# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry
# This journal is © The Royal Society of Chemistry 2011
data_global
_journal_name_full Org.Biomol.Chem.
_journal_coden_cambridge 0177
_audit_creation_date 06-06-11
_publ_contact_author_name 'Catherine Guillou'
_publ_contact_author_address
;Centre de Recherches de Gif
Institut de Chimie des Substances Naturelles-CNRS
1 avenue de la Terrasse
91198 Gif sur Yvette
France
;
_publ_contact_author_phone +3316982
_publ_contact_author_fax +33169077247
_publ_contact_author_email catherine.guillou@icsn.cnrs-gif.fr
_publ_contact_letter
;
;
_publ_requested_category FM
_publ_section_title
;
Routes to ................
..........................
..........................
;
loop_
_publ_author_name
_publ_author_address
C.Guillou
;Centre de Recherches de Gif
Institut de Chimie des Substances Naturelles-CNRS
1 avenue de la Terrasse
91198 Gif sur Yvette
France
;
L.Chabaud
;Centre de Recherches de Gif
Institut de Chimie des Substances Naturelles-CNRS
1 avenue de la Terrasse
91198 Gif sur Yvette
France
;
L.Duroure
;Centre de Recherches de Gif
Institut de Chimie des Substances Naturelles-CNRS
1 avenue de la Terrasse
91198 Gif sur Yvette
France
;
P.Retailleau ''
T.Jousseaume ''
E.Barre ''
R.Araoz ''
J.Molgo ''
_publ_section_abstract
; ?
;
_publ_section_comment
; ?
;
_publ_section_exptl_prep
; ?
;
_publ_section_exptl_refinement
; ?
;
_publ_section_references
;
Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C.,
Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J.
Appl. Cryst. 32, 115-119.
Beurskens,P.T., Beurskens, G., de Gelder, R. Garcia-Granda, S., Gould,R.O.,
Israel, R. and Smits, J.M.M. (1999). The DIRDIF-99 program system,
Crystallography Laboratory, University of Nijmegen, The Netherlands.
Coppens, P. (1970). Crystallographic Computing, edited by F. R. Ahmed,
S. R. Hall & C. P. Huber, pp. 255-270. Copenhagen: Munksgaard.
Macrae, C. F., Edgington, P. R., McCabe, P., Pidcock, E., Shields, G. P.,
Taylor, R., Towler, M. & van de Streek, J. (2006). Mercury: visualization and
analysis of crystal structures. J.Appl. Cryst. 39, 453-457.
Nonius, B. V. (1999). COLLECT, data collection software.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Volume 276,
Macromolecular Crystallography, part A, edited by C.W. Carter, Jr. & R.M.
Sweet, 307-326, 1997, New York: Academic Press.
Palatinus L., Chapuis G. (2007): Superflip - a computer program for the
solution of crystal structures by charge flipping in arbitrary dimensions.
J.Appl. Cryst. 40, 786-790.
Sheldrick, G.M. (2008).Acta Cryst. A64, 112-122.
Spek, A. L. (2003). J.Appl. Cryst. 36, 7-13.
Welter, R. (2006). The Crystalbuilder Project
Acta Cryst. A62, s252.
Westrip, S. P. (2008). publCIF. In preparation.
;
_publ_section_figure_captions
; ?
;
_publ_section_acknowledgements
; ?
;
data_LC382
_database_code_depnum_ccdc_archive 'CCDC 828699'
#TrackingRef 'Cif-lactone-OBC-Guillou-et-al.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
rac-7-hydroxy-2-oxaspiro[5.5]undec-8-en-1-one
;
_chemical_name_common rac-7-hydroxy-2-oxaspiro(5.5)undec-8-en-1-one
_chemical_melting_point ?
_chemical_formula_moiety 'C10 H14 O3'
_chemical_formula_sum 'C10 H14 O3'
_chemical_formula_weight 182.21
_chemical_absolute_configuration .
