# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Nakcheol Jeong'
_publ_contact_author_email       NJEONG.KU@GMAIL.COM

_publ_section_title              
;
Guest Dependent Self-Assembly of
(R,R)-2,3-Diphenylsuccinic Acids: Formation of a Cyclotetrameric Chiral
Square
;
loop_
_publ_author_name
'Nakcheol Jeong'
'Jaheon Kim'
'Bohyung Lee'
'Jeong Seok'

# Attachment 'xtal1.cif'

data_xtal1
_database_code_depnum_ccdc_archive 'CCDC 706643'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H24 O5'
_chemical_formula_weight         344.39

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                   9.4617(7)
_cell_length_b                   10.3642(8)
_cell_length_c                   19.7932(15)
_cell_angle_alpha                91.369(2)
_cell_angle_beta                 94.8330(10)
_cell_angle_gamma                101.759(2)
_cell_volume                     1891.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    4065
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      26.3

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             736
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_correction_T_min  
;
Ratio of minimum to maximum apparent transmission: 0.809662
;
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(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  'Bruker SMART CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10669
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0656
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.01
_diffrn_reflns_theta_max         26.37
_reflns_number_total             7475
_reflns_number_gt                4533
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  'Bruker XCIF'

_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)+(0.0681P)²+0.5676P] 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         7475
_refine_ls_number_parameters     482
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1154
_refine_ls_R_factor_gt           0.0608
_refine_ls_wR_factor_ref         0.1638
_refine_ls_wR_factor_gt          0.1377
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.010
_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 1.0155(2) 0.66319(17) 0.49520(9) 0.0370(5) Uani 1 1 d . . .
O2 O 0.9309(2) 0.50988(19) 0.41286(10) 0.0394(5) Uani 1 1 d . . .
H2O H 0.949(3) 0.463(3) 0.4465(16) 0.047 Uiso 1 1 d . . .
O3 O 0.7943(2) 0.90602(19) 0.51505(9) 0.0413(5) Uani 1 1 d . . .
O4 O 0.7012(2) 0.71476(19) 0.45762(10) 0.0396(5) Uani 1 1 d . . .
H4O H 0.648(3) 0.704(3) 0.4888(16) 0.048 Uiso 1 1 d . . .
O5 O 0.4621(2) 0.66520(19) 0.02406(9) 0.0426(5) Uani 1 1 d . . .
O6 O 0.4982(3) 0.7909(2) 0.11968(10) 0.0517(6) Uani 1 1 d . . .
H6O H 0.543(4) 0.844(3) 0.0925(17) 0.062 Uiso 1 1 d . . .
O7 O 0.1358(2) 0.4030(2) -0.00843(10) 0.0437(5) Uani 1 1 d . . .
H7O H 0.062(4) 0.430(3) -0.0275(16) 0.052 Uiso 1 1 d . . .
O8 O 0.1125(2) 0.5564(2) 0.06868(9) 0.0423(5) Uani 1 1 d . . .
C1 C 0.9654(3) 0.6318(3) 0.43677(13) 0.0286(6) Uani 1 1 d . . .
C2 C 0.9380(3) 0.7303(2) 0.38392(13) 0.0295(6) Uani 1 1 d . . .
H2A H 0.8521 0.6879 0.3524 0.035 Uiso 1 1 calc R . .
C3 C 1.0710(3) 0.7610(2) 0.34296(13) 0.0281(6) Uani 1 1 d . . .
C4 C 1.2060(3) 0.8203(3) 0.37352(14) 0.0374(7) Uani 1 1 d . . .
H4A H 1.2170 0.8466 0.4203 0.045 Uiso 1 1 calc R . .
C5 C 1.3266(3) 0.8418(3) 0.33569(15) 0.0428(7) Uani 1 1 d . . .
H5A H 1.4198 0.8809 0.3570 0.051 Uiso 1 1 calc R . .
C6 C 1.3097(3) 0.8062(3) 0.26762(15) 0.0407(7) Uani 1 1 d . . .
H6A H 1.3914 0.8201 0.2419 0.049 Uiso 1 1 calc R . .
C7 C 1.1747(3) 0.7505(3) 0.23697(15) 0.0433(7) Uani 1 1 d . . .
H7A H 1.1631 0.7269 0.1898 0.052 Uiso 1 1 calc R . .
C8 C 1.0556(3) 0.7284(3) 0.27427(13) 0.0350(6) Uani 1 1 d . . .
H8A H 0.9625 0.6906 0.2525 0.042 Uiso 1 1 calc R . .
C9 C 0.7954(3) 0.8292(3) 0.46904(13) 0.0296(6) Uani 1 1 d . . .
