# 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

_publ_contact_author_name        'Vincenzo Piccialli'
_publ_contact_author_email       VINPICCI@UNINA.IT

_publ_section_title              
;
Discovery of a new PCC-mediated stereoselective
oxidative spiroketalization process. An access to a new type of
poly-THF spiroketal compounds displaying anticancer activity
;
loop_
_publ_author_name
'Vincenzo Piccialli'
'Nicola Borbone'
'Roberto Centore'
'Vincenzo Cerullo'
'Akseli Hemminki'
;
G.Oliviero
;
'Angela Tuzi'
'Matteo Ugolini'

# Attachment 'Compound 2.cif'

data_picc2lt
_database_code_depnum_ccdc_archive 'CCDC 717142'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
dioxaspiro[bicyclo[3.2.1]octane-2,2'-oxolane]
derivative 1
;
_chemical_name_common            
"dioxaspiro(bicyclo(3.2.1)octane-2,2'-oxolane) derivative 1"
_chemical_formula_moiety         'C27 H42 O7'
_chemical_formula_sum            'C27 H42 O7'
_chemical_formula_weight         478.61

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
_space_group_name_H-M_alt        'P 1 21/c 1'

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

_cell_length_a                   13.2090(10)
_cell_length_b                   7.4940(10)
_cell_length_c                   25.505(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.450(10)
_cell_angle_gamma                90.00
_cell_volume                     2523.9(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    114
_cell_measurement_theta_min      3.177
_cell_measurement_theta_max      19.731

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1040
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9702
_exptl_absorpt_correction_T_max  0.9915
_exptl_absorpt_process_details   
;
SADABS (Bruker, 2000)
;

_exptl_special_details           
;
Crystals are twinned according to the matrix
-1 0 0
0 -1 0
0 0 1
HKLF5 was used in the refinement.
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_probe          x-ray
_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  'Bruker-Nonius KappaCCD'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            
;
Bruker-Nonius 95mm CCD camera on \k-goniostat
;
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_method       
;
CCD rotation images, thick slices
;

