# Supplementary Material (ESI) for Organic & Biomolecular Chemistry
# This journal is © The Royal Society of Chemistry 2005



data_global
_journal_name_full               Org.Biomol.Chem.

_journal_coden_Cambridge         0177

_publ_contact_author_name        'Prof Richard Taylor'
_publ_contact_author_address     
;
Department of Chemistry
University of York
Heslington
York
North Yorkshire
YO10 5DD
UNITED KINGDOM
;

_publ_contact_author_email       RJKT1@YORK.AC.UK

_publ_section_title              
;
Unexpected Z-selectivity in the Ramberg-Backlund
reaction of diarylsulfones leading to cis-stilbenes: the effect of aryl
substituents and application in the synthesis of the integrastatin
nucleus
;
loop_
_publ_author_name
R.Taylor
'Jonathan Foot'
'Gerard M.P.Giblin'
'Adrian C.Whitwood'

data_rjt0303m
_database_code_depnum_ccdc_archive 'CCDC 219622'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H16 O2'
_chemical_formula_sum            'C17 H16 O2'
_chemical_formula_weight         252.30

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   19.3595(13)
_cell_length_b                   8.8441(6)
_cell_length_c                   16.7833(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.7010(10)
_cell_angle_gamma                90.00
_cell_volume                     2589.3(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    115(2)
_cell_measurement_reflns_used    5322
_cell_measurement_theta_min      2.58
_cell_measurement_theta_max      28.31

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.27
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1072
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.898
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_process_details   'SADABS v2.03; (Sheldrick)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      115(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            9228
_diffrn_reflns_av_R_equivalents  0.0151
_diffrn_reflns_av_sigmaI/netI    0.0175
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.34
_diffrn_reflns_theta_max         28.31
_reflns_number_total             3209
_reflns_number_gt                2861
_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 F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² 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/[σ²(Fo²)+(0.0608P)²+1.2020P] where P=(Fo²+2Fc²)/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         3209
_refine_ls_number_parameters     174
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0383
_refine_ls_wR_factor_ref         0.1087
_refine_ls_wR_factor_gt          0.1048
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_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
O1 O 0.09599(4) 0.05535(8) 0.10370(4) 0.02317(17) Uani 1 1 d . . .
O2 O 0.09918(4) 0.09585(7) 0.24224(4) 0.02250(16) Uani 1 1 d . . .
C10 C 0.19767(5) 0.20793(10) 0.21104(6) 0.0233(2) Uani 1 1 d . . .
C7 C 0.04729(6) 0.38075(11) 0.17430(7) 0.0242(2) Uani 1 1 d . . .
C15 C 0.16541(5) 0.12702(11) 0.13197(6) 0.0224(2) Uani 1 1 d . . .
C3 C -0.04699(6) 0.27247(12) 0.03854(7) 0.0262(2) Uani 1 1 d . . .
H3 H -0.0674 0.1874 0.0011 0.031 Uiso 1 1 calc R . .
C14 C 0.20376(6) 0.11114(12) 0.07871(7) 0.0269(2) Uani 1 1 d . . .
H14 H 0.1816 0.0536 0.0257 0.032 Uiso 1 1 calc R . .
C1 C 0.05135(5) 0.09879(10) 0.15089(6) 0.02096(19) Uani 1 1 d . . .
C9 C 0.15652(6) 0.21459(11) 0.27018(6) 0.0239(2) Uani 1 1 d . . .
C2 C 0.01657(5) 0.25477(10) 0.12029(6) 0.0220(2) Uani 1 1 d . . .
C16 C -0.00672(6) -0.02632(11) 0.13233(6) 0.0248(2) Uani 1 1 d . . .
H16A H 0.0198 -0.1204 0.1594 0.037 Uiso 1 1 calc R . .
H16B H -0.0352 -0.0404 0.0683 0.037 Uiso 1 1 calc R . .
H16C H -0.0424 0.0007 0.1572 0.037 Uiso 1 1 calc R . .
C5 C -0.05053(6) 0.53867(12) 0.06612(8) 0.0318(2) Uani 1 1 d . . .
H5 H -0.0736 0.6352 0.0481 0.038 Uiso 1 1 calc R . .
C8 C 0.11575(6) 0.36495(11) 0.26267(7) 0.0268(2) Uani 1 1 d . . .
H8A H 0.0988 0.3722 0.3103 0.032 Uiso 1 1 calc R . .
H8B H 0.1520 0.4488 0.2705 0.032 Uiso 1 1 calc R . .
C4 C -0.08045(6) 0.41362(13) 0.01188(7) 0.0310(2) Uani 1 1 d . . .
H4 H -0.1239 0.4247 -0.0435 0.037 Uiso 1 1 calc R . .
C11 C 0.26835(6) 0.27871(12) 0.23365(7) 0.0295(2) Uani 1 1 d . . .
H11 H 0.2907 0.3369 0.2864 0.035 Uiso 1 1 calc R . .
C6 C 0.01304(6) 0.52208(11) 0.14642(7) 0.0291(2) Uani 1 1 d . . .
H6 H 0.0337 0.6080 0.1831 0.035 Uiso 1 1 calc R . .
C12 C 0.30635(6) 0.26537(12) 0.18054(8) 0.0322(2) Uani 1 1 d . . .
H12 H 0.3542 0.3146 0.1967 0.039 Uiso 1 1 calc R . .
C17 C 0.20927(6) 0.17804(13) 0.36620(7) 0.0314(2) Uani 1 1 d . . .
H17A H 0.1793 0.1740 0.4005 0.047 Uiso 1 1 calc R . .
H17B H 0.2486 0.2566 0.3905 0.047 Uiso 1 1 calc R . .
H17C H 0.2339 0.0799 0.3694 0.047 Uiso 1 1 calc R . .
C13 C 0.27449(6) 0.18002(13) 0.10371(7) 0.0308(2) Uani 1 1 d . . .
H13 H 0.3012 0.1687 0.0681 0.037 Uiso 1 1 calc R . .


