# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2012


data_global
_journal_name_full               Chem.Commun.
_journal_coden_cambridge         0182
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_email       yasu.y.aa@m.titech.ac.jp
_publ_contact_author_name        'Yusuke Yasu'
loop_
_publ_author_name
'Yusuke Yasu'
'Takashi Koike'
'Munetaka Akita'

data_1234_0ma
_database_code_depnum_ccdc_archive 'CCDC 869541'
#TrackingRef 'web_deposit_cif_file_0_YusukeYasu_1330430092.1234_0ma.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H24 O4'
_chemical_formula_weight         352.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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                   6.9714(17)
_cell_length_b                   9.360(3)
_cell_length_c                   15.546(4)
_cell_angle_alpha                75.680(4)
_cell_angle_beta                 82.150(3)
_cell_angle_gamma                68.441(3)
_cell_volume                     913.0(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    90
_cell_measurement_reflns_used    1633
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      28.29
_exptl_crystal_description       platet
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             376
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9913
_exptl_absorpt_correction_T_max  0.9957
_exptl_absorpt_process_details   
;
SADABS Sheldrick 1996
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_reflns_number            4336
_diffrn_reflns_av_R_equivalents  0.1354
_diffrn_reflns_av_sigmaI/netI    0.0922
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.40
_diffrn_reflns_theta_max         25.02
_reflns_number_total             3152
_reflns_number_gt                2203
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_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^)+(0.1544P)^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_extinction_coef       ?
_refine_ls_number_reflns         3152
_refine_ls_number_parameters     236
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1027
_refine_ls_R_factor_gt           0.0812
_refine_ls_wR_factor_ref         0.2357
_refine_ls_wR_factor_gt          0.2169
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_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 1.5598(3) 0.8621(2) -0.10015(14) 0.0289(6) Uani 1 1 d . . .
O2 O 0.9516(3) 0.5788(2) 0.15409(13) 0.0233(5) Uani 1 1 d . . .
O3 O 0.1969(3) 0.4788(2) 0.40586(14) 0.0289(6) Uani 1 1 d . . .
O4 O 0.2260(4) 0.1295(3) 0.45506(17) 0.0463(7) Uani 1 1 d . . .
C1 C 1.6694(5) 0.7937(4) -0.1732(2) 0.0344(8) Uani 1 1 d . . .
H1 H 1.7173 0.6788 -0.1546 0.052 Uiso 1 1 calc R . .
H3 H 1.7885 0.8278 -0.1927 0.052 Uiso 1 1 calc R . .
H24 H 1.5776 0.8278 -0.2225 0.052 Uiso 1 1 calc R . .
C2 C 1.3965(5) 0.8174(3) -0.06015(19) 0.0234(7) Uani 1 1 d . . .
C3 C 1.3081(4) 0.8706(3) 0.01677(19) 0.0238(7) Uani 1 1 d . . .
H4 H 1.3623 0.9330 0.0391 0.029 Uiso 1 1 calc R . .
C4 C 1.1418(5) 0.8332(3) 0.06086(19) 0.0232(7) Uani 1 1 d . . .
H5 H 1.0825 0.8704 0.1134 0.028 Uiso 1 1 calc R . .
C5 C 1.0592(5) 0.7421(3) 0.02977(19) 0.0229(7) Uani 1 1 d . . .
C6 C 0.8771(5) 0.7030(4) 0.07710(19) 0.0255(7) Uani 1 1 d . . .
H23 H 0.7729 0.7967 0.0957 0.031 Uiso 1 1 calc R . .
H22 H 0.8124 0.6676 0.0375 0.031 Uiso 1 1 calc R . .
C7 C 0.8060(5) 0.5379(3) 0.21259(19) 0.0206(7) Uani 1 1 d . . .
C8 C 0.8805(5) 0.4339(3) 0.29225(19) 0.0227(7) Uani 1 1 d . . .
H21 H 1.0240 0.3949 0.3020 0.027 Uiso 1 1 calc R . .