_diffrn_reflns_number            18190
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2385
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.09
_diffrn_reflns_theta_max         27.81
_reflns_number_total             18190
_reflns_number_gt                5205
_reflns_threshold_expression     >3sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       
;
Dirax/lsq (Duisenberg et al., 2000)
;
_computing_data_reduction        
;
EvalCCD (Duisenberg & Schreurs 1990-2000)
;
_computing_structure_solution    'SIR97 (Altomare at al, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0851P)^2^+0.0000P] 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_number_reflns         18190
_refine_ls_number_parameters     307
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2249
_refine_ls_R_factor_gt           0.0575
_refine_ls_wR_factor_ref         0.2048
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_restrained_S_all      0.959
_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 0.4028(2) 0.8021(4) 0.01723(12) 0.0432(10) Uani 1 1 d . . .
H1A H 0.4462 0.7326 -0.0058 0.065 Uiso 1 1 calc R . .
H1B H 0.4067 0.9287 0.0079 0.065 Uiso 1 1 calc R . .
H1C H 0.3326 0.7610 0.0130 0.065 Uiso 1 1 calc R . .
C2 C 0.4383(2) 0.7768(5) 0.07430(14) 0.0334(9) Uani 1 1 d . . .
C3 C 0.3746(3) 0.8840(4) 0.11180(13) 0.0379(10) Uani 1 1 d . . .
H3 H 0.3024 0.8439 0.1101 0.045 Uiso 1 1 calc R . .
C4 C 0.3821(2) 1.0860(4) 0.10426(14) 0.0398(10) Uani 1 1 d . . .
H4A H 0.3197 1.1466 0.1155 0.048 Uiso 1 1 calc R . .
H4B H 0.3941 1.1163 0.0672 0.048 Uiso 1 1 calc R . .
C5 C 0.4741(2) 1.1384(4) 0.13980(13) 0.0317(8) Uani 1 1 d . . .
H5A H 0.5280 1.1936 0.1190 0.038 Uiso 1 1 calc R . .
H5B H 0.4538 1.2232 0.1674 0.038 Uiso 1 1 calc R . .
C6 C 0.5102(3) 0.9608(4) 0.16402(13) 0.0290(9) Uani 1 1 d . . .
C7 C 0.5856(2) 0.8713(4) 0.12766(12) 0.0249(8) Uani 1 1 d . . .
C8 C 0.6839(2) 0.9714(4) 0.11863(12) 0.0279(9) Uani 1 1 d . . .
H8A H 0.6755 1.0605 0.0902 0.033 Uiso 1 1 calc R . .
H8B H 0.7084 1.0324 0.1510 0.033 Uiso 1 1 calc R . .
C9 C 0.7556(2) 0.8228(4) 0.10312(11) 0.0268(8) Uani 1 1 d . . .
H9A H 0.8264 0.8522 0.1135 0.032 Uiso 1 1 calc R . .
H9B H 0.7518 0.8018 0.0648 0.032 Uiso 1 1 calc R . .
C10 C 0.7185(2) 0.6589(4) 0.13309(13) 0.0256(8) Uani 1 1 d . . .
C11 C 0.7828(3) 0.6176(4) 0.18074(11) 0.0289(8) Uani 1 1 d . . .
H11 H 0.8518 0.5836 0.1689 0.035 Uiso 1 1 calc R . .
C12 C 0.7456(2) 0.4711(4) 0.21708(11) 0.0272(8) Uani 1 1 d . . .
H12A H 0.7692 0.3520 0.2059 0.033 Uiso 1 1 calc R . .
H12B H 0.6707 0.4704 0.2185 0.033 Uiso 1 1 calc R . .
C13 C 0.7939(3) 0.5248(4) 0.26989(11) 0.0305(9) Uani 1 1 d . . .
H13A H 0.7570 0.4727 0.2996 0.037 Uiso 1 1 calc R . .
H13B H 0.8659 0.4888 0.2725 0.037 Uiso 1 1 calc R . .
C14 C 0.7826(2) 0.7261(4) 0.26797(11) 0.0278(8) Uani 1 1 d . . .
H14 H 0.7125 0.7575 0.2787 0.033 Uiso 1 1 calc R . .
C15 C 0.8576(2) 0.8382(4) 0.30012(13) 0.0296(9) Uani 1 1 d . . .
C16 C 0.9673(2) 0.8081(4) 0.28692(13) 0.0342(9) Uani 1 1 d . . .
H16A H 1.0048 0.9226 0.2874 0.041 Uiso 1 1 calc R . .
H16B H 0.9723 0.7545 0.2516 0.041 Uiso 1 1 calc R . .
C17 C 1.0110(2) 0.6817(4) 0.32856(11) 0.0384(9) Uani 1 1 d . . .
H17A H 1.0766 0.7269 0.3427 0.046 Uiso 1 1 calc R . .
H17B H 1.0214 0.5613 0.3137 0.046 Uiso 1 1 calc R . .
C18 C 0.9320(2) 0.6763(4) 0.37157(12) 0.0311(9) Uani 1 1 d . . .
H18 H 0.9074 0.5510 0.3757 0.037 Uiso 1 1 calc R . .
C19 C 0.9705(3) 0.7470(4) 0.42517(12) 0.0289(8) Uani 1 1 d . . .
C20 C 0.8843(2) 0.7727(5) 0.46322(12) 0.0391(9) Uani 1 1 d . . .
H20A H 0.8272 0.6912 0.4547 0.047 Uiso 1 1 calc R . .
H20B H 0.9078 0.7510 0.4998 0.047 Uiso 1 1 calc R . .
C21 C 0.8531(3) 0.9660(5) 0.45540(15) 0.0486(11) Uani 1 1 d . . .
H21A H 0.7907 0.9743 0.4332 0.058 Uiso 1 1 calc R . .
H21B H 0.8409 1.0241 0.4895 0.058 Uiso 1 1 calc R . .
C22 C 0.9389(3) 1.0506(5) 0.42931(13) 0.0448(11) Uani 1 1 d . . .
C23 C 0.4356(2) 0.5780(4) 0.08809(14) 0.0465(11) Uani 1 1 d . . .
H23A H 0.4575 0.5616 0.1248 0.070 Uiso 1 1 calc R . .
H23B H 0.4811 0.5124 0.0652 0.070 Uiso 1 1 calc R . .
H23C H 0.3664 0.5328 0.0831 0.070 Uiso 1 1 calc R . .
C24 C 0.5482(3) 0.9748(4) 0.22025(12) 0.0417(10) Uani 1 1 d . . .
H24A H 0.4968 1.0331 0.2414 0.062 Uiso 1 1 calc R . .
H24B H 0.6107 1.0454 0.2217 0.062 Uiso 1 1 calc R . .
H24C H 0.5619 0.8551 0.2341 0.062 Uiso 1 1 calc R . .
C25 C 0.7096(2) 0.4934(4) 0.09774(12) 0.0327(9) Uani 1 1 d . . .
H25A H 0.6661 0.5208 0.0671 0.049 Uiso 1 1 calc R . .
H25B H 0.6800 0.3949 0.1174 0.049 Uiso 1 1 calc R . .
H25C H 0.7770 0.4589 0.0861 0.049 Uiso 1 1 calc R . .
C26 C 0.8255(3) 1.0351(4) 0.29680(13) 0.0393(10) Uani 1 1 d . . .
H26A H 0.7543 1.0462 0.3061 0.059 Uiso 1 1 calc R . .
H26B H 0.8342 1.0787 0.2610 0.059 Uiso 1 1 calc R . .
H26C H 0.8676 1.1058 0.3212 0.059 Uiso 1 1 calc R . .
C27 C 1.0573(2) 0.6350(4) 0.44659(12) 0.0375(9) Uani 1 1 d . . .
H27A H 1.1100 0.6266 0.4203 0.056 Uiso 1 1 calc R . .
H27B H 1.0326 0.5151 0.4548 0.056 Uiso 1 1 calc R . .
H27C H 1.0855 0.6905 0.4785 0.056 Uiso 1 1 calc R . .
O1 O 0.41870(16) 0.8556(3) 0.16375(8) 0.0348(6) Uani 1 1 d . . .
O2 O 0.54169(15) 0.8436(3) 0.07649(8) 0.0308(6) Uani 1 1 d . . .
O3 O 0.61761(14) 0.7052(3) 0.14991(8) 0.0259(6) Uani 1 1 d . . .
O4 O 0.79301(16) 0.7741(2) 0.21356(7) 0.0305(6) Uani 1 1 d . . .
O5 O 0.84941(16) 0.7871(3) 0.35464(7) 0.0345(6) Uani 1 1 d . . .
O6 O 1.00924(17) 0.9273(3) 0.41659(8) 0.0355(6) Uani 1 1 d . . .
O7 O 0.9538(2) 1.2076(3) 0.42021(9) 0.0622(8) 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 0.038(2) 0.051(2) 0.041(2) -0.005(2) -0.009(2) -0.003(2)
C2 0.031(2) 0.033(2) 0.036(2) 0.0028(19) -0.0006(19) 0.003(2)
C3 0.031(2) 0.041(3) 0.042(2) 0.004(2) -0.003(2) 0.000(2)
C4 0.037(2) 0.035(2) 0.048(2) 0.0050(19) 0.003(2) 0.016(2)
C5 0.0244(17) 0.023(2) 0.048(2) -0.0027(17) 0.0033(19) 0.0050(18)
C6 0.032(2) 0.024(2) 0.031(2) 0.0012(17) 0.0041(19) 0.0009(19)
C7 0.030(2) 0.026(2) 0.0192(19) -0.0019(17) -0.0028(18) -0.0029(19)
C8 0.0254(19) 0.029(2) 0.028(2) -0.0002(17) -0.0068(17) -0.0073(18)
C9 0.0243(17) 0.036(2) 0.0206(17) 0.0023(16) 0.0052(16) -0.001(2)
C10 0.0199(18) 0.026(2) 0.031(2) -0.0022(17) 0.0044(17) 0.0039(18)
C11 0.0374(19) 0.026(2) 0.0233(18) -0.0006(16) 0.0048(19) -0.0030(19)
C12 0.0240(17) 0.0247(19) 0.0328(19) 0.0040(17) -0.0007(17) 0.0000(18)
C13 0.038(2) 0.024(2) 0.031(2) 0.0026(16) 0.0049(19) -0.0045(19)
C14 0.0348(19) 0.027(2) 0.0217(18) 0.0022(16) 0.0011(17) -0.0034(19)
C15 0.038(2) 0.027(2) 0.024(2) 0.0046(17) 0.0042(19) -0.002(2)
C16 0.039(2) 0.039(2) 0.0251(19) 0.0012(18) 0.0055(18) -0.014(2)
C17 0.0351(19) 0.054(2) 0.0269(19) -0.0042(19) 0.0063(19) 0.010(2)
C18 0.039(2) 0.026(2) 0.0285(19) -0.0013(17) 0.0038(19) 0.005(2)
C19 0.0317(19) 0.024(2) 0.031(2) 0.0037(16) 0.0007(18) 0.0009(18)
C20 0.033(2) 0.059(3) 0.0244(19) 0.001(2) -0.0005(18) 0.006(2)
C21 0.038(2) 0.069(3) 0.038(2) -0.015(2) -0.002(2) 0.010(2)
C22 0.062(3) 0.035(3) 0.036(2) -0.007(2) -0.018(2) 0.017(3)
C23 0.031(2) 0.034(2) 0.074(3) -0.002(2) -0.005(2) -0.008(2)
C24 0.051(2) 0.044(2) 0.031(2) -0.0070(17) 0.011(2) 0.011(2)
C25 0.0296(19) 0.040(2) 0.0290(19) -0.0092(17) 0.0013(18) 0.0001(19)
C26 0.043(2) 0.037(2) 0.037(2) 0.0003(18) -0.010(2) -0.006(2)
C27 0.052(2) 0.031(2) 0.0292(19) -0.0032(17) 0.001(2) 0.006(2)
O1 0.0307(12) 0.0422(16) 0.0317(14) 0.0067(12) 0.0041(13) 0.0005(13)
O2 0.0315(13) 0.0309(14) 0.0300(14) 0.0001(11) 0.0027(12) -0.0023(13)
O3 0.0223(12) 0.0229(13) 0.0326(13) 0.0061(11) 0.0002(11) 0.0040(12)
O4 0.0471(14) 0.0255(13) 0.0188(12) -0.0005(10) -0.0028(13) -0.0065(13)
O5 0.0399(13) 0.0451(15) 0.0188(12) 0.0052(12) 0.0050(12) 0.0111(14)
O6 0.0323(13) 0.0294(14) 0.0446(15) -0.0012(12) -0.0024(14) 0.0036(13)
O7 0.092(2) 0.0352(16) 0.0586(17) -0.0094(15) -0.0196(18) 0.013(2)