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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_space_group_name_Hall '-P 2ybc'
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 9.1149(11)
_cell_length_b 6.9784(8)
_cell_length_c 14.9231(15)
_cell_angle_alpha 90.00
_cell_angle_beta 98.171(7)
_cell_angle_gamma 90.00
_cell_volume 939.58(18)
_cell_formula_units_Z 4
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 1259
_cell_measurement_theta_min 7.0
_cell_measurement_theta_max 71.3
_exptl_crystal_description block
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.48
_exptl_crystal_size_mid 0.43
_exptl_crystal_size_min 0.32
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.288
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 392
_exptl_absorpt_coefficient_mu 0.775
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.739
_exptl_absorpt_process_details 'FS_ABSCOR (Rigaku, 2009)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 1.54187
_diffrn_radiation_type CuK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Rigaku rapid II RAXIS conversion'
_diffrn_measurement_method 'profile data from \w-scans'
_diffrn_detector_type
'RAPID II large area curved imaging plate detector '
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 3666
_diffrn_reflns_av_R_equivalents 0.0430
_diffrn_reflns_av_sigmaI/netI 0.0369
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_k_max 5
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_theta_min 7.02
_diffrn_reflns_theta_max 68.97
_reflns_number_total 1676
_reflns_number_gt 1173
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_cell_refinement 'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction 'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_structure_solution 'Superflip (Sheldrick, 2008)'
_computing_structure_refinement
'SHELXL97 (Sheldrick, 2008); CRYSTALBUILDER (Welter, 2006)'
_computing_molecular_graphics 'PLATON (Spek, 2003)'
_computing_publication_material 'SHELXL97 (Sheldrick, 2008)'
_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^)+(0.0948P)^2^+0.0818P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method SHELXL
_refine_ls_extinction_coef 0.012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns 1676
_refine_ls_number_parameters 130
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0682
_refine_ls_R_factor_gt 0.0524
_refine_ls_wR_factor_ref 0.1804
_refine_ls_wR_factor_gt 0.1617
_refine_ls_goodness_of_fit_ref 1.091
_refine_ls_restrained_S_all 1.091
_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
O10 O -0.02665(19) 0.8004(2) 0.05606(11) 0.0886(6) Uani 1 1 d . A .
O12 O 0.2116(2) 0.3596(3) 0.13632(12) 0.1064(7) Uani 1 1 d . . .
H12 H 0.1337 0.3311 0.1045 0.160 Uiso 1 1 calc R . .
O13 O 0.08325(18) 0.6705(2) -0.04810(10) 0.0877(6) Uani 1 1 d . A .
C1 C 0.5035(3) 0.8159(5) 0.1114(2) 0.1212(12) Uani 1 1 d . . .
H1A H 0.5757 0.8670 0.0758 0.145 Uiso 1 1 calc R . .
H1B H 0.5066 0.8941 0.1653 0.145 Uiso 1 1 calc R . .
C2 C 0.5451(3) 0.6180(6) 0.13823(19) 0.1170(11) Uani 1 1 d . . .
H2 H 0.6424 0.5940 0.1638 0.140 Uiso 1 1 calc R . .
C3 C 0.4523(3) 0.4743(5) 0.12795(15) 0.0990(9) Uani 1 1 d . . .
H3 H 0.4880 0.3536 0.1462 0.119 Uiso 1 1 calc R . .
C4 C 0.2924(2) 0.4914(4) 0.08870(13) 0.0790(7) Uani 1 1 d . . .
H4 H 0.2813 0.4535 0.0249 0.095 Uiso 1 1 calc R . .
C5 C 0.2382(2) 0.6991(3) 0.09462(13) 0.0684(6) Uani 1 1 d . A .
C6 C 0.3502(3) 0.8301(4) 0.05656(17) 0.0928(8) Uani 1 1 d . . .
H6A H 0.3557 0.7946 -0.0057 0.111 Uiso 1 1 calc R . .