C10 C 0.9060(3) 0.8552(2) 0.41638(12) 0.0278(6) Uani 1 1 d . . .
H10A H 0.9989 0.9058 0.4402 0.033 Uiso 1 1 calc R . .
C11 C 0.8514(3) 0.9457(3) 0.36499(12) 0.0280(6) Uani 1 1 d . . .
C12 C 0.8937(3) 1.0803(3) 0.37662(14) 0.0367(7) Uani 1 1 d . . .
H12A H 0.9615 1.1144 0.4141 0.044 Uiso 1 1 calc R . .
C13 C 0.8386(3) 1.1663(3) 0.33443(14) 0.0433(7) Uani 1 1 d . . .
H13A H 0.8675 1.2587 0.3438 0.052 Uiso 1 1 calc R . .
C14 C 0.7420(3) 1.1191(3) 0.27894(14) 0.0376(7) Uani 1 1 d . . .
H14A H 0.7047 1.1784 0.2499 0.045 Uiso 1 1 calc R . .
C15 C 0.7008(3) 0.9859(3) 0.26630(14) 0.0408(7) Uani 1 1 d . . .
H15A H 0.6356 0.9526 0.2278 0.049 Uiso 1 1 calc R . .
C16 C 0.7534(3) 0.8985(3) 0.30931(14) 0.0377(7) Uani 1 1 d . . .
H16A H 0.7221 0.8061 0.3005 0.045 Uiso 1 1 calc R . .
C17 C 0.4542(3) 0.6774(3) 0.08420(13) 0.0325(6) Uani 1 1 d . . .
C18 C 0.3978(3) 0.5652(2) 0.12907(12) 0.0301(6) Uani 1 1 d . . .
H18A H 0.3316 0.5955 0.1600 0.036 Uiso 1 1 calc R . .
C19 C 0.5246(3) 0.5312(2) 0.17193(13) 0.0314(6) Uani 1 1 d . . .
C20 C 0.6400(3) 0.4982(3) 0.14140(15) 0.0431(7) Uani 1 1 d . . .
H20A H 0.6405 0.4982 0.0934 0.052 Uiso 1 1 calc R . .
C21 C 0.7551(3) 0.4651(3) 0.18099(17) 0.0514(8) Uani 1 1 d . . .
H21A H 0.8348 0.4437 0.1602 0.062 Uiso 1 1 calc R . .
C22 C 0.7528(4) 0.4637(3) 0.25081(17) 0.0522(9) Uani 1 1 d . . .
H22A H 0.8310 0.4406 0.2778 0.063 Uiso 1 1 calc R . .
C23 C 0.6386(4) 0.4952(3) 0.28150(16) 0.0494(8) Uani 1 1 d . . .
H23A H 0.6374 0.4933 0.3294 0.059 Uiso 1 1 calc R . .
C24 C 0.5250(3) 0.5297(3) 0.24197(13) 0.0393(7) Uani 1 1 d . . .
H24A H 0.4465 0.5526 0.2631 0.047 Uiso 1 1 calc R . .
C25 C 0.1783(3) 0.4758(3) 0.04782(13) 0.0310(6) Uani 1 1 d . . .
C26 C 0.3116(3) 0.4442(3) 0.08596(12) 0.0301(6) Uani 1 1 d . . .
H26A H 0.3752 0.4191 0.0522 0.036 Uiso 1 1 calc R . .
C27 C 0.2654(3) 0.3265(3) 0.12969(13) 0.0343(6) Uani 1 1 d . . .
C28 C 0.3275(4) 0.2171(3) 0.12493(17) 0.0544(9) Uani 1 1 d . . .
H28A H 0.3953 0.2138 0.0925 0.065 Uiso 1 1 calc R . .
C29 C 0.2924(5) 0.1126(4) 0.1667(2) 0.0722(11) Uani 1 1 d . . .
H29A H 0.3371 0.0387 0.1634 0.087 Uiso 1 1 calc R . .
C30 C 0.1931(5) 0.1157(4) 0.2129(2) 0.0703(11) Uani 1 1 d . . .
H30A H 0.1691 0.0439 0.2417 0.084 Uiso 1 1 calc R . .
C31 C 0.1287(4) 0.2214(4) 0.21783(17) 0.0641(10) Uani 1 1 d . . .
H31A H 0.0585 0.2222 0.2493 0.077 Uiso 1 1 calc R . .
C32 C 0.1655(3) 0.3282(3) 0.17676(15) 0.0484(8) Uani 1 1 d . . .
H32A H 0.1219 0.4025 0.1811 0.058 Uiso 1 1 calc R . .
O1E O 0.5666(2) 0.67663(19) 0.57206(9) 0.0392(5) Uani 1 1 d . . .
C1E C 0.5209(4) 0.7916(3) 0.59552(16) 0.0495(8) Uani 1 1 d . . .
H1EA H 0.6058 0.8650 0.6050 0.059 Uiso 1 1 calc R . .
H1EB H 0.4737 0.7735 0.6381 0.059 Uiso 1 1 calc R . .
C2E C 0.4170(4) 0.8289(4) 0.54259(19) 0.0694(11) Uani 1 1 d . . .
H2EA H 0.3854 0.9078 0.5584 0.083 Uiso 1 1 calc R . .
H2EB H 0.3327 0.7562 0.5337 0.083 Uiso 1 1 calc R . .
H2EC H 0.4645 0.8472 0.5007 0.083 Uiso 1 1 calc R . .
C3E C 0.6751(4) 0.6400(3) 0.61808(16) 0.0520(9) Uani 1 1 d . . .
H3EA H 0.6459 0.6416 0.6649 0.062 Uiso 1 1 calc R . .
H3EB H 0.7682 0.7037 0.6167 0.062 Uiso 1 1 calc R . .
C4E C 0.6933(5) 0.5056(4) 0.5987(2) 0.0792(13) Uani 1 1 d . . .
H4EA H 0.7679 0.4807 0.6302 0.095 Uiso 1 1 calc R . .
H4EB H 0.7229 0.5047 0.5525 0.095 Uiso 1 1 calc R . .
H4EC H 0.6013 0.4427 0.6007 0.095 Uiso 1 1 calc R . .
O2E O 0.6991(3) -0.0366(2) 0.06224(14) 0.0733(8) Uani 1 1 d . . .
C5E C 0.8230(6) -0.0918(5) 0.0546(3) 0.1068(18) Uani 1 1 d . A .
H5EA H 0.8993 -0.0237 0.0375 0.128 Uiso 1 1 calc R . .
H5EB H 0.7966 -0.1651 0.0199 0.128 Uiso 1 1 calc R . .
C6E C 0.8821(5) -0.1409(5) 0.1161(2) 0.0977(16) Uani 1 1 d . . .
H6EA H 0.9663 -0.1776 0.1066 0.117 Uiso 1 1 calc R A .
H6EB H 0.8082 -0.2098 0.1331 0.117 Uiso 1 1 calc R . .
H6EC H 0.9120 -0.0685 0.1504 0.117 Uiso 1 1 calc R . .