_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 1.530(4) . no
C1 H1A 0.9800 . no
C1 H1B 0.9800 . no
C1 H1C 0.9800 . no
C2 O2 1.455(4) . no
C2 C3 1.519(4) . no
C2 C23 1.531(4) . no
C3 O1 1.449(4) . no
C3 C4 1.530(4) . no
C3 H3 1.0000 . no
C4 C5 1.547(4) . no
C4 H4A 0.9900 . no
C4 H4B 0.9900 . no
C5 C6 1.538(4) . no
C5 H5A 0.9900 . no
C5 H5B 0.9900 . no
C6 O1 1.442(4) . no
C6 C24 1.511(4) . no
C6 C7 1.533(4) . no
C7 O3 1.428(3) . no
C7 O2 1.430(4) . no
C7 C8 1.523(4) . no
C8 C9 1.521(4) . no
C8 H8A 0.9900 . no
C8 H8B 0.9900 . no
C9 C10 1.533(4) . no
C9 H9A 0.9900 . no
C9 H9B 0.9900 . no
C10 O3 1.453(3) . no
C10 C11 1.497(4) . no
C10 C25 1.536(4) . no
C11 O4 1.445(3) . no
C11 C12 1.527(4) . no
C11 H11 1.0000 . no
C12 C13 1.530(4) . no
C12 H12A 0.9900 . no
C12 H12B 0.9900 . no
C13 C14 1.517(3) . no
C13 H13A 0.9900 . no
C13 H13B 0.9900 . no
C14 O4 1.444(3) . no
C14 C15 1.523(4) . no
C14 H14 1.0000 . no
C15 O5 1.449(4) . no
C15 C16 1.514(4) . no
C15 C26 1.536(4) . no
C16 C17 1.525(4) . no
C16 H16A 0.9900 . no
C16 H16B 0.9900 . no
C17 C18 1.534(4) . no
C17 H17A 0.9900 . no
C17 H17B 0.9900 . no
C18 O5 1.429(3) . no
C18 C19 1.540(4) . no
C18 H18 1.0000 . no
C19 O6 1.463(3) . no
C19 C27 1.512(4) . no
C19 C20 1.527(4) . no
C20 C21 1.518(4) . no
C20 H20A 0.9900 . no
C20 H20B 0.9900 . no
C21 C22 1.471(5) . no
C21 H21A 0.9900 . no
C21 H21B 0.9900 . no
C22 O7 1.216(4) . no
C22 O6 1.356(4) . no
C23 H23A 0.9800 . no
C23 H23B 0.9800 . no
C23 H23C 0.9800 . no
C24 H24A 0.9800 . no
C24 H24B 0.9800 . no
C24 H24C 0.9800 . no
C25 H25A 0.9800 . no
C25 H25B 0.9800 . no
C25 H25C 0.9800 . no
C26 H26A 0.9800 . no
C26 H26B 0.9800 . no
C26 H26C 0.9800 . no
C27 H27A 0.9800 . no
C27 H27B 0.9800 . no
C27 H27C 0.9800 . no

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 H1A 109.5 . . no
C2 C1 H1B 109.5 . . no
H1A C1 H1B 109.5 . . no
C2 C1 H1C 109.5 . . no
H1A C1 H1C 109.5 . . no
H1B C1 H1C 109.5 . . no
O2 C2 C3 109.2(3) . . no
O2 C2 C1 105.0(3) . . no
C3 C2 C1 111.9(3) . . no
O2 C2 C23 110.7(3) . . no
C3 C2 C23 110.7(3) . . no
C1 C2 C23 109.3(3) . . no
O1 C3 C2 106.4(3) . . no
O1 C3 C4 103.5(3) . . no
C2 C3 C4 113.9(3) . . no
O1 C3 H3 110.9 . . no
C2 C3 H3 110.9 . . no
C4 C3 H3 110.9 . . no
C3 C4 C5 103.3(3) . . no
C3 C4 H4A 111.1 . . no
C5 C4 H4A 111.1 . . no
C3 C4 H4B 111.1 . . no
C5 C4 H4B 111.1 . . no
H4A C4 H4B 109.1 . . no
C6 C5 C4 104.3(2) . . no
C6 C5 H5A 110.9 . . no
C4 C5 H5A 110.9 . . no
C6 C5 H5B 110.9 . . no
C4 C5 H5B 110.9 . . no
H5A C5 H5B 108.9 . . no
O1 C6 C24 107.5(3) . . no
O1 C6 C7 108.4(2) . . no
C24 C6 C7 113.5(3) . . no
O1 C6 C5 102.7(2) . . no
C24 C6 C5 114.4(3) . . no
C7 C6 C5 109.6(3) . . no
O3 C7 O2 110.2(2) . . no
O3 C7 C8 104.2(2) . . no
O2 C7 C8 105.2(2) . . no
O3 C7 C6 109.4(2) . . no
O2 C7 C6 111.2(2) . . no
C8 C7 C6 116.5(3) . . no
C9 C8 C7 102.6(2) . . no
C9 C8 H8A 111.3 . . no
C7 C8 H8A 111.3 . . no
C9 C8 H8B 111.3 . . no
C7 C8 H8B 111.3 . . no
H8A C8 H8B 109.2 . . no
C8 C9 C10 104.3(2) . . no
C8 C9 H9A 110.9 . . no
C10 C9 H9A 110.9 . . no
C8 C9 H9B 110.9 . . no
C10 C9 H9B 110.9 . . no
H9A C9 H9B 108.9 . . no
O3 C10 C11 108.4(3) . . no
O3 C10 C9 105.3(3) . . no
C11 C10 C9 112.9(3) . . no
O3 C10 C25 108.0(2) . . no
C11 C10 C25 110.1(3) . . no
C9 C10 C25 112.0(3) . . no
O4 C11 C10 110.2(2) . . no
O4 C11 C12 105.0(2) . . no
C10 C11 C12 117.2(3) . . no
O4 C11 H11 108.0 . . no
C10 C11 H11 108.0 . . no
C12 C11 H11 108.0 . . no
C11 C12 C13 102.2(2) . . no
C11 C12 H12A 111.3 . . no
C13 C12 H12A 111.3 . . no
C11 C12 H12B 111.3 . . no
C13 C12 H12B 111.3 . . no
H12A C12 H12B 109.2 . . no
C14 C13 C12 101.2(2) . . no
C14 C13 H13A 111.5 . . no
C12 C13 H13A 111.5 . . no
C14 C13 H13B 111.5 . . no
C12 C13 H13B 111.5 . . no
H13A C13 H13B 109.3 . . no
O4 C14 C13 105.5(2) . . no
O4 C14 C15 107.7(2) . . no
C13 C14 C15 118.0(3) . . no
O4 C14 H14 108.4 . . no
C13 C14 H14 108.4 . . no
C15 C14 H14 108.4 . . no
O5 C15 C16 105.6(3) . . no
O5 C15 C14 107.9(2) . . no
C16 C15 C14 114.3(3) . . no
O5 C15 C26 106.2(3) . . no
C16 C15 C26 113.3(3) . . no
C14 C15 C26 109.0(3) . . no
C15 C16 C17 106.6(3) . . no
C15 C16 H16A 110.4 . . no
C17 C16 H16A 110.4 . . no
C15 C16 H16B 110.4 . . no
C17 C16 H16B 110.4 . . no
H16A C16 H16B 108.6 . . no
C16 C17 C18 105.2(2) . . no
C16 C17 H17A 110.7 . . no
C18 C17 H17A 110.7 . . no
C16 C17 H17B 110.7 . . no
C18 C17 H17B 110.7 . . no
H17A C17 H17B 108.8 . . no
O5 C18 C17 107.3(2) . . no
O5 C18 C19 107.5(3) . . no
C17 C18 C19 114.2(3) . . no
O5 C18 H18 109.2 . . no
C17 C18 H18 109.2 . . no
C19 C18 H18 109.2 . . no
O6 C19 C27 107.6(3) . . no
O6 C19 C20 104.3(3) . . no
C27 C19 C20 114.3(3) . . no
O6 C19 C18 107.1(3) . . no
C27 C19 C18 111.1(3) . . no
C20 C19 C18 111.9(3) . . no
C21 C20 C19 104.0(3) . . no
C21 C20 H20A 111.0 . . no
C19 C20 H20A 111.0 . . no
C21 C20 H20B 111.0 . . no
C19 C20 H20B 111.0 . . no
H20A C20 H20B 109.0 . . no
C22 C21 C20 105.1(3) . . no
C22 C21 H21A 110.7 . . no
C20 C21 H21A 110.7 . . no
C22 C21 H21B 110.7 . . no
C20 C21 H21B 110.7 . . no
H21A C21 H21B 108.8 . . no
O7 C22 O6 119.9(4) . . no
O7 C22 C21 129.3(4) . . no
O6 C22 C21 110.8(3) . . no
C2 C23 H23A 109.5 . . no
C2 C23 H23B 109.5 . . no
H23A C23 H23B 109.5 . . no
C2 C23 H23C 109.5 . . no
H23A C23 H23C 109.5 . . no
H23B C23 H23C 109.5 . . no
C6 C24 H24A 109.5 . . no
C6 C24 H24B 109.5 . . no
H24A C24 H24B 109.5 . . no
C6 C24 H24C 109.5 . . no
H24A C24 H24C 109.5 . . no
H24B C24 H24C 109.5 . . no
C10 C25 H25A 109.5 . . no
C10 C25 H25B 109.5 . . no
H25A C25 H25B 109.5 . . no
C10 C25 H25C 109.5 . . no
H25A C25 H25C 109.5 . . no
H25B C25 H25C 109.5 . . no
C15 C26 H26A 109.5 . . no
C15 C26 H26B 109.5 . . no
H26A C26 H26B 109.5 . . no
C15 C26 H26C 109.5 . . no
H26A C26 H26C 109.5 . . no
H26B C26 H26C 109.5 . . no
C19 C27 H27A 109.5 . . no
C19 C27 H27B 109.5 . . no
H27A C27 H27B 109.5 . . no
C19 C27 H27C 109.5 . . no
H27A C27 H27C 109.5 . . no
H27B C27 H27C 109.5 . . no
C6 O1 C3 104.0(2) . . no
C7 O2 C2 116.4(3) . . no
C7 O3 C10 110.8(2) . . no
C14 O4 C11 110.2(2) . . no
C18 O5 C15 111.6(2) . . no
C22 O6 C19 110.4(3) . . no