H6B H 0.3160 0.9616 0.0570 0.111 Uiso 1 1 calc R . .
C7 C 0.2205(3) 0.7499(4) 0.19235(15) 0.0963(8) Uani 1 1 d . . .
H7A H 0.1959 0.6342 0.2230 0.116 Uiso 0.708(13) 1 calc PR A 1
H7B H 0.3150 0.7956 0.2230 0.116 Uiso 0.708(13) 1 calc PR A 1
H7C H 0.2678 0.6499 0.2314 0.116 Uiso 0.292(13) 1 calc PR A 2
H7D H 0.2747 0.8676 0.2081 0.116 Uiso 0.292(13) 1 calc PR A 2
C8A C 0.1088(5) 0.8932(11) 0.2013(3) 0.0926(18) Uani 0.708(13) 1 d P A 1
H8A1 H 0.0948 0.9003 0.2645 0.111 Uiso 0.708(13) 1 calc PR A 1
H8A2 H 0.1457 1.0167 0.1848 0.111 Uiso 0.708(13) 1 calc PR A 1
C8B C 0.0775(15) 0.774(2) 0.2122(6) 0.089(4) Uani 0.292(13) 1 d P A 2
H8B1 H 0.0843 0.8489 0.2673 0.107 Uiso 0.292(13) 1 calc PR A 2
H8B2 H 0.0411 0.6481 0.2260 0.107 Uiso 0.292(13) 1 calc PR A 2
C9 C -0.0332(3) 0.8605(5) 0.1477(2) 0.1042(9) Uani 1 1 d . . .
H9A H -0.0855 0.7634 0.1773 0.125 Uiso 0.708(13) 1 calc PR A 1
H9B H -0.0906 0.9777 0.1461 0.125 Uiso 0.708(13) 1 calc PR A 1
H9C H -0.0218 0.9986 0.1513 0.125 Uiso 0.292(13) 1 calc PR A 2
H9D H -0.1301 0.8292 0.1632 0.125 Uiso 0.292(13) 1 calc PR A 2
C11 C 0.0927(3) 0.7219(3) 0.03037(14) 0.0723(6) 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
O10 0.0841(11) 0.0862(12) 0.0907(11) -0.0064(8) -0.0039(8) 0.0117(8)
O12 0.1118(14) 0.0966(12) 0.0994(13) 0.0395(10) -0.0243(10) -0.0177(10)
O13 0.1005(12) 0.0992(13) 0.0581(9) 0.0048(7) -0.0073(7) 0.0014(8)
C1 0.0891(18) 0.160(3) 0.111(2) 0.044(2) 0.0016(15) -0.0382(18)
C2 0.0769(16) 0.173(3) 0.0987(19) 0.046(2) 0.0049(14) -0.003(2)
C3 0.0914(17) 0.120(2) 0.0825(16) 0.0203(15) 0.0021(12) 0.0184(17)
C4 0.0878(14) 0.0871(16) 0.0585(10) 0.0088(11) -0.0016(9) 0.0053(12)
C5 0.0742(13) 0.0743(14) 0.0546(11) 0.0062(9) 0.0014(9) -0.0063(10)
C6 0.0922(17) 0.0992(19) 0.0845(16) 0.0245(13) 0.0042(12) -0.0175(14)
C7 0.0997(18) 0.123(2) 0.0626(13) -0.0104(13) 0.0001(12) 0.0027(17)
C8A 0.112(3) 0.095(4) 0.072(2) -0.011(2) 0.0178(19) -0.001(3)
C8B 0.133(9) 0.072(8) 0.066(5) 0.012(4) 0.029(5) 0.002(6)
C9 0.107(2) 0.113(2) 0.0930(18) -0.0089(16) 0.0167(15) 0.0154(16)
C11 0.0852(15) 0.0669(13) 0.0614(12) 0.0097(9) -0.0017(10) -0.0051(11)
_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
O10 C11 1.322(3) . ?