C7E C 0.7234(11) 0.1026(9) 0.0792(8) 0.074(4) Uani 0.515(15) 1 d P A 1
H7EA H 0.7657 0.1153 0.1270 0.089 Uiso 0.515(15) 1 calc PR A 1
H7EB H 0.6269 0.1259 0.0781 0.089 Uiso 0.515(15) 1 calc PR A 1
C8E C 0.815(2) 0.2024(14) 0.0398(11) 0.155(9) Uani 0.515(15) 1 d P A 1
H8EA H 0.9046 0.1733 0.0319 0.186 Uiso 0.515(15) 1 calc PR A 1
H8EB H 0.8384 0.2872 0.0655 0.186 Uiso 0.515(15) 1 calc PR A 1
H8EC H 0.7618 0.2123 -0.0038 0.186 Uiso 0.515(15) 1 calc PR A 1
C7E' C 0.6937(9) 0.0783(7) 0.0321(7) 0.055(3) Uani 0.485(15) 1 d P A 2
H7E1 H 0.5934 0.0930 0.0312 0.067 Uiso 0.485(15) 1 calc PR A 2
H7E2 H 0.7165 0.0699 -0.0155 0.067 Uiso 0.485(15) 1 calc PR A 2
C8E' C 0.789(2) 0.1902(11) 0.0639(10) 0.135(10) Uani 0.485(15) 1 d P A 2
H8E1 H 0.8711 0.1625 0.0891 0.162 Uiso 0.485(15) 1 calc PR A 2
H8E2 H 0.7377 0.2340 0.0954 0.162 Uiso 0.485(15) 1 calc PR A 2
H8E3 H 0.8256 0.2516 0.0294 0.162 Uiso 0.485(15) 1 calc PR A 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
O1 C1 1.223(3) . ?
O2 C1 1.306(3) . ?
O2 H2O 0.86(3) . ?
O3 C9 1.198(3) . ?
O4 C9 1.332(3) . ?
O4 H4O 0.83(3) . ?
O5 C17 1.204(3) . ?
O6 C17 1.328(3) . ?
O6 H6O 0.85(3) . ?
O7 C25 1.316(3) . ?
O7 H7O 0.86(3) . ?
O8 C25 1.223(3) . ?
C1 C2 1.522(3) . ?
C2 C10 1.528(3) . ?
C2 C3 1.537(3) . ?
C2 H2A 1.0000 . ?
C3 C8 1.381(4) . ?
C3 C4 1.381(4) . ?
C4 C5 1.401(4) . ?
C4 H4A 0.9500 . ?
C5 C6 1.376(4) . ?
C5 H5A 0.9500 . ?
C6 C7 1.373(4) . ?
C6 H6A 0.9500 . ?
C7 C8 1.383(4) . ?
C7 H7A 0.9500 . ?
C8 H8A 0.9500 . ?
C9 C10 1.528(3) . ?
C10 C11 1.528(3) . ?
C10 H10A 1.0000 . ?
C11 C12 1.378(4) . ?
C11 C16 1.390(4) . ?
C12 C13 1.385(4) . ?
C12 H12A 0.9500 . ?
C13 C14 1.380(4) . ?
C13 H13A 0.9500 . ?
C14 C15 1.367(4) . ?
C14 H14A 0.9500 . ?
C15 C16 1.394(4) . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9500 . ?
C17 C18 1.517(4) . ?
C18 C19 1.516(4) . ?
C18 C26 1.543(4) . ?
C18 H18A 1.0000 . ?
C19 C24 1.386(4) . ?
C19 C20 1.389(4) . ?
C20 C21 1.392(4) . ?
C20 H20A 0.9500 . ?
C21 C22 1.384(5) . ?
C21 H21A 0.9500 . ?
C22 C23 1.374(5) . ?
C22 H22A 0.9500 . ?
C23 C24 1.387(4) . ?
C23 H23A 0.9500 . ?
C24 H24A 0.9500 . ?
C25 C26 1.512(4) . ?
C26 C27 1.525(4) . ?
C26 H26A 1.0000 . ?
C27 C28 1.384(4) . ?
C27 C32 1.384(4) . ?
C28 C29 1.382(5) . ?
C28 H28A 0.9500 . ?
C29 C30 1.370(5) . ?
C29 H29A 0.9500 . ?
C30 C31 1.363(5) . ?
C30 H30A 0.9500 . ?
C31 C32 1.394(4) . ?
C31 H31A 0.9500 . ?
C32 H32A 0.9500 . ?
O1E C1E 1.428(3) . ?
O1E C3E 1.430(4) . ?
C1E C2E 1.488(5) . ?
C1E H1EA 0.9900 . ?
C1E H1EB 0.9900 . ?
C2E H2EA 0.9800 . ?
C2E H2EB 0.9800 . ?
C2E H2EC 0.9800 . ?
C3E C4E 1.483(5) . ?
C3E H3EA 0.9900 . ?
C3E H3EB 0.9900 . ?
C4E H4EA 0.9800 . ?
C4E H4EB 0.9800 . ?
C4E H4EC 0.9800 . ?
O2E C7E' 1.353(8) . ?
O2E C7E 1.441(10) . ?
O2E C5E 1.422(5) . ?
C5E C6E 1.443(6) . ?
C5E H5EA 0.9900 . ?
C5E H5EB 0.9900 . ?
C6E H6EA 0.9800 . ?
C6E H6EB 0.9800 . ?
C6E H6EC 0.9800 . ?
C7E C8E 1.488(19) . ?
C7E H7EA 0.9900 . ?
C7E H7EB 0.9900 . ?
C8E H8EA 0.9800 . ?
C8E H8EB 0.9800 . ?
C8E H8EC 0.9800 . ?
C7E' C8E' 1.415(13) . ?
C7E' H7E1 0.9900 . ?
C7E' H7E2 0.9900 . ?
C8E' H8E1 0.9800 . ?
C8E' H8E2 0.9800 . ?
C8E' H8E3 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
C1 O2 H2O 105(2) . . ?
C9 O4 H4O 109(2) . . ?
C17 O6 H6O 105(2) . . ?
C25 O7 H7O 107(2) . . ?
O1 C1 O2 123.4(2) . . ?
O1 C1 C2 123.8(2) . . ?
O2 C1 C2 112.7(2) . . ?
C1 C2 C10 111.8(2) . . ?
C1 C2 C3 108.0(2) . . ?
C10 C2 C3 111.8(2) . . ?
C1 C2 H2A 108.4 . . ?
C10 C2 H2A 108.4 . . ?
C3 C2 H2A 108.4 . . ?
C8 C3 C4 119.2(2) . . ?
C8 C3 C2 119.5(2) . . ?
C4 C3 C2 121.3(2) . . ?
C3 C4 C5 120.1(3) . . ?
C3 C4 H4A 119.9 . . ?
C5 C4 H4A 119.9 . . ?
C6 C5 C4 119.8(3) . . ?
C6 C5 H5A 120.1 . . ?
C4 C5 H5A 120.1 . . ?
C7 C6 C5 119.9(3) . . ?
C7 C6 H6A 120.0 . . ?
C5 C6 H6A 120.0 . . ?
C6 C7 C8 120.4(3) . . ?
C6 C7 H7A 119.8 . . ?
C8 C7 H7A 119.8 . . ?