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
O2 C2 C3 O1 -61.5(3) . . . . no
C1 C2 C3 O1 -177.3(3) . . . . no
C23 C2 C3 O1 60.6(3) . . . . no
O2 C2 C3 C4 51.9(4) . . . . no
C1 C2 C3 C4 -63.9(4) . . . . no
C23 C2 C3 C4 174.0(3) . . . . no
O1 C3 C4 C5 26.9(3) . . . . no
C2 C3 C4 C5 -88.1(3) . . . . no
C3 C4 C5 C6 0.2(3) . . . . no
C4 C5 C6 O1 -27.3(3) . . . . no
C4 C5 C6 C24 -143.5(3) . . . . no
C4 C5 C6 C7 87.8(3) . . . . no
O1 C6 C7 O3 -67.7(3) . . . . no
C24 C6 C7 O3 51.6(3) . . . . no
C5 C6 C7 O3 -179.1(2) . . . . no
O1 C6 C7 O2 54.2(3) . . . . no
C24 C6 C7 O2 173.5(2) . . . . no
C5 C6 C7 O2 -57.2(3) . . . . no
O1 C6 C7 C8 174.6(3) . . . . no
C24 C6 C7 C8 -66.1(3) . . . . no
C5 C6 C7 C8 63.2(3) . . . . no
O3 C7 C8 C9 35.7(3) . . . . no
O2 C7 C8 C9 -80.2(3) . . . . no
C6 C7 C8 C9 156.2(3) . . . . no
C7 C8 C9 C10 -31.2(3) . . . . no
C8 C9 C10 O3 15.9(3) . . . . no
C8 C9 C10 C11 -102.2(3) . . . . no
C8 C9 C10 C25 133.0(2) . . . . no
O3 C10 C11 O4 -63.3(3) . . . . no
C9 C10 C11 O4 52.9(3) . . . . no
C25 C10 C11 O4 178.9(2) . . . . no
O3 C10 C11 C12 56.7(3) . . . . no
C9 C10 C11 C12 172.9(3) . . . . no
C25 C10 C11 C12 -61.2(3) . . . . no
O4 C11 C12 C13 -31.0(3) . . . . no
C10 C11 C12 C13 -153.7(3) . . . . no
C11 C12 C13 C14 39.1(3) . . . . no
C12 C13 C14 O4 -33.8(3) . . . . no
C12 C13 C14 C15 -154.1(3) . . . . no
O4 C14 C15 O5 -178.5(2) . . . . no
C13 C14 C15 O5 -59.3(3) . . . . no
O4 C14 C15 C16 -61.3(4) . . . . no
C13 C14 C15 C16 57.8(4) . . . . no
O4 C14 C15 C26 66.6(3) . . . . no
C13 C14 C15 C26 -174.3(3) . . . . no
O5 C15 C16 C17 19.0(3) . . . . no
C14 C15 C16 C17 -99.5(3) . . . . no
C26 C15 C16 C17 134.8(3) . . . . no
C15 C16 C17 C18 -12.5(3) . . . . no
C16 C17 C18 O5 1.4(3) . . . . no
C16 C17 C18 C19 -117.6(3) . . . . no
O5 C18 C19 O6 -63.8(3) . . . . no
C17 C18 C19 O6 55.1(3) . . . . no
O5 C18 C19 C27 179.0(2) . . . . no
C17 C18 C19 C27 -62.1(3) . . . . no
O5 C18 C19 C20 49.9(3) . . . . no
C17 C18 C19 C20 168.8(3) . . . . no
O6 C19 C20 C21 22.9(3) . . . . no
C27 C19 C20 C21 140.1(3) . . . . no
C18 C19 C20 C21 -92.5(3) . . . . no
C19 C20 C21 C22 -18.0(3) . . . . no
C20 C21 C22 O7 -171.2(4) . . . . no
C20 C21 C22 O6 6.3(4) . . . . no
C24 C6 O1 C3 166.8(3) . . . . no
C7 C6 O1 C3 -70.2(3) . . . . no
C5 C6 O1 C3 45.8(3) . . . . no
C2 C3 O1 C6 74.2(3) . . . . no
C4 C3 O1 C6 -46.1(3) . . . . no
O3 C7 O2 C2 78.4(3) . . . . no
C8 C7 O2 C2 -169.9(2) . . . . no
C6 C7 O2 C2 -43.1(3) . . . . no
C3 C2 O2 C7 46.8(4) . . . . no
C1 C2 O2 C7 166.9(3) . . . . no
C23 C2 O2 C7 -75.2(3) . . . . no
O2 C7 O3 C10 85.2(3) . . . . no
C8 C7 O3 C10 -27.1(3) . . . . no
C6 C7 O3 C10 -152.3(2) . . . . no
C11 C10 O3 C7 128.1(3) . . . . no
C9 C10 O3 C7 7.1(3) . . . . no
C25 C10 O3 C7 -112.7(3) . . . . no
C13 C14 O4 C11 15.2(3) . . . . no
C15 C14 O4 C11 142.0(3) . . . . no
C10 C11 O4 C14 137.3(3) . . . . no
C12 C11 O4 C14 10.2(3) . . . . no
C17 C18 O5 C15 11.0(3) . . . . no
C19 C18 O5 C15 134.3(3) . . . . no
C16 C15 O5 C18 -18.9(3) . . . . no
C14 C15 O5 C18 103.7(3) . . . . no
C26 C15 O5 C18 -139.5(3) . . . . no
O7 C22 O6 C19 -173.3(3) . . . . no
C21 C22 O6 C19 9.0(4) . . . . no
C27 C19 O6 C22 -142.1(3) . . . . no
C20 C19 O6 C22 -20.3(3) . . . . no
C18 C19 O6 C22 98.4(3) . . . . no

_diffrn_measured_fraction_theta_max 0.855
_diffrn_reflns_theta_full        27.81
_diffrn_measured_fraction_theta_full 0.855
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.078

# Attachment 'Compound 5.cif'

data_picc3lt
_database_code_depnum_ccdc_archive 'CCDC 717143'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
dioxaspiro[bicyclo[3.2.1]octane-2,2'-oxolane]
derivative 2
;
_chemical_name_common            
"dioxaspiro(bicyclo(3.2.1)octane-2,2'-oxolane) derivative 2"
_chemical_formula_moiety         'C30 H50 O7'
_chemical_formula_sum            'C30 H50 O7'
_chemical_formula_weight         522.70

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
_space_group_name_H-M_alt        'P 1 21/c 1'

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

_cell_length_a                   15.162(4)
_cell_length_b                   8.489(9)
_cell_length_c                   24.593(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.634(9)
_cell_angle_gamma                90.00
_cell_volume                     2942(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    120
_cell_measurement_theta_min      4.093
_cell_measurement_theta_max      16.869

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1144
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9658
_exptl_absorpt_correction_T_max  0.9970

_exptl_special_details           
;
SADABS (Bruker, 2000)
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_probe          x-ray
_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  'Bruker-Nonius KappaCCD'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            
;
Bruker-Nonius 95mm CCD camera on \k-goniostat
;
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_method       
;
CCD rotation images, thick slices
;