_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 C15 1.3712(11) . ?
O1 C1 1.4544(11) . ?
O2 C1 1.4061(11) . ?
O2 C9 1.4503(11) . ?
C10 C15 1.3945(13) . ?
C10 C11 1.3992(14) . ?
C10 C9 1.5195(14) . ?
C7 C2 1.3962(13) . ?
C7 C6 1.3970(14) . ?
C7 C8 1.5068(14) . ?
C15 C14 1.3947(14) . ?
C3 C4 1.3881(14) . ?
C3 C2 1.3988(13) . ?
C3 H3 0.9500 . ?
C14 C13 1.3871(15) . ?
C14 H14 0.9500 . ?
C1 C16 1.5105(13) . ?
C1 C2 1.5232(13) . ?
C9 C17 1.5222(13) . ?
C9 C8 1.5235(14) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C5 C6 1.3836(16) . ?
C5 C4 1.3892(16) . ?
C5 H5 0.9500 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C4 H4 0.9500 . ?
C11 C12 1.3852(16) . ?
C11 H11 0.9500 . ?
C6 H6 0.9500 . ?
C12 C13 1.3867(17) . ?
C12 H12 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C13 H13 0.9500 . ?

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
C15 O1 C1 114.47(7) . . ?
C1 O2 C9 112.89(7) . . ?
C15 C10 C11 117.99(9) . . ?
C15 C10 C9 119.76(8) . . ?
C11 C10 C9 122.24(9) . . ?
C2 C7 C6 119.33(9) . . ?
C2 C7 C8 120.68(9) . . ?
C6 C7 C8 119.98(9) . . ?
O1 C15 C10 122.25(8) . . ?
O1 C15 C14 116.49(8) . . ?
C10 C15 C14 121.23(9) . . ?
C4 C3 C2 120.39(10) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C13 C14 C15 119.47(10) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
O2 C1 O1 108.84(7) . . ?
O2 C1 C16 106.90(7) . . ?
O1 C1 C16 105.01(7) . . ?
O2 C1 C2 111.73(7) . . ?
O1 C1 C2 109.62(7) . . ?
C16 C1 C2 114.41(8) . . ?
O2 C9 C10 107.77(7) . . ?
O2 C9 C17 104.86(8) . . ?
C10 C9 C17 112.48(8) . . ?
O2 C9 C8 107.99(8) . . ?
C10 C9 C8 112.30(8) . . ?
C17 C9 C8 111.01(8) . . ?
C7 C2 C3 119.56(9) . . ?
C7 C2 C1 120.15(8) . . ?
C3 C2 C1 120.28(8) . . ?
C1 C16 H16A 109.5 . . ?
C1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C6 C5 C4 119.72(10) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C7 C8 C9 111.43(8) . . ?
C7 C8 H8A 109.3 . . ?
C9 C8 H8A 109.3 . . ?
C7 C8 H8B 109.3 . . ?
C9 C8 H8B 109.3 . . ?
H8A C8 H8B 108.0 . . ?
C3 C4 C5 120.07(10) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C12 C11 C10 121.15(10) . . ?
C12 C11 H11 119.4 . . ?
C10 C11 H11 119.4 . . ?
C5 C6 C7 120.91(10) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C11 C12 C13 119.90(9) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C9 C17 H17A 109.5 . . ?
C9 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C9 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C12 C13 C14 120.20(10) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?