C9 C 0.7455(5) 0.3887(3) 0.35613(19) 0.0229(7) Uani 1 1 d . . .
H20 H 0.7972 0.3171 0.4098 0.027 Uiso 1 1 calc R . .
C10 C 0.5339(5) 0.4456(3) 0.34394(19) 0.0218(7) Uani 1 1 d . . .
C11 C 0.3806(5) 0.4084(3) 0.41451(19) 0.0219(7) Uani 1 1 d . . .
C12 C 0.4593(5) 0.2867(3) 0.49765(19) 0.0231(7) Uani 1 1 d . . .
H19 H 0.5416 0.3237 0.5284 0.028 Uiso 1 1 calc R . .
H18 H 0.5524 0.1880 0.4805 0.028 Uiso 1 1 calc R . .
C13 C 0.2904(5) 0.2521(3) 0.56175(19) 0.0232(7) Uani 1 1 d . . .
H17 H 0.1856 0.3549 0.5705 0.028 Uiso 1 1 calc R . .
C14 C 0.1798(5) 0.1649(3) 0.52764(19) 0.0253(7) Uani 1 1 d . . .
C15 C 0.0147(5) 0.1264(4) 0.5897(2) 0.0329(8) Uani 1 1 d . . .
H10 H -0.0399 0.0622 0.5647 0.039 Uiso 1 1 calc R . .
H11 H -0.1002 0.2249 0.5957 0.039 Uiso 1 1 calc R . .
C16 C 0.0957(6) 0.0359(4) 0.6815(2) 0.0347(8) Uani 1 1 d . . .
H2 H -0.0208 0.0227 0.7229 0.042 Uiso 1 1 calc R . .
H12 H 0.1945 -0.0700 0.6772 0.042 Uiso 1 1 calc R . .
C17 C 1.1481(5) 0.6907(4) -0.0478(2) 0.0282(8) Uani 1 1 d . . .
H7 H 1.0919 0.6297 -0.0704 0.034 Uiso 1 1 calc R . .
C18 C 1.3165(5) 0.7257(4) -0.0932(2) 0.0282(8) Uani 1 1 d . . .
H6 H 1.3762 0.6883 -0.1457 0.034 Uiso 1 1 calc R . .
C19 C 0.4634(5) 0.5458(4) 0.26345(19) 0.0244(7) Uani 1 1 d . . .
H9 H 0.3202 0.5832 0.2533 0.029 Uiso 1 1 calc R . .
C20 C 0.5965(5) 0.5919(4) 0.1981(2) 0.0256(7) Uani 1 1 d . . .
H8 H 0.5453 0.6601 0.1435 0.031 Uiso 1 1 calc R . .
C21 C 0.3722(5) 0.1564(4) 0.65304(19) 0.0278(7) Uani 1 1 d . . .
H16 H 0.4805 0.0555 0.6457 0.033 Uiso 1 1 calc R . .
H15 H 0.4362 0.2151 0.6777 0.033 Uiso 1 1 calc R . .
C22 C 0.2026(5) 0.1231(4) 0.7179(2) 0.0284(7) Uani 1 1 d . . .
H14 H 0.0997 0.2236 0.7291 0.034 Uiso 1 1 calc R . .