O10 C9 1.439(3) . ?
O12 C4 1.429(3) . ?
O12 H12 0.8200 . ?
O13 C11 1.216(2) . ?
C1 C2 1.472(5) . ?
C1 C6 1.519(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.306(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.496(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.538(3) . ?
C4 H4 0.9800 . ?
C5 C11 1.530(3) . ?
C5 C7 1.532(3) . ?
C5 C6 1.538(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8B 1.387(12) . ?
C7 C8A 1.447(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 H7C 0.9700 . ?
C7 H7D 0.9700 . ?
C8A C9 1.440(5) . ?
C8A H8A1 0.9700 . ?
C8A H8A2 0.9700 . ?
C8B C9 1.426(11) . ?
C8B H8B1 0.9700 . ?
C8B H8B2 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 H9C 0.9700 . ?
C9 H9D 0.9700 . ?
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
C11 O10 C9 122.88(19) . . ?
C4 O12 H12 109.5 . . ?
C2 C1 C6 112.9(3) . . ?
C2 C1 H1A 109.0 . . ?
C6 C1 H1A 109.0 . . ?
C2 C1 H1B 109.0 . . ?
C6 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
C3 C2 C1 123.4(3) . . ?
C3 C2 H2 118.3 . . ?
C1 C2 H2 118.3 . . ?
C2 C3 C4 124.3(3) . . ?
C2 C3 H3 117.9 . . ?
C4 C3 H3 117.9 . . ?
O12 C4 C3 107.26(18) . . ?
O12 C4 C5 112.65(19) . . ?
C3 C4 C5 110.8(2) . . ?
O12 C4 H4 108.7 . . ?
C3 C4 H4 108.7 . . ?
C5 C4 H4 108.7 . . ?
C11 C5 C7 111.93(19) . . ?
C11 C5 C6 105.57(16) . . ?
C7 C5 C6 112.3(2) . . ?
C11 C5 C4 108.61(16) . . ?
C7 C5 C4 110.56(18) . . ?
C6 C5 C4 107.66(19) . . ?
C1 C6 C5 111.76(19) . . ?
C1 C6 H6A 109.3 . . ?
C5 C6 H6A 109.3 . . ?
C1 C6 H6B 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 107.9 . . ?
C8B C7 C8A 37.1(5) . . ?
C8B C7 C5 117.4(5) . . ?
C8A C7 C5 114.8(3) . . ?
C8B C7 H7A 73.2 . . ?
C8A C7 H7A 108.6 . . ?
C5 C7 H7A 108.6 . . ?
C8B C7 H7B 131.2 . . ?
C8A C7 H7B 108.6 . . ?
C5 C7 H7B 108.6 . . ?
H7A C7 H7B 107.6 . . ?
C8B C7 H7C 108.0 . . ?
C8A C7 H7C 134.4 . . ?
C5 C7 H7C 108.0 . . ?
H7A C7 H7C 39.7 . . ?
H7B C7 H7C 70.4 . . ?
C8B C7 H7D 108.0 . . ?
C8A C7 H7D 74.5 . . ?
C5 C7 H7D 108.0 . . ?
H7A C7 H7D 137.3 . . ?
H7B C7 H7D 38.7 . . ?
H7C C7 H7D 107.2 . . ?
C9 C8A C7 115.3(4) . . ?
C9 C8A H8A1 108.4 . . ?
C7 C8A H8A1 108.4 . . ?
C9 C8A H8A2 108.4 . . ?
C7 C8A H8A2 108.4 . . ?
H8A1 C8A H8A2 107.5 . . ?
C7 C8B C9 120.2(7) . . ?
C7 C8B H8B1 107.3 . . ?
C9 C8B H8B1 107.3 . . ?
C7 C8B H8B2 107.3 . . ?
C9 C8B H8B2 107.3 . . ?
H8B1 C8B H8B2 106.9 . . ?