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 O1 C15 C10 13.55(12) . . . . ?
C1 O1 C15 C14 -168.37(8) . . . . ?
C11 C10 C15 O1 -179.23(8) . . . . ?
C9 C10 C15 O1 1.80(14) . . . . ?
C11 C10 C15 C14 2.79(14) . . . . ?
C9 C10 C15 C14 -176.18(9) . . . . ?
O1 C15 C14 C13 -179.63(9) . . . . ?
C10 C15 C14 C13 -1.54(15) . . . . ?
C9 O2 C1 O1 69.14(9) . . . . ?
C9 O2 C1 C16 -177.93(7) . . . . ?
C9 O2 C1 C2 -52.04(10) . . . . ?
C15 O1 C1 O2 -47.16(10) . . . . ?
C15 O1 C1 C16 -161.33(7) . . . . ?
C15 O1 C1 C2 75.31(9) . . . . ?
C1 O2 C9 C10 -51.49(10) . . . . ?
C1 O2 C9 C17 -171.52(7) . . . . ?
C1 O2 C9 C8 70.04(9) . . . . ?
C15 C10 C9 O2 15.95(12) . . . . ?
C11 C10 C9 O2 -162.97(8) . . . . ?
C15 C10 C9 C17 131.05(9) . . . . ?
C11 C10 C9 C17 -47.87(12) . . . . ?
C15 C10 C9 C8 -102.86(10) . . . . ?
C11 C10 C9 C8 78.22(11) . . . . ?
C6 C7 C2 C3 1.20(14) . . . . ?
C8 C7 C2 C3 -179.99(9) . . . . ?
C6 C7 C2 C1 -177.86(8) . . . . ?
C8 C7 C2 C1 0.95(14) . . . . ?
C4 C3 C2 C7 -1.34(14) . . . . ?
C4 C3 C2 C1 177.72(8) . . . . ?
O2 C1 C2 C7 15.84(12) . . . . ?
O1 C1 C2 C7 -104.90(9) . . . . ?
C16 C1 C2 C7 137.48(9) . . . . ?
O2 C1 C2 C3 -163.21(8) . . . . ?
O1 C1 C2 C3 76.05(10) . . . . ?
C16 C1 C2 C3 -41.58(12) . . . . ?
C2 C7 C8 C9 15.97(13) . . . . ?
C6 C7 C8 C9 -165.24(9) . . . . ?
O2 C9 C8 C7 -48.47(11) . . . . ?
C10 C9 C8 C7 70.21(10) . . . . ?
C17 C9 C8 C7 -162.90(8) . . . . ?
C2 C3 C4 C5 0.49(15) . . . . ?
C6 C5 C4 C3 0.50(15) . . . . ?
C15 C10 C11 C12 -1.85(15) . . . . ?
C9 C10 C11 C12 177.09(9) . . . . ?
C4 C5 C6 C7 -0.63(15) . . . . ?
C2 C7 C6 C5 -0.23(15) . . . . ?
C8 C7 C6 C5 -179.04(9) . . . . ?
C10 C11 C12 C13 -0.34(16) . . . . ?
C11 C12 C13 C14 1.66(16) . . . . ?
C15 C14 C13 C12 -0.73(15) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        28.31
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.205
_refine_diff_density_rms         0.041

data_rjt0413m
_database_code_depnum_ccdc_archive 'CCDC 257403'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H14 O3'
_chemical_formula_sum            'C17 H14 O3'
_chemical_formula_weight         266.28

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'