H13 H 0.2626 0.0589 0.7751 0.034 Uiso 1 1 calc 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
O1 0.0308(12) 0.0360(13) 0.0254(12) -0.0031(10) 0.0015(9) -0.0211(10)
O2 0.0276(11) 0.0284(11) 0.0175(11) 0.0017(9) -0.0038(9) -0.0172(9)
O3 0.0285(13) 0.0338(12) 0.0255(12) -0.0023(10) -0.0037(9) -0.0141(10)
O4 0.0593(17) 0.0519(16) 0.0394(15) -0.0155(13) -0.0013(13) -0.0294(13)
C1 0.0341(18) 0.0400(19) 0.0292(18) -0.0062(15) 0.0066(14) -0.0166(16)
C2 0.0278(16) 0.0242(15) 0.0189(15) 0.0039(12) -0.0048(13) -0.0139(13)
C3 0.0299(17) 0.0250(15) 0.0204(15) -0.0011(12) -0.0079(13) -0.0143(13)
C4 0.0306(17) 0.0254(16) 0.0145(14) 0.0005(12) -0.0044(12) -0.0127(13)
C5 0.0287(16) 0.0227(15) 0.0177(15) 0.0031(12) -0.0066(12) -0.0124(13)
C6 0.0326(17) 0.0298(16) 0.0167(15) 0.0028(13) -0.0058(13) -0.0171(14)
C7 0.0303(17) 0.0223(15) 0.0155(14) -0.0051(12) -0.0009(12) -0.0158(13)
C8 0.0260(16) 0.0267(16) 0.0206(15) -0.0040(13) -0.0063(12) -0.0140(13)
C9 0.0323(17) 0.0266(16) 0.0145(14) -0.0020(12) -0.0073(12) -0.0151(13)
C10 0.0303(17) 0.0219(15) 0.0206(15) -0.0066(12) -0.0031(13) -0.0157(13)
C11 0.0263(17) 0.0229(15) 0.0234(16) -0.0082(13) -0.0035(13) -0.0137(13)
C12 0.0271(16) 0.0255(16) 0.0207(15) -0.0037(13) -0.0046(13) -0.0132(13)
C13 0.0298(16) 0.0253(15) 0.0192(15) -0.0035(13) -0.0025(12) -0.0154(13)
C14 0.0341(17) 0.0251(16) 0.0201(16) -0.0075(13) -0.0064(13) -0.0109(14)
C15 0.0406(19) 0.0334(18) 0.0348(19) -0.0071(15) -0.0040(15) -0.0240(16)
C16 0.047(2) 0.0331(18) 0.0311(18) -0.0051(15) 0.0068(15) -0.0268(16)
C17 0.0415(19) 0.0323(17) 0.0207(16) -0.0048(13) -0.0035(14) -0.0242(15)
C18 0.0417(19) 0.0301(17) 0.0186(15) -0.0041(13) 0.0014(14) -0.0210(15)
C19 0.0259(16) 0.0301(17) 0.0217(15) -0.0044(13) -0.0059(13) -0.0139(13)
C20 0.0333(17) 0.0279(16) 0.0191(15) -0.0003(13) -0.0063(13) -0.0161(14)
C21 0.0344(18) 0.0331(17) 0.0206(16) -0.0043(14) -0.0050(13) -0.0167(15)
C22 0.0441(19) 0.0290(16) 0.0167(15) -0.0001(13) -0.0037(14) -0.0204(15)

_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 C2 1.373(3) . ?
O1 C1 1.431(4) . ?
O2 C7 1.365(3) . ?
O2 C6 1.446(3) . ?
O3 C11 1.215(4) . ?
O4 C14 1.222(4) . ?
C1 H1 0.9800 . ?
C1 H3 0.9800 . ?
C1 H24 0.9800 . ?
C2 C3 1.388(4) . ?
C2 C18 1.400(4) . ?
C3 C4 1.378(4) . ?
C3 H4 0.9500 . ?
C4 C5 1.391(4) . ?
C4 H5 0.9500 . ?
C5 C17 1.390(4) . ?
C5 C6 1.497(4) . ?
C6 H23 0.9900 . ?
C6 H22 0.9900 . ?
C7 C20 1.390(4) . ?
C7 C8 1.399(4) . ?
C8 C9 1.371(4) . ?
C8 H21 0.9500 . ?
C9 C10 1.395(4) . ?
C9 H20 0.9500 . ?
C10 C19 1.391(4) . ?
C10 C11 1.494(4) . ?
C11 C12 1.508(4) . ?
C12 C13 1.512(4) . ?
C12 H19 0.9900 . ?
C12 H18 0.9900 . ?
C13 C14 1.526(4) . ?
C13 C21 1.536(4) . ?
C13 H17 1.0000 . ?