_diffrn_reflns_number            22393
_diffrn_reflns_av_R_equivalents  0.2294
_diffrn_reflns_av_sigmaI/netI    0.2028
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         25.07
_reflns_number_total             5101
_reflns_number_gt                1593
_reflns_threshold_expression     >3sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       
;
Dirax/lsq (Duisenberg et al., 2000)
;
_computing_data_reduction        
;
EvalCCD (Duisenberg & Schreurs 1990-2000)
;
_computing_structure_solution    'SIR97 (Altomare at al, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The poor quality of the crystal, an irregularly shaped low diffracting
specimen, can justify the relatively high Rint value.
;

_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^)+(0.1066P)^2^+0.0000P] 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_number_reflns         5101
_refine_ls_number_parameters     342
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2423
_refine_ls_R_factor_gt           0.0687
_refine_ls_wR_factor_ref         0.2574
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.013
_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 -0.0069(4) 0.6573(8) 0.0560(3) 0.068(2) Uani 1 1 d . . .
H1A H -0.0178 0.6863 0.0155 0.068 Uiso 1 1 calc R . .
H1B H -0.0445 0.7261 0.0712 0.068 Uiso 1 1 calc R . .
H1C H -0.0259 0.5475 0.0574 0.068 Uiso 1 1 calc R . .
C2 C 0.0964(4) 0.6757(7) 0.0928(3) 0.0466(16) Uani 1 1 d . . .
C3 C 0.1339(4) 0.8451(6) 0.0910(3) 0.0442(16) Uani 1 1 d . . .
H3 H 0.1018 0.9209 0.1088 0.044 Uiso 1 1 calc R . .
C4 C 0.1240(5) 0.9017(8) 0.0298(3) 0.064(2) Uani 1 1 d . . .
H4A H 0.0698 0.8498 -0.0009 0.064 Uiso 1 1 calc R . .
H4B H 0.1154 1.0174 0.0262 0.064 Uiso 1 1 calc R . .
C5 C 0.2184(5) 0.8519(7) 0.0260(3) 0.0547(18) Uani 1 1 d . . .
H5A H 0.2541 0.9450 0.0211 0.055 Uiso 1 1 calc R . .
H5B H 0.2079 0.7795 -0.0073 0.055 Uiso 1 1 calc R . .
C6 C 0.2727(4) 0.7685(7) 0.0844(3) 0.0433(16) Uani 1 1 d . . .
C7 C 0.2457(4) 0.5944(6) 0.0812(2) 0.0354(14) Uani 1 1 d . . .
C8 C 0.2760(5) 0.4923(7) 0.0391(3) 0.0499(17) Uani 1 1 d . . .
H8A H 0.3382 0.5262 0.0387 0.050 Uiso 1 1 calc R . .
H8B H 0.2282 0.4966 -0.0012 0.050 Uiso 1 1 calc R . .
C9 C 0.2819(4) 0.3252(6) 0.0657(3) 0.0478(17) Uani 1 1 d . . .
H9A H 0.3299 0.2601 0.0576 0.048 Uiso 1 1 calc R . .
H9B H 0.2197 0.2712 0.0498 0.048 Uiso 1 1 calc R . .
C10 C 0.3116(4) 0.3566(6) 0.1325(2) 0.0385(15) Uani 1 1 d . . .
C11 C 0.4152(4) 0.3258(7) 0.1661(3) 0.0438(16) Uani 1 1 d . . .
H11 H 0.4267 0.2097 0.1665 0.044 Uiso 1 1 calc R . .
C12 C 0.4556(4) 0.3865(7) 0.2289(2) 0.0476(17) Uani 1 1 d . . .
H12A H 0.4271 0.4889 0.2325 0.048 Uiso 1 1 calc R . .
H12B H 0.4449 0.3101 0.2563 0.048 Uiso 1 1 calc R . .
C13 C 0.5592(4) 0.4035(7) 0.2401(3) 0.0471(16) Uani 1 1 d . . .
H13A H 0.5929 0.3020 0.2524 0.047 Uiso 1 1 calc R . .
H13B H 0.5891 0.4835 0.2707 0.047 Uiso 1 1 calc R . .
C14 C 0.5599(4) 0.4562(7) 0.1809(2) 0.0424(15) Uani 1 1 d . . .
H14 H 0.5607 0.5739 0.1799 0.042 Uiso 1 1 calc R . .
C15 C 0.6428(4) 0.3946(6) 0.1669(3) 0.0413(15) Uani 1 1 d . . .
C16 C 0.6321(4) 0.4251(7) 0.1036(2) 0.0437(15) Uani 1 1 d . . .
H16A H 0.5925 0.5196 0.0881 0.044 Uiso 1 1 calc R . .
H16B H 0.6949 0.4415 0.1008 0.044 Uiso 1 1 calc R . .
C17 C 0.5842(5) 0.2786(7) 0.0695(3) 0.0508(17) Uani 1 1 d . . .
H17A H 0.5151 0.2959 0.0494 0.051 Uiso 1 1 calc R . .
H17B H 0.6118 0.2502 0.0401 0.051 Uiso 1 1 calc R . .
C18 C 0.6034(4) 0.1508(7) 0.1158(3) 0.0452(16) Uani 1 1 d . . .
H18 H 0.5415 0.1029 0.1127 0.045 Uiso 1 1 calc R . .
C19 C 0.6698(4) 0.0192(7) 0.1130(3) 0.0442(16) Uani 1 1 d . . .
C20 C 0.7036(5) -0.0877(7) 0.1678(3) 0.0564(19) Uani 1 1 d . . .
H20A H 0.6861 -0.0418 0.1995 0.056 Uiso 1 1 calc R . .
H20B H 0.6752 -0.1940 0.1584 0.056 Uiso 1 1 calc R . .
C21 C 0.8101(5) -0.0955(7) 0.1858(3) 0.0587(19) Uani 1 1 d . . .
H21A H 0.8414 -0.1130 0.2285 0.059 Uiso 1 1 calc R . .
H21B H 0.8288 -0.1806 0.1647 0.059 Uiso 1 1 calc R . .
C22 C 0.8345(4) 0.0639(7) 0.1686(3) 0.0443(16) Uani 1 1 d . . .
H22 H 0.8328 0.1429 0.1984 0.044 Uiso 1 1 calc R . .
C23 C 0.9267(4) 0.0823(7) 0.1589(3) 0.0464(16) Uani 1 1 d . . .
C24 C 0.9384(5) 0.2505(8) 0.1420(3) 0.0617(19) Uani 1 1 d . . .
H24A H 0.9969 0.2592 0.1340 0.062 Uiso 1 1 calc R . .
H24B H 0.9419 0.3213 0.1742 0.062 Uiso 1 1 calc R . .
H24C H 0.8840 0.2796 0.1070 0.062 Uiso 1 1 calc R . .
C25 C 0.1172(5) 0.6275(6) 0.1552(3) 0.0518(18) Uani 1 1 d . . .
H25A H 0.0962 0.5187 0.1562 0.052 Uiso 1 1 calc R . .
H25B H 0.0832 0.6975 0.1726 0.052 Uiso 1 1 calc R . .
H25C H 0.1855 0.6351 0.1775 0.052 Uiso 1 1 calc R . .
C26 C 0.3785(4) 0.7977(7) 0.1079(3) 0.0462(16) Uani 1 1 d . . .
H26A H 0.3908 0.9106 0.1150 0.046 Uiso 1 1 calc R . .
H26B H 0.4050 0.7615 0.0792 0.046 Uiso 1 1 calc R . .
H26C H 0.4082 0.7398 0.1446 0.046 Uiso 1 1 calc R . .
C27 C 0.2505(4) 0.2646(7) 0.1581(3) 0.0526(18) Uani 1 1 d . . .
H27A H 0.2670 0.2944 0.1992 0.053 Uiso 1 1 calc R . .
H27B H 0.2616 0.1516 0.1556 0.053 Uiso 1 1 calc R . .
H27C H 0.1835 0.2884 0.1362 0.053 Uiso 1 1 calc R . .
C28 C 0.7361(4) 0.4542(7) 0.2120(3) 0.0523(17) Uani 1 1 d . . .
H28A H 0.7450 0.4095 0.2504 0.052 Uiso 1 1 calc R . .
H28B H 0.7343 0.5694 0.2141 0.052 Uiso 1 1 calc R . .
H28C H 0.7887 0.4220 0.2004 0.052 Uiso 1 1 calc R . .
C29 C 0.6319(5) -0.0758(7) 0.0569(3) 0.066(2) Uani 1 1 d . . .
H29A H 0.6182 -0.0052 0.0233 0.066 Uiso 1 1 calc R . .
H29B H 0.5735 -0.1299 0.0546 0.066 Uiso 1 1 calc R . .
H29C H 0.6793 -0.1538 0.0566 0.066 Uiso 1 1 calc R . .
C30 C 1.0112(5) 0.0326(9) 0.2122(3) 0.066(2) Uani 1 1 d . . .
H30A H 1.0032 -0.0771 0.2219 0.066 Uiso 1 1 calc R . .
H30B H 1.0158 0.1005 0.2453 0.066 Uiso 1 1 calc R . .
H30C H 1.0693 0.0422 0.2037 0.066 Uiso 1 1 calc R . .
O1 O 0.2354(3) 0.8456(4) 0.12399(16) 0.0415(11) Uani 1 1 d . . .
O2 O 0.1461(3) 0.5745(4) 0.06495(16) 0.0422(10) Uani 1 1 d . . .
O3 O 0.2952(3) 0.5250(4) 0.13738(15) 0.0397(10) Uani 1 1 d . . .
O4 O 0.4714(3) 0.4014(4) 0.13868(16) 0.0457(11) Uani 1 1 d . . .
O5 O 0.6447(3) 0.2240(4) 0.17202(16) 0.0457(11) Uani 1 1 d . . .
O6 O 0.7583(3) 0.0961(4) 0.11457(17) 0.0432(10) Uani 1 1 d . . .
O7 O 0.9252(3) -0.0189(5) 0.11188(18) 0.0620(13) Uani 1 1 d . . .
H7 H 0.8697 -0.0076 0.0839 0.062 Uiso 1 1 d R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.045(5) 0.063(5) 0.091(6) -0.026(4) 0.020(4) 0.007(4)
C2 0.039(4) 0.049(4) 0.049(4) -0.011(3) 0.014(3) 0.005(3)
C3 0.047(4) 0.036(3) 0.047(4) -0.007(3) 0.015(3) 0.005(3)
C4 0.064(5) 0.062(4) 0.064(5) 0.017(4) 0.021(4) 0.018(4)
C5 0.064(5) 0.053(4) 0.046(4) 0.016(3) 0.020(4) 0.011(3)
C6 0.046(4) 0.047(4) 0.033(4) 0.005(3) 0.009(3) 0.004(3)
C7 0.035(4) 0.040(4) 0.025(3) -0.003(3) 0.005(3) 0.004(3)
C8 0.060(4) 0.046(4) 0.034(4) -0.010(3) 0.007(3) 0.002(3)
C9 0.049(4) 0.041(4) 0.047(4) -0.016(3) 0.011(3) 0.007(3)
C10 0.037(4) 0.033(3) 0.046(4) 0.003(3) 0.015(3) 0.003(3)
C11 0.043(4) 0.038(3) 0.054(4) -0.007(3) 0.023(3) -0.002(3)
C12 0.066(5) 0.047(4) 0.034(4) 0.003(3) 0.024(3) 0.006(3)
C13 0.050(4) 0.052(4) 0.034(4) 0.000(3) 0.010(3) 0.002(3)
C14 0.044(4) 0.045(4) 0.032(4) 0.000(3) 0.007(3) -0.005(3)
C15 0.045(4) 0.027(3) 0.044(4) -0.004(3) 0.007(3) 0.002(3)
C16 0.037(4) 0.052(4) 0.041(4) 0.000(3) 0.014(3) 0.000(3)
C17 0.053(4) 0.057(4) 0.037(4) 0.003(3) 0.010(3) 0.010(3)
C18 0.036(4) 0.046(4) 0.056(4) -0.009(3) 0.020(3) -0.003(3)
C19 0.053(4) 0.042(4) 0.046(4) -0.009(3) 0.028(3) -0.004(3)
C20 0.086(6) 0.029(3) 0.067(5) 0.011(3) 0.044(4) 0.002(3)
C21 0.068(5) 0.045(4) 0.070(5) 0.015(3) 0.034(4) 0.014(3)
C22 0.051(4) 0.043(4) 0.035(4) 0.003(3) 0.011(3) 0.007(3)
C23 0.038(4) 0.053(4) 0.042(4) -0.002(3) 0.008(3) 0.012(3)
C24 0.052(5) 0.074(5) 0.056(5) -0.006(4) 0.017(4) -0.006(4)
C25 0.056(4) 0.038(4) 0.069(5) -0.011(3) 0.032(4) -0.003(3)
C26 0.049(4) 0.045(4) 0.045(4) -0.001(3) 0.018(3) 0.002(3)
C27 0.051(4) 0.038(4) 0.068(5) 0.003(3) 0.021(4) -0.002(3)
C28 0.044(4) 0.041(4) 0.064(5) -0.006(3) 0.010(3) 0.001(3)
C29 0.079(5) 0.056(4) 0.065(5) -0.024(4) 0.031(4) -0.016(4)
C30 0.053(5) 0.088(5) 0.053(5) -0.008(4) 0.014(4) 0.010(4)
O1 0.047(3) 0.036(2) 0.038(2) -0.0039(18) 0.012(2) -0.0009(19)
O2 0.036(3) 0.040(2) 0.046(3) -0.0142(19) 0.009(2) 0.0031(19)
O3 0.049(3) 0.035(2) 0.033(2) 0.0021(18) 0.012(2) 0.0046(19)
O4 0.037(3) 0.060(3) 0.036(2) -0.002(2) 0.009(2) -0.005(2)
O5 0.059(3) 0.037(2) 0.035(3) -0.0047(19) 0.009(2) 0.004(2)
O6 0.040(3) 0.048(2) 0.041(3) 0.0093(19) 0.014(2) 0.008(2)
O7 0.060(3) 0.076(3) 0.053(3) -0.007(2) 0.025(2) 0.014(2)