_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                   9.2508(9)
_cell_length_b                   9.3130(9)
_cell_length_c                   15.5363(15)
_cell_angle_alpha                100.325(2)
_cell_angle_beta                 90.360(2)
_cell_angle_gamma                99.592(2)
_cell_volume                     1297.5(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    115(2)
_cell_measurement_reflns_used    1679
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      23.23

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             560
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.916
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'SADABS v2.03; (Sheldrick)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      115(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            10629
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0604
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.33
_diffrn_reflns_theta_max         25.03
_reflns_number_total             4551
_reflns_number_gt                3241
_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 F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² 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/[σ²(Fo²)+(0.0368P)²+0.3314P] where P=(Fo²+2Fc²)/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         4551
_refine_ls_number_parameters     365
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0427
_refine_ls_wR_factor_ref         0.1019
_refine_ls_wR_factor_gt          0.0917
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_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 0.4213(2) 0.7519(2) 0.34423(13) 0.0210(5) Uani 1 1 d . . .
C2 C 0.4733(2) 0.7408(2) 0.43529(13) 0.0195(5) Uani 1 1 d . . .
C3 C 0.5924(2) 0.6721(2) 0.44741(14) 0.0236(5) Uani 1 1 d . . .
H3 H 0.6409 0.6299 0.3979 0.028 Uiso 1 1 calc R . .
C4 C 0.6410(2) 0.6645(2) 0.53031(14) 0.0277(5) Uani 1 1 d . . .
H4 H 0.7224 0.6171 0.5376 0.033 Uiso 1 1 calc R . .
C5 C 0.5711(2) 0.7259(2) 0.60311(14) 0.0279(5) Uani 1 1 d . . .
H5 H 0.6052 0.7213 0.6602 0.033 Uiso 1 1 calc R . .
C6 C 0.4521(2) 0.7935(2) 0.59261(13) 0.0255(5) Uani 1 1 d . . .
H6 H 0.4045 0.8356 0.6425 0.031 Uiso 1 1 calc R . .
C7 C 0.4014(2) 0.8005(2) 0.50891(13) 0.0221(5) Uani 1 1 d . . .
C8 C 0.2677(2) 0.8653(2) 0.49765(13) 0.0230(5) Uani 1 1 d . . .
C9 C 0.2062(2) 0.8376(2) 0.40367(13) 0.0218(5) Uani 1 1 d . . .
C10 C 0.1315(2) 0.6771(2) 0.38176(12) 0.0206(5) Uani 1 1 d . . .
C11 C -0.0076(2) 0.6291(2) 0.41042(13) 0.0264(5) Uani 1 1 d . . .
H11 H -0.0577 0.6985 0.4451 0.032 Uiso 1 1 calc R . .
C12 C -0.0739(2) 0.4823(3) 0.38924(14) 0.0296(5) Uani 1 1 d . . .
H12 H -0.1682 0.4509 0.4100 0.035 Uiso 1 1 calc R . .
C13 C -0.0022(2) 0.3813(2) 0.33758(14) 0.0286(5) Uani 1 1 d . . .
H13 H -0.0481 0.2806 0.3223 0.034 Uiso 1 1 calc R . .