C8B C9 O10 113.4(5) . . ?
C8B C9 C8A 36.7(5) . . ?
O10 C9 C8A 114.8(3) . . ?
C8B C9 H9A 75.1 . . ?
O10 C9 H9A 108.6 . . ?
C8A C9 H9A 108.6 . . ?
C8B C9 H9B 134.5 . . ?
O10 C9 H9B 108.6 . . ?
C8A C9 H9B 108.6 . . ?
H9A C9 H9B 107.6 . . ?
C8B C9 H9C 108.9 . . ?
O10 C9 H9C 108.9 . . ?
C8A C9 H9C 74.4 . . ?
H9A C9 H9C 136.4 . . ?
H9B C9 H9C 38.4 . . ?
C8B C9 H9D 108.9 . . ?
O10 C9 H9D 108.9 . . ?
C8A C9 H9D 132.8 . . ?
H9A C9 H9D 37.9 . . ?
H9B C9 H9D 71.9 . . ?
H9C C9 H9D 107.7 . . ?
O13 C11 O10 116.92(19) . . ?
O13 C11 C5 120.6(2) . . ?
O10 C11 C5 122.46(19) . . ?
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
C6 C1 C2 C3 -9.6(5) . . . . ?
C1 C2 C3 C4 -0.6(5) . . . . ?
C2 C3 C4 O12 -144.1(3) . . . . ?
C2 C3 C4 C5 -20.8(4) . . . . ?
O12 C4 C5 C11 -76.3(2) . . . . ?
C3 C4 C5 C11 163.49(18) . . . . ?
O12 C4 C5 C7 46.8(2) . . . . ?
C3 C4 C5 C7 -73.3(2) . . . . ?
O12 C4 C5 C6 169.82(17) . . . . ?
C3 C4 C5 C6 49.6(2) . . . . ?
C2 C1 C6 C5 41.2(4) . . . . ?
C11 C5 C6 C1 -177.4(2) . . . . ?
C7 C5 C6 C1 60.4(3) . . . . ?
C4 C5 C6 C1 -61.5(3) . . . . ?
C11 C5 C7 C8B 11.3(8) . . . . ?
C6 C5 C7 C8B 129.8(8) . . . . ?
C4 C5 C7 C8B -109.9(8) . . . . ?
C11 C5 C7 C8A -30.1(5) . . . . ?
C6 C5 C7 C8A 88.5(4) . . . . ?
C4 C5 C7 C8A -151.3(4) . . . . ?
C8B C7 C8A C9 -54.2(7) . . . . ?
C5 C7 C8A C9 49.1(7) . . . . ?
C8A C7 C8B C9 58.9(9) . . . . ?
C5 C7 C8B C9 -36.6(16) . . . . ?
C7 C8B C9 O10 40.4(15) . . . . ?
C7 C8B C9 C8A -60.2(11) . . . . ?
C11 O10 C9 C8B -19.4(8) . . . . ?
C11 O10 C9 C8A 21.0(5) . . . . ?
C7 C8A C9 C8B 52.7(7) . . . . ?
C7 C8A C9 O10 -43.7(7) . . . . ?
C9 O10 C11 O13 177.4(2) . . . . ?
C9 O10 C11 C5 -3.9(3) . . . . ?
C7 C5 C11 O13 -173.1(2) . . . . ?
C6 C5 C11 O13 64.5(3) . . . . ?
C4 C5 C11 O13 -50.7(3) . . . . ?
C7 C5 C11 O10 8.2(3) . . . . ?
C6 C5 C11 O10 -114.2(2) . . . . ?
C4 C5 C11 O10 130.6(2) . . . . ?
_diffrn_measured_fraction_theta_max 0.962
_diffrn_reflns_theta_full 68.97
_diffrn_measured_fraction_theta_full 0.962
_refine_diff_density_max 0.188
_refine_diff_density_min -0.174
_refine_diff_density_rms 0.037
#===END