C14 C15 1.488(4) . ?
C15 C16 1.532(5) . ?
C15 H10 0.9900 . ?
C15 H11 0.9900 . ?
C16 C22 1.527(4) . ?
C16 H2 0.9900 . ?
C16 H12 0.9900 . ?
C17 C18 1.388(4) . ?
C17 H7 0.9500 . ?
C18 H6 0.9500 . ?
C19 C20 1.378(4) . ?
C19 H9 0.9500 . ?
C20 H8 0.9500 . ?
C21 C22 1.517(4) . ?
C21 H16 0.9900 . ?
C21 H15 0.9900 . ?
C22 H14 0.9900 . ?
C22 H13 0.9900 . ?

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 O1 C1 117.2(2) . . ?
C7 O2 C6 116.8(2) . . ?
O1 C1 H1 109.5 . . ?
O1 C1 H3 109.5 . . ?
H1 C1 H3 109.5 . . ?
O1 C1 H24 109.5 . . ?
H1 C1 H24 109.5 . . ?
H3 C1 H24 109.5 . . ?
O1 C2 C3 116.1(3) . . ?
O1 C2 C18 123.9(3) . . ?
C3 C2 C18 120.0(3) . . ?
C4 C3 C2 120.2(3) . . ?
C4 C3 H4 119.9 . . ?
C2 C3 H4 119.9 . . ?
C3 C4 C5 121.2(3) . . ?
C3 C4 H5 119.4 . . ?
C5 C4 H5 119.4 . . ?
C17 C5 C4 118.1(3) . . ?
C17 C5 C6 120.8(3) . . ?
C4 C5 C6 121.2(3) . . ?
O2 C6 C5 107.3(2) . . ?
O2 C6 H23 110.2 . . ?
C5 C6 H23 110.2 . . ?
O2 C6 H22 110.2 . . ?
C5 C6 H22 110.2 . . ?
H23 C6 H22 108.5 . . ?
O2 C7 C20 124.9(3) . . ?
O2 C7 C8 115.4(2) . . ?
C20 C7 C8 119.7(3) . . ?
C9 C8 C7 119.7(3) . . ?
C9 C8 H21 120.1 . . ?
C7 C8 H21 120.1 . . ?
C8 C9 C10 121.3(3) . . ?
C8 C9 H20 119.3 . . ?
C10 C9 H20 119.3 . . ?
C19 C10 C9 118.1(3) . . ?
C19 C10 C11 119.0(3) . . ?
C9 C10 C11 122.9(3) . . ?
O3 C11 C10 120.3(3) . . ?
O3 C11 C12 121.1(3) . . ?
C10 C11 C12 118.6(3) . . ?
C11 C12 C13 113.8(2) . . ?
C11 C12 H19 108.8 . . ?
C13 C12 H19 108.8 . . ?
C11 C12 H18 108.8 . . ?
C13 C12 H18 108.8 . . ?
H19 C12 H18 107.7 . . ?
C12 C13 C14 113.3(2) . . ?
C12 C13 C21 111.9(2) . . ?
C14 C13 C21 108.4(2) . . ?
C12 C13 H17 107.7 . . ?
C14 C13 H17 107.7 . . ?
C21 C13 H17 107.7 . . ?
O4 C14 C15 123.4(3) . . ?
O4 C14 C13 121.8(3) . . ?
C15 C14 C13 114.8(2) . . ?
C14 C15 C16 111.5(3) . . ?
C14 C15 H10 109.3 . . ?
C16 C15 H10 109.3 . . ?
C14 C15 H11 109.3 . . ?
C16 C15 H11 109.3 . . ?
H10 C15 H11 108.0 . . ?
C22 C16 C15 110.9(3) . . ?
C22 C16 H2 109.5 . . ?
C15 C16 H2 109.5 . . ?
C22 C16 H12 109.5 . . ?
C15 C16 H12 109.5 . . ?
H2 C16 H12 108.1 . . ?
C18 C17 C5 122.0(3) . . ?