C14 C 0.1355(2) 0.4257(2) 0.30801(13) 0.0247(5) Uani 1 1 d . . .
H14 H 0.1837 0.3564 0.2717 0.030 Uiso 1 1 calc R . .
C15 C 0.2030(2) 0.5722(2) 0.33182(12) 0.0201(5) Uani 1 1 d . . .
C16 C 0.5428(2) 0.7929(2) 0.28438(13) 0.0262(5) Uani 1 1 d . . .
H16A H 0.5003 0.8042 0.2285 0.039 Uiso 1 1 calc R . .
H16B H 0.6030 0.7148 0.2740 0.039 Uiso 1 1 calc R . .
H16C H 0.6039 0.8866 0.3117 0.039 Uiso 1 1 calc R . .
C17 C 0.1093(2) 0.9470(2) 0.38875(15) 0.0283(5) Uani 1 1 d . . .
H17A H 0.1655 1.0478 0.4027 0.043 Uiso 1 1 calc R . .
H17B H 0.0251 0.9385 0.4266 0.043 Uiso 1 1 calc R . .
H17C H 0.0745 0.9258 0.3273 0.043 Uiso 1 1 calc R . .
O1 O 0.32940(15) 0.85918(15) 0.34759(9) 0.0221(3) Uani 1 1 d . . .
O2 O 0.34180(15) 0.60947(15) 0.30163(8) 0.0219(3) Uani 1 1 d . . .
O3 O 0.20678(17) 0.92602(19) 0.55927(10) 0.0375(4) Uani 1 1 d . . .
C18 C 0.2640(2) 0.9137(2) 1.07535(12) 0.0177(4) Uani 1 1 d . . .
C19 C 0.1279(2) 0.7962(2) 1.07540(13) 0.0178(4) Uani 1 1 d . . .
C20 C 0.0989(2) 0.7263(2) 1.14682(13) 0.0216(5) Uani 1 1 d . . .
H20 H 0.1674 0.7479 1.1951 0.026 Uiso 1 1 calc R . .
C21 C -0.0289(2) 0.6256(2) 1.14820(14) 0.0244(5) Uani 1 1 d . . .
H21 H -0.0476 0.5788 1.1975 0.029 Uiso 1 1 calc R . .
C22 C -0.1299(2) 0.5924(2) 1.07805(14) 0.0249(5) Uani 1 1 d . . .
H22 H -0.2186 0.5251 1.0800 0.030 Uiso 1 1 calc R . .
C23 C -0.1012(2) 0.6574(2) 1.00569(14) 0.0224(5) Uani 1 1 d . . .
H23 H -0.1692 0.6333 0.9571 0.027 Uiso 1 1 calc R . .
C24 C 0.0277(2) 0.7588(2) 1.00354(13) 0.0183(4) Uani 1 1 d . . .
C25 C 0.0629(2) 0.8203(2) 0.92311(13) 0.0180(4) Uani 1 1 d . . .
C26 C 0.2178(2) 0.9063(2) 0.92313(12) 0.0183(5) Uani 1 1 d . . .
C27 C 0.3218(2) 0.7951(2) 0.90666(13) 0.0182(5) Uani 1 1 d . . .
C28 C 0.3364(2) 0.7135(2) 0.82359(13) 0.0199(5) Uani 1 1 d . . .
H28 H 0.2789 0.7265 0.7756 0.024 Uiso 1 1 calc R . .
C29 C 0.4329(2) 0.6142(2) 0.80989(14) 0.0241(5) Uani 1 1 d . . .
H29 H 0.4414 0.5591 0.7530 0.029 Uiso 1 1 calc R . .
C30 C 0.5177(2) 0.5955(2) 0.87988(14) 0.0242(5) Uani 1 1 d . . .
H30 H 0.5860 0.5291 0.8704 0.029 Uiso 1 1 calc R . .
C31 C 0.5034(2) 0.6723(2) 0.96283(14) 0.0216(5) Uani 1 1 d . . .
H31 H 0.5612 0.6587 1.0105 0.026 Uiso 1 1 calc R . .
C32 C 0.4039(2) 0.7700(2) 0.97641(13) 0.0185(5) Uani 1 1 d . . .
C33 C 0.2950(2) 1.0231(2) 1.15980(13) 0.0215(5) Uani 1 1 d . . .
H33A H 0.3806 1.0978 1.1537 0.032 Uiso 1 1 calc R . .
H33B H 0.3150 0.9711 1.2070 0.032 Uiso 1 1 calc R . .
H33C H 0.2097 1.0716 1.1738 0.032 Uiso 1 1 calc R . .
C34 C 0.2320(2) 1.0125(2) 0.85926(13) 0.0244(5) Uani 1 1 d . . .
H34A H 0.1638 1.0825 0.8740 0.037 Uiso 1 1 calc R . .
H34B H 0.2087 0.9568 0.7997 0.037 Uiso 1 1 calc R . .
H34C H 0.3327 1.0671 0.8627 0.037 Uiso 1 1 calc R . .
O4 O 0.25147(14) 0.99668(14) 1.00897(8) 0.0188(3) Uani 1 1 d . . .
O5 O 0.39148(14) 0.84110(15) 1.06108(8) 0.0205(3) Uani 1 1 d . . .
O6 O -0.02032(16) 0.79594(17) 0.85959(9) 0.0290(4) Uani 1 1 d . . .