_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 1.501(8) . no
C1 H1A 0.9800 . no
C1 H1B 0.9800 . no
C1 H1C 0.9800 . no
C2 O2 1.467(7) . no
C2 C25 1.506(8) . no
C2 C3 1.553(8) . no
C3 O1 1.451(7) . no
C3 C4 1.532(8) . no
C3 H3 1.0000 . no
C4 C5 1.529(9) . no
C4 H4A 0.9900 . no
C4 H4B 0.9900 . no
C5 C6 1.538(8) . no
C5 H5A 0.9900 . no
C5 H5B 0.9900 . no
C6 O1 1.450(7) . no
C6 C26 1.512(8) . no
C6 C7 1.528(8) . no
C7 O2 1.423(6) . no
C7 O3 1.434(6) . no
C7 C8 1.544(8) . no
C8 C9 1.551(8) . no
C8 H8A 0.9900 . no
C8 H8B 0.9900 . no
C9 C10 1.559(8) . no
C9 H9A 0.9900 . no
C9 H9B 0.9900 . no
C10 O3 1.464(6) . no
C10 C11 1.504(8) . no
C10 C27 1.514(8) . no
C11 O4 1.419(7) . no
C11 C12 1.526(8) . no
C11 H11 1.0000 . no
C12 C13 1.499(8) . no
C12 H12A 0.9900 . no
C12 H12B 0.9900 . no
C13 C14 1.527(8) . no
C13 H13A 0.9900 . no
C13 H13B 0.9900 . no
C14 O4 1.439(6) . no
C14 C15 1.514(8) . no
C14 H14 1.0000 . no
C15 O5 1.453(6) . no
C15 C28 1.525(8) . no
C15 C16 1.527(8) . no
C16 C17 1.525(8) . no
C16 H16A 0.9900 . no
C16 H16B 0.9900 . no
C17 C18 1.522(8) . no
C17 H17A 0.9900 . no
C17 H17B 0.9900 . no
C18 O5 1.432(6) . no
C18 C19 1.522(8) . no
C18 H18 1.0000 . no
C19 O6 1.480(7) . no
C19 C29 1.516(8) . no
C19 C20 1.548(8) . no
C20 C21 1.509(8) . no
C20 H20A 0.9900 . no
C20 H20B 0.9900 . no
C21 C22 1.505(8) . no
C21 H21A 0.9900 . no
C21 H21B 0.9900 . no
C22 O6 1.430(6) . no
C22 C23 1.510(8) . no
C22 H22 1.0000 . no
C23 O7 1.435(7) . no
C23 C24 1.516(8) . no
C23 C30 1.516(8) . no
C24 H24A 0.9800 . no
C24 H24B 0.9800 . no
C24 H24C 0.9800 . no
C25 H25A 0.9800 . no
C25 H25B 0.9800 . no
C25 H25C 0.9800 . no
C26 H26A 0.9800 . no
C26 H26B 0.9800 . no
C26 H26C 0.9800 . no
C27 H27A 0.9800 . no
C27 H27B 0.9800 . no
C27 H27C 0.9800 . no
C28 H28A 0.9800 . no
C28 H28B 0.9800 . no
C28 H28C 0.9800 . no
C29 H29A 0.9800 . no
C29 H29B 0.9800 . no
C29 H29C 0.9800 . no
C30 H30A 0.9800 . no
C30 H30B 0.9800 . no
C30 H30C 0.9800 . no
O7 H7 0.8735 . no