C3 C8 C7 120.5(3) . . ?
C3 C8 H8A 119.8 . . ?
C7 C8 H8A 119.8 . . ?
O3 C9 O4 124.4(2) . . ?
O3 C9 C10 122.5(2) . . ?
O4 C9 C10 113.2(2) . . ?
C2 C10 C11 113.5(2) . . ?
C2 C10 C9 114.1(2) . . ?
C11 C10 C9 106.8(2) . . ?
C2 C10 H10A 107.4 . . ?
C11 C10 H10A 107.4 . . ?
C9 C10 H10A 107.4 . . ?
C12 C11 C16 118.3(2) . . ?
C12 C11 C10 118.7(2) . . ?
C16 C11 C10 122.9(2) . . ?
C11 C12 C13 120.9(3) . . ?
C11 C12 H12A 119.5 . . ?
C13 C12 H12A 119.5 . . ?
C14 C13 C12 120.6(3) . . ?
C14 C13 H13A 119.7 . . ?
C12 C13 H13A 119.7 . . ?
C15 C14 C13 119.1(3) . . ?
C15 C14 H14A 120.5 . . ?
C13 C14 H14A 120.5 . . ?
C14 C15 C16 120.7(3) . . ?
C14 C15 H15A 119.6 . . ?
C16 C15 H15A 119.6 . . ?
C11 C16 C15 120.4(3) . . ?
C11 C16 H16A 119.8 . . ?
C15 C16 H16A 119.8 . . ?
O5 C17 O6 123.7(2) . . ?
O5 C17 C18 124.5(2) . . ?
O6 C17 C18 111.7(2) . . ?
C19 C18 C17 109.0(2) . . ?
C19 C18 C26 111.3(2) . . ?
C17 C18 C26 110.8(2) . . ?
C19 C18 H18A 108.6 . . ?
C17 C18 H18A 108.6 . . ?
C26 C18 H18A 108.6 . . ?
C24 C19 C20 119.3(3) . . ?
C24 C19 C18 120.3(2) . . ?
C20 C19 C18 120.4(2) . . ?
C19 C20 C21 120.1(3) . . ?
C19 C20 H20A 119.9 . . ?
C21 C20 H20A 119.9 . . ?
C22 C21 C20 119.6(3) . . ?
C22 C21 H21A 120.2 . . ?
C20 C21 H21A 120.2 . . ?
C23 C22 C21 120.8(3) . . ?
C23 C22 H22A 119.6 . . ?
C21 C22 H22A 119.6 . . ?
C22 C23 C24 119.5(3) . . ?
C22 C23 H23A 120.3 . . ?
C24 C23 H23A 120.3 . . ?
C23 C24 C19 120.8(3) . . ?
C23 C24 H24A 119.6 . . ?
C19 C24 H24A 119.6 . . ?
O8 C25 O7 123.2(2) . . ?
O8 C25 C26 123.5(2) . . ?
O7 C25 C26 113.2(2) . . ?
C25 C26 C27 109.0(2) . . ?
C25 C26 C18 110.9(2) . . ?
C27 C26 C18 111.5(2) . . ?
C25 C26 H26A 108.4 . . ?
C27 C26 H26A 108.4 . . ?
C18 C26 H26A 108.4 . . ?
C28 C27 C32 118.5(3) . . ?
C28 C27 C26 120.3(3) . . ?
C32 C27 C26 121.2(3) . . ?
C27 C28 C29 121.0(3) . . ?
C27 C28 H28A 119.5 . . ?
C29 C28 H28A 119.5 . . ?
C30 C29 C28 119.9(4) . . ?
C30 C29 H29A 120.1 . . ?
C28 C29 H29A 120.1 . . ?
C31 C30 C29 120.2(3) . . ?
C31 C30 H30A 119.9 . . ?
C29 C30 H30A 119.9 . . ?
C30 C31 C32 120.3(3) . . ?
C30 C31 H31A 119.9 . . ?
C32 C31 H31A 119.9 . . ?
C27 C32 C31 120.2(3) . . ?
C27 C32 H32A 119.9 . . ?
C31 C32 H32A 119.9 . . ?
C1E O1E C3E 112.6(2) . . ?
O1E C1E C2E 109.2(3) . . ?
O1E C1E H1EA 109.8 . . ?
C2E C1E H1EA 109.8 . . ?
O1E C1E H1EB 109.8 . . ?
C2E C1E H1EB 109.8 . . ?
H1EA C1E H1EB 108.3 . . ?
C1E C2E H2EA 109.5 . . ?
C1E C2E H2EB 109.5 . . ?
H2EA C2E H2EB 109.5 . . ?
C1E C2E H2EC 109.5 . . ?
H2EA C2E H2EC 109.5 . . ?
H2EB C2E H2EC 109.5 . . ?
O1E C3E C4E 109.5(3) . . ?
O1E C3E H3EA 109.8 . . ?
C4E C3E H3EA 109.8 . . ?
O1E C3E H3EB 109.8 . . ?
C4E C3E H3EB 109.8 . . ?
H3EA C3E H3EB 108.2 . . ?
C3E C4E H4EA 109.5 . . ?
C3E C4E H4EB 109.5 . . ?
H4EA C4E H4EB 109.5 . . ?
C3E C4E H4EC 109.5 . . ?
H4EA C4E H4EC 109.5 . . ?
H4EB C4E H4EC 109.5 . . ?
C7E' O2E C7E 40.2(4) . . ?
C7E' O2E C5E 117.4(5) . . ?
C7E O2E C5E 117.4(5) . . ?
O2E C5E C6E 114.5(4) . . ?
O2E C5E H5EA 108.6 . . ?
C6E C5E H5EA 108.6 . . ?
O2E C5E H5EB 108.6 . . ?
C6E C5E H5EB 108.6 . . ?
H5EA C5E H5EB 107.6 . . ?
C5E C6E H6EA 109.5 . . ?
C5E C6E H6EB 109.5 . . ?
H6EA C6E H6EB 109.5 . . ?
C5E C6E H6EC 109.5 . . ?
H6EA C6E H6EC 109.5 . . ?
H6EB C6E H6EC 109.5 . . ?
O2E C7E C8E 122.0(13) . . ?
O2E C7E H7EA 106.8 . . ?
C8E C7E H7EA 106.8 . . ?
O2E C7E H7EB 106.8 . . ?
C8E C7E H7EB 106.8 . . ?
H7EA C7E H7EB 106.7 . . ?
C7E C8E H8EA 109.5 . . ?
C7E C8E H8EB 109.5 . . ?
H8EA C8E H8EB 109.5 . . ?
C7E C8E H8EC 109.5 . . ?
H8EA C8E H8EC 109.5 . . ?
H8EB C8E H8EC 109.5 . . ?
O2E C7E' C8E' 114.6(11) . . ?
O2E C7E' H7E1 108.6 . . ?
C8E' C7E' H7E1 108.6 . . ?
O2E C7E' H7E2 108.6 . . ?
C8E' C7E' H7E2 108.6 . . ?
H7E1 C7E' H7E2 107.6 . . ?
C7E' C8E' H8E1 109.5 . . ?
C7E' C8E' H8E2 109.5 . . ?
H8E1 C8E' H8E2 109.5 . . ?
C7E' C8E' H8E3 109.5 . . ?
H8E1 C8E' H8E3 109.5 . . ?
H8E2 C8E' H8E3 109.5 . . ?