_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 O1 1.410(2) . ?
C1 O2 1.446(2) . ?
C1 C16 1.507(3) . ?
C1 C2 1.518(3) . ?
C2 C3 1.390(3) . ?
C2 C7 1.401(3) . ?
C3 C4 1.379(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.387(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.379(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.395(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.487(3) . ?
C8 O3 1.213(2) . ?
C8 C9 1.526(3) . ?
C9 O1 1.448(2) . ?
C9 C17 1.510(3) . ?
C9 C10 1.516(3) . ?
C10 C11 1.393(3) . ?
C10 C15 1.394(3) . ?
C11 C12 1.382(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.383(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.380(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.386(3) . ?
C14 H14 0.9500 . ?
C15 O2 1.381(2) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 O4 1.410(2) . ?
C18 O5 1.453(2) . ?
C18 C33 1.503(3) . ?
C18 C19 1.525(3) . ?
C19 C20 1.389(3) . ?
C19 C24 1.402(3) . ?
C20 C21 1.384(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.388(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.377(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.397(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.481(3) . ?
C25 O6 1.213(2) . ?
C25 C26 1.521(3) . ?
C26 O4 1.445(2) . ?
C26 C34 1.514(3) . ?
C26 C27 1.518(3) . ?
C27 C32 1.395(3) . ?
C27 C28 1.395(3) . ?
C28 C29 1.380(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.390(3) . ?
C29 H29 0.9500 . ?
C30 C31 1.376(3) . ?
C30 H30 0.9500 . ?
C31 C32 1.390(3) . ?
C31 H31 0.9500 . ?
C32 O5 1.377(2) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 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 O2 109.26(15) . . ?
O1 C1 C16 106.32(16) . . ?
O2 C1 C16 105.93(16) . . ?
O1 C1 C2 111.32(16) . . ?
O2 C1 C2 109.33(15) . . ?
C16 C1 C2 114.44(17) . . ?
C3 C2 C7 118.85(19) . . ?
C3 C2 C1 121.03(18) . . ?
C7 C2 C1 120.11(19) . . ?
C4 C3 C2 120.9(2) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C3 C4 C5 120.1(2) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C6 C5 C4 120.0(2) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 120.2(2) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C6 C7 C2 119.9(2) . . ?
C6 C7 C8 120.06(19) . . ?
C2 C7 C8 120.00(18) . . ?
O3 C8 C7 122.35(19) . . ?
O3 C8 C9 122.8(2) . . ?
C7 C8 C9 114.62(17) . . ?
O1 C9 C17 106.32(16) . . ?
O1 C9 C10 108.78(16) . . ?
C17 C9 C10 114.04(17) . . ?
O1 C9 C8 107.39(16) . . ?
C17 C9 C8 112.73(17) . . ?
C10 C9 C8 107.34(16) . . ?
C11 C10 C15 118.01(19) . . ?
C11 C10 C9 122.20(19) . . ?
C15 C10 C9 119.78(18) . . ?
C12 C11 C10 121.2(2) . . ?
C12 C11 H11 119.4 . . ?
C10 C11 H11 119.4 . . ?
C11 C12 C13 119.6(2) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C14 C13 C12 120.5(2) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C13 C14 C15 119.4(2) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
O2 C15 C14 116.81(18) . . ?
O2 C15 C10 121.98(18) . . ?
C14 C15 C10 121.18(19) . . ?
C1 C16 H16A 109.5 . . ?
C1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C9 C17 H17A 109.5 . . ?
C9 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C9 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C1 O1 C9 113.86(15) . . ?
C15 O2 C1 114.70(15) . . ?
O4 C18 O5 109.47(15) . . ?
O4 C18 C33 106.66(16) . . ?
O5 C18 C33 106.46(15) . . ?
O4 C18 C19 110.98(15) . . ?
O5 C18 C19 108.87(15) . . ?
C33 C18 C19 114.25(16) . . ?
C20 C19 C24 118.74(18) . . ?
C20 C19 C18 121.00(17) . . ?
C24 C19 C18 120.24(17) . . ?
C21 C20 C19 120.56(19) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
C20 C21 C22 120.5(2) . . ?
C20 C21 H21 119.8 . . ?
C22 C21 H21 119.8 . . ?
C23 C22 C21 119.8(2) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C22 C23 C24 120.16(19) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C23 C24 C19 120.23(18) . . ?
C23 C24 C25 119.84(18) . . ?
C19 C24 C25 119.83(18) . . ?
O6 C25 C24 123.25(19) . . ?
O6 C25 C26 122.02(18) . . ?
C24 C25 C26 114.53(17) . . ?
O4 C26 C34 106.08(16) . . ?
O4 C26 C27 109.05(15) . . ?
C34 C26 C27 113.42(16) . . ?
O4 C26 C25 107.88(15) . . ?
C34 C26 C25 112.42(17) . . ?
C27 C26 C25 107.81(16) . . ?
C32 C27 C28 118.15(18) . . ?
C32 C27 C26 119.71(17) . . ?
C28 C27 C26 122.13(18) . . ?
C29 C28 C27 121.16(19) . . ?
C29 C28 H28 119.4 . . ?
C27 C28 H28 119.4 . . ?
C28 C29 C30 119.55(19) . . ?
C28 C29 H29 120.2 . . ?
C30 C29 H29 120.2 . . ?
C31 C30 C29 120.5(2) . . ?
C31 C30 H30 119.8 . . ?
C29 C30 H30 119.8 . . ?
C30 C31 C32 119.60(19) . . ?
C30 C31 H31 120.2 . . ?
C32 C31 H31 120.2 . . ?
O5 C32 C31 117.12(17) . . ?
O5 C32 C27 121.93(18) . . ?
C31 C32 C27 120.95(19) . . ?
C18 C33 H33A 109.5 . . ?
C18 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C18 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C26 C34 H34A 109.5 . . ?
C26 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C26 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C18 O4 C26 113.46(14) . . ?
C32 O5 C18 114.87(14) . . ?