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 H1A 109.5 . . no
C2 C1 H1B 109.5 . . no
H1A C1 H1B 109.5 . . no
C2 C1 H1C 109.5 . . no
H1A C1 H1C 109.5 . . no
H1B C1 H1C 109.5 . . no
O2 C2 C1 105.0(5) . . no
O2 C2 C25 111.5(5) . . no
C1 C2 C25 111.4(6) . . no
O2 C2 C3 105.8(5) . . no
C1 C2 C3 113.0(5) . . no
C25 C2 C3 109.8(5) . . no
O1 C3 C4 104.4(5) . . no
O1 C3 C2 108.1(4) . . no
C4 C3 C2 114.4(5) . . no
O1 C3 H3 109.9 . . no
C4 C3 H3 109.9 . . no
C2 C3 H3 109.9 . . no
C5 C4 C3 102.6(5) . . no
C5 C4 H4A 111.3 . . no
C3 C4 H4A 111.3 . . no
C5 C4 H4B 111.3 . . no
C3 C4 H4B 111.3 . . no
H4A C4 H4B 109.2 . . no
C4 C5 C6 105.1(5) . . no
C4 C5 H5A 110.7 . . no
C6 C5 H5A 110.7 . . no
C4 C5 H5B 110.7 . . no
C6 C5 H5B 110.7 . . no
H5A C5 H5B 108.8 . . no
O1 C6 C26 106.9(5) . . no
O1 C6 C7 108.0(5) . . no
C26 C6 C7 113.8(5) . . no
O1 C6 C5 102.2(5) . . no
C26 C6 C5 114.1(5) . . no
C7 C6 C5 110.9(5) . . no
O2 C7 O3 110.2(4) . . no
O2 C7 C6 111.4(4) . . no
O3 C7 C6 108.3(4) . . no
O2 C7 C8 107.0(4) . . no
O3 C7 C8 103.7(4) . . no
C6 C7 C8 116.0(5) . . no
C7 C8 C9 102.5(5) . . no
C7 C8 H8A 111.3 . . no
C9 C8 H8A 111.3 . . no
C7 C8 H8B 111.3 . . no
C9 C8 H8B 111.3 . . no
H8A C8 H8B 109.2 . . no
C8 C9 C10 103.7(4) . . no
C8 C9 H9A 111.0 . . no
C10 C9 H9A 111.0 . . no
C8 C9 H9B 111.0 . . no
C10 C9 H9B 111.0 . . no
H9A C9 H9B 109.0 . . no
O3 C10 C11 107.4(4) . . no
O3 C10 C27 108.7(4) . . no
C11 C10 C27 111.0(5) . . no
O3 C10 C9 105.1(4) . . no
C11 C10 C9 112.7(5) . . no
C27 C10 C9 111.5(5) . . no
O4 C11 C10 110.4(5) . . no
O4 C11 C12 104.0(4) . . no
C10 C11 C12 116.4(5) . . no
O4 C11 H11 108.6 . . no
C10 C11 H11 108.6 . . no
C12 C11 H11 108.6 . . no
C13 C12 C11 102.8(5) . . no
C13 C12 H12A 111.2 . . no
C11 C12 H12A 111.2 . . no
C13 C12 H12B 111.2 . . no
C11 C12 H12B 111.2 . . no
H12A C12 H12B 109.1 . . no
C12 C13 C14 103.2(5) . . no
C12 C13 H13A 111.1 . . no
C14 C13 H13A 111.1 . . no
C12 C13 H13B 111.1 . . no
C14 C13 H13B 111.1 . . no
H13A C13 H13B 109.1 . . no
O4 C14 C15 110.9(5) . . no
O4 C14 C13 105.2(5) . . no
C15 C14 C13 114.4(5) . . no
O4 C14 H14 108.7 . . no
C15 C14 H14 108.7 . . no
C13 C14 H14 108.7 . . no
O5 C15 C14 108.4(5) . . no
O5 C15 C28 106.5(4) . . no
C14 C15 C28 110.2(5) . . no
O5 C15 C16 104.4(4) . . no
C14 C15 C16 112.8(5) . . no
C28 C15 C16 114.0(5) . . no
C17 C16 C15 105.8(5) . . no
C17 C16 H16A 110.6 . . no
C15 C16 H16A 110.6 . . no
C17 C16 H16B 110.6 . . no
C15 C16 H16B 110.6 . . no
H16A C16 H16B 108.7 . . no
C18 C17 C16 104.4(5) . . no
C18 C17 H17A 110.9 . . no
C16 C17 H17A 110.9 . . no
C18 C17 H17B 110.9 . . no
C16 C17 H17B 110.9 . . no
H17A C17 H17B 108.9 . . no
O5 C18 C17 107.9(5) . . no
O5 C18 C19 107.6(5) . . no
C17 C18 C19 115.9(5) . . no
O5 C18 H18 108.4 . . no
C17 C18 H18 108.4 . . no
C19 C18 H18 108.4 . . no
O6 C19 C29 107.1(5) . . no
O6 C19 C18 106.5(4) . . no
C29 C19 C18 113.4(5) . . no
O6 C19 C20 103.3(5) . . no
C29 C19 C20 111.9(5) . . no
C18 C19 C20 113.7(5) . . no
C21 C20 C19 104.8(5) . . no
C21 C20 H20A 110.8 . . no
C19 C20 H20A 110.8 . . no
C21 C20 H20B 110.8 . . no
C19 C20 H20B 110.8 . . no
H20A C20 H20B 108.9 . . no
C22 C21 C20 103.1(5) . . no
C22 C21 H21A 111.2 . . no
C20 C21 H21A 111.2 . . no
C22 C21 H21B 111.2 . . no
C20 C21 H21B 111.2 . . no
H21A C21 H21B 109.1 . . no
O6 C22 C21 103.6(5) . . no
O6 C22 C23 108.1(5) . . no
C21 C22 C23 118.4(5) . . no
O6 C22 H22 108.8 . . no
C21 C22 H22 108.8 . . no
C23 C22 H22 108.8 . . no
O7 C23 C22 109.0(5) . . no
O7 C23 C24 108.2(5) . . no
C22 C23 C24 110.5(5) . . no
O7 C23 C30 106.7(5) . . no
C22 C23 C30 111.8(5) . . no
C24 C23 C30 110.6(5) . . no
C23 C24 H24A 109.5 . . no
C23 C24 H24B 109.5 . . no
H24A C24 H24B 109.5 . . no
C23 C24 H24C 109.5 . . no
H24A C24 H24C 109.5 . . no
H24B C24 H24C 109.5 . . no
C2 C25 H25A 109.5 . . no
C2 C25 H25B 109.5 . . no
H25A C25 H25B 109.5 . . no
C2 C25 H25C 109.5 . . no
H25A C25 H25C 109.5 . . no
H25B C25 H25C 109.5 . . no
C6 C26 H26A 109.5 . . no
C6 C26 H26B 109.5 . . no
H26A C26 H26B 109.5 . . no
C6 C26 H26C 109.5 . . no
H26A C26 H26C 109.5 . . no
H26B C26 H26C 109.5 . . no
C10 C27 H27A 109.5 . . no
C10 C27 H27B 109.5 . . no
H27A C27 H27B 109.5 . . no
C10 C27 H27C 109.5 . . no
H27A C27 H27C 109.5 . . no
H27B C27 H27C 109.5 . . no
C15 C28 H28A 109.5 . . no
C15 C28 H28B 109.5 . . no
H28A C28 H28B 109.5 . . no
C15 C28 H28C 109.5 . . no
H28A C28 H28C 109.5 . . no
H28B C28 H28C 109.5 . . no
C19 C29 H29A 109.5 . . no
C19 C29 H29B 109.5 . . no
H29A C29 H29B 109.5 . . no
C19 C29 H29C 109.5 . . no
H29A C29 H29C 109.5 . . no
H29B C29 H29C 109.5 . . no
C23 C30 H30A 109.5 . . no
C23 C30 H30B 109.5 . . no
H30A C30 H30B 109.5 . . no
C23 C30 H30C 109.5 . . no
H30A C30 H30C 109.5 . . no
H30B C30 H30C 109.5 . . no
C6 O1 C3 102.6(4) . . no
C7 O2 C2 118.3(4) . . no
C7 O3 C10 111.5(4) . . no
C11 O4 C14 111.5(4) . . no
C18 O5 C15 111.2(4) . . no
C22 O6 C19 110.7(4) . . no
C23 O7 H7 107.0 . . no