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 C10 -28.7(4) . . . . ?
O2 C1 C2 C10 151.9(2) . . . . ?
O1 C1 C2 C3 94.7(3) . . . . ?
O2 C1 C2 C3 -84.7(3) . . . . ?
C1 C2 C3 C8 117.0(3) . . . . ?
C10 C2 C3 C8 -119.6(3) . . . . ?
C1 C2 C3 C4 -62.8(3) . . . . ?
C10 C2 C3 C4 60.6(3) . . . . ?
C8 C3 C4 C5 -2.7(4) . . . . ?
C2 C3 C4 C5 177.1(2) . . . . ?
C3 C4 C5 C6 1.4(4) . . . . ?
C4 C5 C6 C7 0.4(4) . . . . ?
C5 C6 C7 C8 -0.8(4) . . . . ?
C4 C3 C8 C7 2.3(4) . . . . ?
C2 C3 C8 C7 -177.5(2) . . . . ?
C6 C7 C8 C3 -0.6(4) . . . . ?
C1 C2 C10 C11 -169.7(2) . . . . ?
C3 C2 C10 C11 69.1(3) . . . . ?
C1 C2 C10 C9 -47.0(3) . . . . ?
C3 C2 C10 C9 -168.2(2) . . . . ?
O3 C9 C10 C2 152.9(2) . . . . ?
O4 C9 C10 C2 -28.0(3) . . . . ?
O3 C9 C10 C11 -80.9(3) . . . . ?
O4 C9 C10 C11 98.2(2) . . . . ?
C2 C10 C11 C12 -143.7(2) . . . . ?
C9 C10 C11 C12 89.7(3) . . . . ?
C2 C10 C11 C16 40.6(3) . . . . ?
C9 C10 C11 C16 -85.9(3) . . . . ?
C16 C11 C12 C13 0.8(4) . . . . ?
C10 C11 C12 C13 -175.0(2) . . . . ?
C11 C12 C13 C14 -1.2(4) . . . . ?
C12 C13 C14 C15 0.3(4) . . . . ?
C13 C14 C15 C16 1.0(4) . . . . ?
C12 C11 C16 C15 0.5(4) . . . . ?
C10 C11 C16 C15 176.2(2) . . . . ?
C14 C15 C16 C11 -1.5(4) . . . . ?
O5 C17 C18 C19 106.2(3) . . . . ?
O6 C17 C18 C19 -72.0(3) . . . . ?
O5 C17 C18 C26 -16.6(4) . . . . ?
O6 C17 C18 C26 165.2(2) . . . . ?
C17 C18 C19 C24 125.7(3) . . . . ?
C26 C18 C19 C24 -111.8(3) . . . . ?
C17 C18 C19 C20 -55.8(3) . . . . ?
C26 C18 C19 C20 66.7(3) . . . . ?
C24 C19 C20 C21 -0.5(4) . . . . ?
C18 C19 C20 C21 -179.0(3) . . . . ?
C19 C20 C21 C22 0.9(5) . . . . ?
C20 C21 C22 C23 -0.4(5) . . . . ?
C21 C22 C23 C24 -0.5(5) . . . . ?
C22 C23 C24 C19 0.8(4) . . . . ?
C20 C19 C24 C23 -0.3(4) . . . . ?
C18 C19 C24 C23 178.2(2) . . . . ?
O8 C25 C26 C27 93.1(3) . . . . ?
O7 C25 C26 C27 -83.6(3) . . . . ?
O8 C25 C26 C18 -30.1(3) . . . . ?
O7 C25 C26 C18 153.2(2) . . . . ?
C19 C18 C26 C25 175.3(2) . . . . ?
C17 C18 C26 C25 -63.3(3) . . . . ?
C19 C18 C26 C27 53.6(3) . . . . ?
C17 C18 C26 C27 175.0(2) . . . . ?
C25 C26 C27 C28 126.7(3) . . . . ?
C18 C26 C27 C28 -110.5(3) . . . . ?
C25 C26 C27 C32 -55.9(3) . . . . ?
C18 C26 C27 C32 66.9(3) . . . . ?
C32 C27 C28 C29 -0.9(5) . . . . ?
C26 C27 C28 C29 176.6(3) . . . . ?
C27 C28 C29 C30 1.0(6) . . . . ?
C28 C29 C30 C31 0.1(6) . . . . ?
C29 C30 C31 C32 -1.3(6) . . . . ?
C28 C27 C32 C31 -0.3(5) . . . . ?
C26 C27 C32 C31 -177.8(3) . . . . ?
C30 C31 C32 C27 1.4(5) . . . . ?
C3E O1E C1E C2E 175.7(2) . . . . ?
C1E O1E C3E C4E 167.4(3) . . . . ?
C7E' O2E C5E C6E 136.1(7) . . . . ?
C7E O2E C5E C6E 90.5(8) . . . . ?
C7E' O2E C7E C8E -49.4(14) . . . . ?
C5E O2E C7E C8E 51.5(18) . . . . ?
C7E O2E C7E' C8E' 28.1(14) . . . . ?
C5E O2E C7E' C8E' -72.8(17) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2O O1 0.86(3) 1.83(3) 2.675(3) 168(3) 2_766
O4 H4O O1E 0.83(3) 1.88(3) 2.690(3) 166(3) .
O6 H6O O2E 0.85(3) 1.87(4) 2.679(3) 157(3) 1_565
O7 H7O O8 0.86(3) 1.81(3) 2.660(3) 165(3) 2_565