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 -163.31(18) . . . . ?
O2 C1 C2 C3 75.9(2) . . . . ?
C16 C1 C2 C3 -42.7(3) . . . . ?
O1 C1 C2 C7 16.6(3) . . . . ?
O2 C1 C2 C7 -104.2(2) . . . . ?
C16 C1 C2 C7 137.2(2) . . . . ?
C7 C2 C3 C4 -1.0(3) . . . . ?
C1 C2 C3 C4 178.87(18) . . . . ?
C2 C3 C4 C5 -0.1(3) . . . . ?
C3 C4 C5 C6 0.5(3) . . . . ?
C4 C5 C6 C7 0.1(3) . . . . ?
C5 C6 C7 C2 -1.2(3) . . . . ?
C5 C6 C7 C8 176.27(19) . . . . ?
C3 C2 C7 C6 1.6(3) . . . . ?
C1 C2 C7 C6 -178.26(18) . . . . ?
C3 C2 C7 C8 -175.82(18) . . . . ?
C1 C2 C7 C8 4.3(3) . . . . ?
C6 C7 C8 O3 7.0(3) . . . . ?
C2 C7 C8 O3 -175.5(2) . . . . ?
C6 C7 C8 C9 -167.95(18) . . . . ?
C2 C7 C8 C9 9.5(3) . . . . ?
O3 C8 C9 O1 142.8(2) . . . . ?
C7 C8 C9 O1 -42.2(2) . . . . ?
O3 C8 C9 C17 26.0(3) . . . . ?
C7 C8 C9 C17 -159.02(17) . . . . ?
O3 C8 C9 C10 -100.4(2) . . . . ?
C7 C8 C9 C10 74.6(2) . . . . ?
O1 C9 C10 C11 -165.70(18) . . . . ?
C17 C9 C10 C11 -47.2(3) . . . . ?
C8 C9 C10 C11 78.4(2) . . . . ?
O1 C9 C10 C15 14.7(2) . . . . ?
C17 C9 C10 C15 133.2(2) . . . . ?
C8 C9 C10 C15 -101.2(2) . . . . ?
C15 C10 C11 C12 -0.8(3) . . . . ?
C9 C10 C11 C12 179.66(19) . . . . ?
C10 C11 C12 C13 -1.0(3) . . . . ?
C11 C12 C13 C14 0.8(3) . . . . ?
C12 C13 C14 C15 1.2(3) . . . . ?
C13 C14 C15 O2 178.80(18) . . . . ?
C13 C14 C15 C10 -3.0(3) . . . . ?
C11 C10 C15 O2 -179.11(17) . . . . ?
C9 C10 C15 O2 0.5(3) . . . . ?
C11 C10 C15 C14 2.8(3) . . . . ?
C9 C10 C15 C14 -177.64(18) . . . . ?
O2 C1 O1 C9 66.78(19) . . . . ?
C16 C1 O1 C9 -179.31(16) . . . . ?
C2 C1 O1 C9 -54.1(2) . . . . ?
C17 C9 O1 C1 -171.77(16) . . . . ?
C10 C9 O1 C1 -48.6(2) . . . . ?
C8 C9 O1 C1 67.3(2) . . . . ?
C14 C15 O2 C1 -165.91(17) . . . . ?
C10 C15 O2 C1 15.9(2) . . . . ?
O1 C1 O2 C15 -47.7(2) . . . . ?
C16 C1 O2 C15 -161.81(16) . . . . ?
C2 C1 O2 C15 74.4(2) . . . . ?
O4 C18 C19 C20 -164.04(17) . . . . ?
O5 C18 C19 C20 75.4(2) . . . . ?
C33 C18 C19 C20 -43.4(2) . . . . ?