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
O2 C2 C3 O1 -61.1(6) . . . . no
C1 C2 C3 O1 -175.5(5) . . . . no
C25 C2 C3 O1 59.4(6) . . . . no
O2 C2 C3 C4 54.8(6) . . . . no
C1 C2 C3 C4 -59.6(7) . . . . no
C25 C2 C3 C4 175.3(5) . . . . no
O1 C3 C4 C5 26.9(6) . . . . no
C2 C3 C4 C5 -91.1(6) . . . . no
C3 C4 C5 C6 1.3(7) . . . . no
C4 C5 C6 O1 -28.8(6) . . . . no
C4 C5 C6 C26 -143.8(5) . . . . no
C4 C5 C6 C7 86.1(6) . . . . no
O1 C6 C7 O2 55.1(6) . . . . no
C26 C6 C7 O2 173.6(4) . . . . no
C5 C6 C7 O2 -56.2(6) . . . . no
O1 C6 C7 O3 -66.2(5) . . . . no
C26 C6 C7 O3 52.3(6) . . . . no
C5 C6 C7 O3 -177.5(5) . . . . no
O1 C6 C7 C8 177.8(4) . . . . no
C26 C6 C7 C8 -63.7(7) . . . . no
C5 C6 C7 C8 66.5(6) . . . . no
O2 C7 C8 C9 -79.9(5) . . . . no
O3 C7 C8 C9 36.5(5) . . . . no
C6 C7 C8 C9 155.1(5) . . . . no
C7 C8 C9 C10 -31.0(6) . . . . no
C8 C9 C10 O3 14.8(6) . . . . no
C8 C9 C10 C11 -101.9(5) . . . . no
C8 C9 C10 C27 132.5(5) . . . . no
O3 C10 C11 O4 -66.4(6) . . . . no
C27 C10 C11 O4 174.9(5) . . . . no
C9 C10 C11 O4 48.9(6) . . . . no
O3 C10 C11 C12 51.8(6) . . . . no
C27 C10 C11 C12 -66.9(6) . . . . no
C9 C10 C11 C12 167.2(5) . . . . no
O4 C11 C12 C13 -34.4(6) . . . . no
C10 C11 C12 C13 -156.1(5) . . . . no
C11 C12 C13 C14 35.2(6) . . . . no
C12 C13 C14 O4 -23.8(6) . . . . no
C12 C13 C14 C15 -145.8(5) . . . . no
O4 C14 C15 O5 -64.0(6) . . . . no
C13 C14 C15 O5 54.8(6) . . . . no
O4 C14 C15 C28 179.8(5) . . . . no
C13 C14 C15 C28 -61.5(6) . . . . no
O4 C14 C15 C16 51.1(6) . . . . no
C13 C14 C15 C16 169.8(5) . . . . no
O5 C15 C16 C17 25.3(6) . . . . no
C14 C15 C16 C17 -92.2(5) . . . . no
C28 C15 C16 C17 141.1(5) . . . . no
C15 C16 C17 C18 -20.8(6) . . . . no
C16 C17 C18 O5 8.7(6) . . . . no
C16 C17 C18 C19 -112.0(6) . . . . no
O5 C18 C19 O6 -66.0(5) . . . . no
C17 C18 C19 O6 54.8(6) . . . . no
O5 C18 C19 C29 176.5(5) . . . . no
C17 C18 C19 C29 -62.7(7) . . . . no
O5 C18 C19 C20 47.1(7) . . . . no
C17 C18 C19 C20 167.9(5) . . . . no
O6 C19 C20 C21 -15.1(6) . . . . no
C29 C19 C20 C21 99.9(6) . . . . no
C18 C19 C20 C21 -130.0(5) . . . . no
C19 C20 C21 C22 32.6(6) . . . . no
C20 C21 C22 O6 -38.2(6) . . . . no
C20 C21 C22 C23 -157.8(5) . . . . no
O6 C22 C23 O7 -55.9(6) . . . . no
C21 C22 C23 O7 61.3(7) . . . . no
O6 C22 C23 C24 62.8(6) . . . . no
C21 C22 C23 C24 -180.0(6) . . . . no
O6 C22 C23 C30 -173.6(5) . . . . no
C21 C22 C23 C30 -56.4(7) . . . . no
C26 C6 O1 C3 166.5(4) . . . . no
C7 C6 O1 C3 -70.7(5) . . . . no
C5 C6 O1 C3 46.3(5) . . . . no
C4 C3 O1 C6 -46.5(5) . . . . no
C2 C3 O1 C6 75.7(5) . . . . no
O3 C7 O2 C2 76.2(6) . . . . no
C6 C7 O2 C2 -44.0(6) . . . . no
C8 C7 O2 C2 -171.7(5) . . . . no
C1 C2 O2 C7 165.4(5) . . . . no
C25 C2 O2 C7 -73.8(6) . . . . no
C3 C2 O2 C7 45.6(6) . . . . no
O2 C7 O3 C10 85.4(5) . . . . no
C6 C7 O3 C10 -152.6(4) . . . . no
C8 C7 O3 C10 -28.8(5) . . . . no
C11 C10 O3 C7 129.1(5) . . . . no
C27 C10 O3 C7 -110.8(5) . . . . no
C9 C10 O3 C7 8.8(5) . . . . no
C10 C11 O4 C14 145.7(5) . . . . no
C12 C11 O4 C14 20.1(6) . . . . no
C15 C14 O4 C11 126.3(5) . . . . no
C13 C14 O4 C11 2.1(6) . . . . no
C17 C18 O5 C15 7.7(6) . . . . no
C19 C18 O5 C15 133.4(5) . . . . no
C14 C15 O5 C18 99.8(5) . . . . no
C28 C15 O5 C18 -141.6(5) . . . . no
C16 C15 O5 C18 -20.7(6) . . . . no
C21 C22 O6 C19 30.0(6) . . . . no
C23 C22 O6 C19 156.4(4) . . . . no
C29 C19 O6 C22 -127.6(5) . . . . no
C18 C19 O6 C22 110.8(5) . . . . no
C20 C19 O6 C22 -9.3(6) . . . . no

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        25.07
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.061