . ?
S6" O8" 1.432(18) . ?
S6" C9" 1.767(15) . ?
C9" C10" 1.3900 . ?
C9" C14" 1.3900 . ?
C10" C11" 1.3900 . ?
C11" C12" 1.3900 . ?
C12" C13" 1.3900 . ?
C12" C15" 1.516(17) . ?
C13" C14" 1.3900 . ?
C16 O16 1.216(6) . ?
C16 C17 1.446(8) . ?
C18 C20 1.530(8) . ?
C18 C19 1.537(8) . ?

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 N1 C5 112.3(3) . . ?
C2 N1 S6" 107.6(9) . . ?
C5 N1 S6" 121.2(9) . . ?
C2 N1 S6 119.6(3) . . ?
C5 N1 S6 120.1(3) . . ?
S6" N1 S6 16.9(9) . . ?
C2 N1 S6' 80.5(5) . . ?
C5 N1 S6' 117.4(5) . . ?
S6" N1 S6' 33.5(8) . . ?
S6 N1 S6' 50.4(4) . . ?
N1 C2 C16 110.3(4) . . ?
N1 C2 C3 102.7(3) . . ?
C16 C2 C3 114.8(3) . . ?
C18 C3 C4 117.3(4) . . ?
C18 C3 C2 116.5(4) . . ?
C4 C3 C2 102.9(4) . . ?
C5 C4 C3 104.6(4) . . ?
N1 C5 C4 102.0(3) . . ?
O7 S6 O8 120.7(3) . . ?
O7 S6 N1 106.7(2) . . ?
O8 S6 N1 106.7(2) . . ?
O7 S6 C9 107.5(2) . . ?
O8 S6 C9 107.10(18) . . ?
N1 S6 C9 107.57(19) . . ?
C10 C9 C14 120.0 . . ?
C10 C9 S6 120.36(16) . . ?
C14 C9 S6 119.64(16) . . ?
C9 C10 C11 120.0 . . ?
C12 C11 C10 120.0 . . ?
C13 C12 C11 120.0 . . ?
C13 C12 C15 119.9(3) . . ?
C11 C12 C15 120.1(3) . . ?
C14 C13 C12 120.0 . . ?
C13 C14 C9 120.0 . . ?
O7' S6' O8' 123(2) . . ?
O7' S6' N1 115(2) . . ?
O8' S6' N1 98.5(17) . . ?
O7' S6' C9' 108.3(16) . . ?
O8' S6' C9' 107.4(17) . . ?
N1 S6' C9' 103.2(14) . . ?
C10' C9' C14' 120.0 . . ?
C10' C9' S6' 120.2(13) . . ?
C14' C9' S6' 119.8(13) . . ?
C9' C10' C11' 120.0 . . ?
C10' C11' C12' 120.0 . . ?
C13' C12' C11' 120.0 . . ?
C13' C12' C15' 118.3(18) . . ?
C11' C12' C15' 121.7(18) . . ?
C12' C13' C14' 120.0 . . ?
C13' C14' C9' 120.0 . . ?
O7" S6" O8" 120(3) . . ?
O7" S6" N1 83(2) . . ?
O8" S6" N1 109(3) . . ?
O7" S6" C9" 105.8(17) . . ?
O8" S6" C9" 109(2) . . ?
N1 S6" C9" 129(2) . . ?
C10" C9" C14" 120.0 . . ?
C10" C9" S6" 121.2(13) . . ?
C14" C9" S6" 118.8(13) . . ?
C11" C10" C9" 120.0 . . ?
C12" C11" C10" 120.0 . . ?
C11" C12" C13" 120.0 . . ?
C11" C12" C15" 122.6(19) . . ?
C13" C12" C15" 117.4(19) . . ?
C14" C13" C12" 120.0 . . ?
C13" C14" C9" 120.0 . . ?
O16 C16 C17 121.6(5) . . ?
O16 C16 C2 117.3(5) . . ?
C17 C16 C2 121.1(4) . . ?
C3 C18 C20 110.6(5) . . ?
C3 C18 C19 110.5(4) . . ?
C20 C18 C19 111.6(5) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        60.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.066

#===END