O4 C18 C19 C24 14.7(2) . . . . ?
O5 C18 C19 C24 -105.89(19) . . . . ?
C33 C18 C19 C24 135.28(19) . . . . ?
C24 C19 C20 C21 -2.2(3) . . . . ?
C18 C19 C20 C21 176.51(18) . . . . ?
C19 C20 C21 C22 0.2(3) . . . . ?
C20 C21 C22 C23 1.6(3) . . . . ?
C21 C22 C23 C24 -1.3(3) . . . . ?
C22 C23 C24 C19 -0.7(3) . . . . ?
C22 C23 C24 C25 175.69(18) . . . . ?
C20 C19 C24 C23 2.4(3) . . . . ?
C18 C19 C24 C23 -176.30(17) . . . . ?
C20 C19 C24 C25 -173.94(17) . . . . ?
C18 C19 C24 C25 7.3(3) . . . . ?
C23 C24 C25 O6 5.8(3) . . . . ?
C19 C24 C25 O6 -177.85(19) . . . . ?
C23 C24 C25 C26 -169.25(18) . . . . ?
C19 C24 C25 C26 7.1(3) . . . . ?
O6 C25 C26 O4 143.04(18) . . . . ?
C24 C25 C26 O4 -41.9(2) . . . . ?
O6 C25 C26 C34 26.4(3) . . . . ?
C24 C25 C26 C34 -158.48(17) . . . . ?
O6 C25 C26 C27 -99.3(2) . . . . ?
C24 C25 C26 C27 75.8(2) . . . . ?
O4 C26 C27 C32 14.7(2) . . . . ?
C34 C26 C27 C32 132.70(19) . . . . ?
C25 C26 C27 C32 -102.2(2) . . . . ?
O4 C26 C27 C28 -166.65(17) . . . . ?
C34 C26 C27 C28 -48.7(3) . . . . ?
C25 C26 C27 C28 76.5(2) . . . . ?
C32 C27 C28 C29 -2.2(3) . . . . ?
C26 C27 C28 C29 179.19(19) . . . . ?
C27 C28 C29 C30 -0.3(3) . . . . ?
C28 C29 C30 C31 1.6(3) . . . . ?
C29 C30 C31 C32 -0.4(3) . . . . ?
C30 C31 C32 O5 178.40(17) . . . . ?
C30 C31 C32 C27 -2.2(3) . . . . ?
C28 C27 C32 O5 -177.21(17) . . . . ?
C26 C27 C32 O5 1.5(3) . . . . ?
C28 C27 C32 C31 3.4(3) . . . . ?
C26 C27 C32 C31 -177.92(18) . . . . ?
O5 C18 O4 C26 66.62(19) . . . . ?
C33 C18 O4 C26 -178.58(15) . . . . ?
C19 C18 O4 C26 -53.6(2) . . . . ?
C34 C26 O4 C18 -171.37(16) . . . . ?
C27 C26 O4 C18 -48.9(2) . . . . ?
C25 C26 O4 C18 67.95(19) . . . . ?
C31 C32 O5 C18 -166.13(16) . . . . ?
C27 C32 O5 C18 14.5(3) . . . . ?
O4 C18 O5 C32 -46.9(2) . . . . ?
C33 C18 O5 C32 -161.78(15) . . . . ?
C19 C18 O5 C32 74.61(19) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.186
_refine_diff_density_rms         0.043