_diffrn_measured_fraction_theta_max 0.966
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.966
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.047

data_xtal2
_database_code_depnum_ccdc_archive 'CCDC 706644'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H22 O5'
_chemical_formula_weight         342.38

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                   9.1569(7)
_cell_length_b                   10.3223(9)
_cell_length_c                   11.0400(9)
_cell_angle_alpha                69.8170(10)
_cell_angle_beta                 74.207(2)
_cell_angle_gamma                64.6770(10)
_cell_volume                     875.72(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2083
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      24.7

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             364
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_correction_T_min  
;
Ratio of minimum to maximum apparent transmission: 0.680779
;
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(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  'Bruker SMART CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            3840
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0739
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.99
_diffrn_reflns_theta_max         24.71
_reflns_number_total             2753
_reflns_number_gt                1643
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruekr XP'
_computing_publication_material  'Bruker XCIF'

_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)+(0.1575P)²+2.5193P] 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         2753
_refine_ls_number_parameters     234
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1637
_refine_ls_R_factor_gt           0.0897
_refine_ls_wR_factor_ref         0.3200
_refine_ls_wR_factor_gt          0.2391
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.004
_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 0.1191(6) 1.0141(4) 0.5997(4) 0.0393(11) Uani 1 1 d . . .
O2 O 0.1715(5) 0.8553(4) 0.4832(4) 0.0394(11) Uani 1 1 d . . .
O3 O 0.5018(6) 0.9300(4) 0.3549(4) 0.0414(11) Uani 1 1 d . . .
O4 O 0.5922(6) 0.7121(5) 0.3072(4) 0.0406(12) Uani 1 1 d . . .
H1O H 0.010(17) 1.062(14) 0.564(12) 0.14(5) Uiso 1 1 d . . .
H2O H 0.623(8) 0.766(7) 0.231(7) 0.042(18) Uiso 1 1 d . . .
C1 C 0.2098(6) 0.8961(6) 0.5565(5) 0.0279(13) Uani 1 1 d . . .
C2 C 0.3692(7) 0.8117(6) 0.6118(5) 0.0302(13) Uani 1 1 d . . .
H2A H 0.4124 0.8849 0.6141 0.036 Uiso 1 1 calc R . .
C3 C 0.4971(7) 0.7101(6) 0.5284(5) 0.0294(13) Uani 1 1 d . . .
H3A H 0.4552 0.6350 0.5286 0.035 Uiso 1 1 calc R . .
C4 C 0.5275(7) 0.7988(6) 0.3880(5) 0.0296(13) Uani 1 1 d . . .
C5 C 0.3341(7) 0.7222(6) 0.7515(5) 0.0298(14) Uani 1 1 d . . .
C6 C 0.2621(8) 0.6187(7) 0.7739(6) 0.0404(16) Uani 1 1 d . . .
H6A H 0.2388 0.6030 0.7025 0.049 Uiso 1 1 calc R . .
C7 C 0.2248(9) 0.5390(7) 0.9005(6) 0.053(2) Uani 1 1 d . . .
H7A H 0.1754 0.4693 0.9164 0.063 Uiso 1 1 calc R . .
C8 C 0.2608(10) 0.5627(8) 1.0033(6) 0.057(2) Uani 1 1 d . . .
H8A H 0.2376 0.5073 1.0899 0.069 Uiso 1 1 calc R . .
C9 C 0.3292(10) 0.6647(8) 0.9819(6) 0.057(2) Uani 1 1 d . . .
H9A H 0.3533 0.6804 1.0529 0.068 Uiso 1 1 calc R . .
C10 C 0.3628(8) 0.7449(7) 0.8553(6) 0.0426(16) Uani 1 1 d . . .
H10A H 0.4073 0.8178 0.8408 0.051 Uiso 1 1 calc R . .
C11 C 0.6601(7) 0.6279(6) 0.5820(5) 0.0297(14) Uani 1 1 d . . .
C12 C 0.7457(9) 0.7049(7) 0.5925(5) 0.0419(17) Uani 1 1 d . . .
H12A H 0.7008 0.8104 0.5693 0.050 Uiso 1 1 calc R . .
C13 C 0.8971(8) 0.6305(7) 0.6364(5) 0.0407(16) Uani 1 1 d . . .
H13A H 0.9546 0.6850 0.6430 0.049 Uiso 1 1 calc R . .
C14 C 0.9629(8) 0.4775(7) 0.6700(5) 0.0434(17) Uani 1 1 d . . .
H14A H 1.0668 0.4264 0.6986 0.052 Uiso 1 1 calc R . .
C15 C 0.8784(8) 0.3987(7) 0.6622(5) 0.0420(17) Uani 1 1 d . . .
H15A H 0.9235 0.2932 0.6862 0.050 Uiso 1 1 calc R . .
C16 C 0.7268(8) 0.4733(6) 0.6192(5) 0.0363(15) Uani 1 1 d . . .
H16A H 0.6683 0.4182 0.6152 0.044 Uiso 1 1 calc R . .
O1S O 0.7087(7) 0.8364(6) 0.0656(4) 0.0619(16) Uani 1 1 d . . .
C17 C 0.8403(10) 0.8794(9) 0.0559(6) 0.0527(19) Uani 1 1 d . . .
H17A H 0.9375 0.7912 0.0841 0.063 Uiso 1 1 calc R . .
H17B H 0.8096 0.9473 0.1114 0.063 Uiso 1 1 calc R . .
C18 C 0.8755(13) 0.9565(10) -0.0850(7) 0.075(3) Uani 1 1 d . . .
H18A H 0.8281 1.0657 -0.0993 0.090 Uiso 1 1 calc R . .
H18B H 0.9946 0.9252 -0.1153 0.090 Uiso 1 1 calc R . .
C19 C 0.6810(11) 0.8557(9) -0.0620(6) 0.059(2) Uani 1 1 d . . .
H19A H 0.5693 0.9275 -0.0766 0.071 Uiso 1 1 calc R . .
H19B H 0.6948 0.7600 -0.0735 0.071 Uiso 1 1 calc R . .
C20 C 0.8002(19) 0.911(2) -0.1503(9) 0.174(8) Uani 1 1 d . . .