C18 C17 H7 119.0 . . ?
C5 C17 H7 119.0 . . ?
C17 C18 C2 118.6(3) . . ?
C17 C18 H6 120.7 . . ?
C2 C18 H6 120.7 . . ?
C20 C19 C10 121.5(3) . . ?
C20 C19 H9 119.2 . . ?
C10 C19 H9 119.2 . . ?
C19 C20 C7 119.6(3) . . ?
C19 C20 H8 120.2 . . ?
C7 C20 H8 120.2 . . ?
C22 C21 C13 112.1(3) . . ?
C22 C21 H16 109.2 . . ?
C13 C21 H16 109.2 . . ?
C22 C21 H15 109.2 . . ?
C13 C21 H15 109.2 . . ?
H16 C21 H15 107.9 . . ?
C21 C22 C16 111.1(3) . . ?
C21 C22 H14 109.4 . . ?
C16 C22 H14 109.4 . . ?
C21 C22 H13 109.4 . . ?
C16 C22 H13 109.4 . . ?
H14 C22 H13 108.0 . . ?

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 C2 C3 172.7(3) . . . . ?
C1 O1 C2 C18 -8.3(4) . . . . ?
O1 C2 C3 C4 179.2(2) . . . . ?
C18 C2 C3 C4 0.2(4) . . . . ?
C2 C3 C4 C5 0.0(4) . . . . ?
C3 C4 C5 C17 -0.6(4) . . . . ?
C3 C4 C5 C6 -179.3(2) . . . . ?
C7 O2 C6 C5 172.5(2) . . . . ?
C17 C5 C6 O2 103.8(3) . . . . ?
C4 C5 C6 O2 -77.6(3) . . . . ?
C6 O2 C7 C20 8.6(4) . . . . ?
C6 O2 C7 C8 -171.2(2) . . . . ?
O2 C7 C8 C9 178.5(2) . . . . ?
C20 C7 C8 C9 -1.3(4) . . . . ?
C7 C8 C9 C10 -0.7(4) . . . . ?
C8 C9 C10 C19 2.3(4) . . . . ?
C8 C9 C10 C11 -175.4(3) . . . . ?
C19 C10 C11 O3 -8.7(4) . . . . ?
C9 C10 C11 O3 169.0(3) . . . . ?
C19 C10 C11 C12 173.6(3) . . . . ?
C9 C10 C11 C12 -8.7(4) . . . . ?
O3 C11 C12 C13 5.8(4) . . . . ?
C10 C11 C12 C13 -176.6(2) . . . . ?
C11 C12 C13 C14 69.6(3) . . . . ?
C11 C12 C13 C21 -167.6(2) . . . . ?
C12 C13 C14 O4 -0.6(4) . . . . ?
C21 C13 C14 O4 -125.4(3) . . . . ?
C12 C13 C14 C15 179.0(2) . . . . ?
C21 C13 C14 C15 54.2(3) . . . . ?
O4 C14 C15 C16 125.5(3) . . . . ?
C13 C14 C15 C16 -54.1(4) . . . . ?
C14 C15 C16 C22 52.8(4) . . . . ?
C4 C5 C17 C18 1.0(4) . . . . ?
C6 C5 C17 C18 179.7(3) . . . . ?
C5 C17 C18 C2 -0.9(5) . . . . ?
O1 C2 C18 C17 -178.7(3) . . . . ?
C3 C2 C18 C17 0.3(4) . . . . ?
C9 C10 C19 C20 -1.8(4) . . . . ?
C11 C10 C19 C20 175.9(3) . . . . ?
C10 C19 C20 C7 -0.2(4) . . . . ?
O2 C7 C20 C19 -178.1(2) . . . . ?
C8 C7 C20 C19 1.8(4) . . . . ?
C12 C13 C21 C22 179.3(2) . . . . ?
C14 C13 C21 C22 -55.1(3) . . . . ?
C13 C21 C22 C16 57.5(3) . . . . ?
C15 C16 C22 C21 -54.9(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max         1.223
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.095