H20A H 0.8841 0.8326 -0.1910 0.209 Uiso 1 1 calc R . .
H20B H 0.7471 0.9964 -0.2205 0.209 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 C1 1.312(7) . ?
O1 H1O 1.03(14) . ?
O2 C1 1.213(7) . ?
O3 C4 1.207(6) . ?
O4 C4 1.325(6) . ?
O4 H2O 0.88(7) . ?
C1 C2 1.514(8) . ?
C2 C5 1.528(7) . ?
C2 C3 1.533(7) . ?
C2 H2A 1.0000 . ?
C3 C4 1.523(7) . ?
C3 C11 1.533(8) . ?
C3 H3A 1.0000 . ?
C5 C10 1.357(9) . ?
C5 C6 1.403(9) . ?
C6 C7 1.391(8) . ?
C6 H6A 0.9500 . ?
C7 C8 1.385(11) . ?
C7 H7A 0.9500 . ?
C8 C9 1.367(11) . ?
C8 H8A 0.9500 . ?
C9 C10 1.385(9) . ?
C9 H9A 0.9500 . ?
C10 H10A 0.9500 . ?
C11 C12 1.381(9) . ?
C11 C16 1.392(8) . ?
C12 C13 1.394(10) . ?
C12 H12A 0.9500 . ?
C13 C14 1.378(9) . ?
C13 H13A 0.9500 . ?
C14 C15 1.375(10) . ?
C14 H14A 0.9500 . ?
C15 C16 1.391(9) . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9500 . ?
O1S C17 1.420(9) . ?
O1S C19 1.431(8) . ?
C17 C18 1.500(10) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C20 1.412(15) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.427(13) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 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
C1 O1 H1O 108(7) . . ?
C4 O4 H2O 107(4) . . ?
O2 C1 O1 125.0(5) . . ?
O2 C1 C2 122.9(5) . . ?
O1 C1 C2 112.1(5) . . ?
C1 C2 C5 108.1(4) . . ?
C1 C2 C3 111.6(5) . . ?
C5 C2 C3 111.0(4) . . ?
C1 C2 H2A 108.7 . . ?
C5 C2 H2A 108.7 . . ?
C3 C2 H2A 108.7 . . ?
C4 C3 C11 108.4(4) . . ?
C4 C3 C2 110.9(4) . . ?
C11 C3 C2 111.7(5) . . ?
C4 C3 H3A 108.6 . . ?
C11 C3 H3A 108.6 . . ?
C2 C3 H3A 108.6 . . ?
O3 C4 O4 124.1(5) . . ?
O3 C4 C3 124.5(5) . . ?
O4 C4 C3 111.3(5) . . ?
C10 C5 C6 118.8(5) . . ?
C10 C5 C2 122.0(6) . . ?
C6 C5 C2 119.1(5) . . ?
C7 C6 C5 120.1(6) . . ?
C7 C6 H6A 120.0 . . ?
C5 C6 H6A 120.0 . . ?
C8 C7 C6 119.1(7) . . ?
C8 C7 H7A 120.4 . . ?
C6 C7 H7A 120.4 . . ?
C9 C8 C7 121.0(6) . . ?
C9 C8 H8A 119.5 . . ?
C7 C8 H8A 119.5 . . ?
C8 C9 C10 119.1(7) . . ?
C8 C9 H9A 120.4 . . ?
C10 C9 H9A 120.4 . . ?
C5 C10 C9 121.9(7) . . ?
C5 C10 H10A 119.1 . . ?
C9 C10 H10A 119.1 . . ?
C12 C11 C16 118.4(6) . . ?
C12 C11 C3 121.0(5) . . ?
C16 C11 C3 120.6(6) . . ?
C11 C12 C13 121.1(6) . . ?
C11 C12 H12A 119.5 . . ?
C13 C12 H12A 119.5 . . ?
C14 C13 C12 119.7(7) . . ?
C14 C13 H13A 120.1 . . ?
C12 C13 H13A 120.1 . . ?
C15 C14 C13 120.1(6) . . ?
C15 C14 H14A 120.0 . . ?
C13 C14 H14A 120.0 . . ?
C14 C15 C16 120.1(6) . . ?
C14 C15 H15A 120.0 . . ?
C16 C15 H15A 120.0 . . ?
C15 C16 C11 120.6(6) . . ?
C15 C16 H16A 119.7 . . ?
C11 C16 H16A 119.7 . . ?
C17 O1S C19 109.8(5) . . ?
O1S C17 C18 106.2(7) . . ?
O1S C17 H17A 110.5 . . ?
C18 C17 H17A 110.5 . . ?
O1S C17 H17B 110.5 . . ?
C18 C17 H17B 110.5 . . ?
H17A C17 H17B 108.7 . . ?
C20 C18 C17 103.9(8) . . ?
C20 C18 H18A 111.0 . . ?
C17 C18 H18A 111.0 . . ?
C20 C18 H18B 111.0 . . ?
C17 C18 H18B 111.0 . . ?
H18A C18 H18B 109.0 . . ?
O1S C19 C20 105.5(8) . . ?
O1S C19 H19A 110.6 . . ?
C20 C19 H19A 110.6 . . ?
O1S C19 H19B 110.6 . . ?
C20 C19 H19B 110.6 . . ?
H19A C19 H19B 108.8 . . ?
C18 C20 C19 111.0(8) . . ?
C18 C20 H20A 109.4 . . ?
C19 C20 H20A 109.4 . . ?
C18 C20 H20B 109.4 . . ?
C19 C20 H20B 109.4 . . ?
H20A C20 H20B 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
O2 C1 C2 C5 -100.8(6) . . . . ?
O1 C1 C2 C5 77.7(6) . . . . ?
O2 C1 C2 C3 21.5(7) . . . . ?
O1 C1 C2 C3 -160.0(4) . . . . ?
C1 C2 C3 C4 57.3(6) . . . . ?
C5 C2 C3 C4 178.0(5) . . . . ?
C1 C2 C3 C11 178.4(4) . . . . ?
C5 C2 C3 C11 -61.0(6) . . . . ?
C11 C3 C4 O3 -99.5(7) . . . . ?
C2 C3 C4 O3 23.5(9) . . . . ?
C11 C3 C4 O4 78.0(6) . . . . ?
C2 C3 C4 O4 -159.1(5) . . . . ?
C1 C2 C5 C10 -118.6(6) . . . . ?
C3 C2 C5 C10 118.7(6) . . . . ?
C1 C2 C5 C6 58.0(6) . . . . ?
C3 C2 C5 C6 -64.6(7) . . . . ?
C10 C5 C6 C7 -1.4(9) . . . . ?
C2 C5 C6 C7 -178.2(6) . . . . ?
C5 C6 C7 C8 -0.5(10) . . . . ?
C6 C7 C8 C9 1.2(11) . . . . ?
C7 C8 C9 C10 -0.1(11) . . . . ?
C6 C5 C10 C9 2.6(9) . . . . ?
C2 C5 C10 C9 179.3(6) . . . . ?
C8 C9 C10 C5 -1.9(10) . . . . ?
C4 C3 C11 C12 62.1(6) . . . . ?
C2 C3 C11 C12 -60.4(6) . . . . ?
C4 C3 C11 C16 -116.8(5) . . . . ?
C2 C3 C11 C16 120.7(5) . . . . ?
C16 C11 C12 C13 1.4(8) . . . . ?
C3 C11 C12 C13 -177.4(5) . . . . ?
C11 C12 C13 C14 0.0(8) . . . . ?
C12 C13 C14 C15 -1.0(8) . . . . ?
C13 C14 C15 C16 0.6(8) . . . . ?
C14 C15 C16 C11 0.9(8) . . . . ?
C12 C11 C16 C15 -1.9(7) . . . . ?
C3 C11 C16 C15 177.0(5) . . . . ?
C19 O1S C17 C18 11.0(8) . . . . ?
O1S C17 C18 C20 -18.0(12) . . . . ?
C17 O1S C19 C20 0.3(11) . . . . ?
C17 C18 C20 C19 19.0(16) . . . . ?
O1S C19 C20 C18 -12.6(16) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1O O2 1.03(14) 1.65(14) 2.672(7) 175(11) 2_576
O4 H2O O1S 0.88(7) 1.81(7) 2.675(6) 167(6) .

_diffrn_measured_fraction_theta_max 0.924
_diffrn_reflns_theta_full        24.71
_diffrn_measured_fraction_theta_full 0.924
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.101

data_xtal3
_database_code_depnum_ccdc_archive 'CCDC 706645'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H22 O5'
_chemical_formula_weight         342.38

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           orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   9.5545(2)
_cell_length_b                   10.2040(2)
_cell_length_c                   36.9589(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3603.28(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    4476
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      25.19

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1456
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_correction_T_min  
;
Ratio of minimum to maximum apparent transmission: 0.806287
;
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298(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  'Bruker APEX CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20167
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0763
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_theta_min         1.10
_diffrn_reflns_theta_max         28.30
_reflns_number_total             8397
_reflns_number_gt                5799
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  'Bruker XCIF'

_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)+(0.0713P)²+0.0100P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.5(10)
_refine_ls_number_reflns         8397
_refine_ls_number_parameters     467
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0578
_refine_ls_wR_factor_ref         0.1459
_refine_ls_wR_factor_gt          0.1219
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.001
_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 0.2500(3) 0.0512(3) 0.89192(7) 0.0243(6) Uani 1 1 d . . .
C2 C 0.2251(3) 0.0431(3) 0.93251(7) 0.0264(6) Uani 1 1 d . . .
H2A H 0.1300 0.0098 0.9363 0.032 Uiso 1 1 calc R . .
C3 C 0.3268(3) -0.0580(3) 0.94762(7) 0.0272(6) Uani 1 1 d . . .
C4 C 0.4661(3) -0.0271(3) 0.95388(8) 0.0376(7) Uani 1 1 d . . .
H4A H 0.4978 0.0577 0.9496 0.045 Uiso 1 1 calc R . .
C5 C 0.5582(4) -0.1214(3) 0.96646(9) 0.0423(8) Uani 1 1 d . . .
H5A H 0.6514 -0.0998 0.9706 0.051 Uiso 1 1 calc R . .
C6 C 0.5119(4) -0.2478(3) 0.97295(8) 0.0411(8) Uani 1 1 d . . .
H6A H 0.5738 -0.3111 0.9814 0.049 Uiso 1 1 calc R . .
C7 C 0.3735(4) -0.2795(3) 0.96683(7) 0.0365(8) Uani 1 1 d . . .
H7A H 0.3418 -0.3642 0.9713 0.044 Uiso 1 1 calc R . .
C8 C 0.2820(3) -0.1854(3) 0.95405(7) 0.0321(7) Uani 1 1 d . . .
H8A H 0.1892 -0.2077 0.9497 0.039 Uiso 1 1 calc R . .
C9 C 0.1421(3) 0.2776(3) 0.93430(7) 0.0309(7) Uani 1 1 d . . .
C10 C 0.2362(3) 0.1763(3) 0.95177(7) 0.0253(6) Uani 1 1 d . . .
H10A H 0.3331 0.2068 0.9499 0.030 Uiso 1 1 calc R . .
C11 C 0.1979(3) 0.1665(3) 0.99203(7) 0.0261(6) Uani 1 1 d . . .
C12 C 0.0852(3) 0.0973(3) 1.00436(8) 0.0351(7) Uani 1 1 d . . .
H12A H 0.0324 0.0487 0.9880 0.042 Uiso 1 1 calc R . .
C13 C 0.0478(4) 0.0978(3) 1.04053(8) 0.0381(8) Uani 1 1 d . . .
H13A H -0.0300 0.0507 1.0482 0.046 Uiso 1 1 calc R . .
C14 C 0.1241(4) 0.1668(4) 1.06490(8) 0.0464(9) Uani 1 1 d . . .
H14A H 0.1000 0.1655 1.0893 0.056 Uiso 1 1 calc R . .
C15 C 0.2377(4) 0.2389(6) 1.05326(9) 0.0808(16) Uani 1 1 d . . .
H15A H 0.2894 0.2881 1.0697 0.097 Uiso 1 1 calc R . .
C16 C 0.2747(4) 0.2378(5) 1.01688(9) 0.0698(13) Uani 1 1 d . . .
H16A H 0.3520 0.2855 1.0092 0.084 Uiso 1 1 calc R . .
C17 C 0.3056(3) 0.0480(2) 0.78971(6) 0.0210(5) Uani 1 1 d . . .
C18 C 0.3234(3) 0.0456(2) 0.74915(6) 0.0202(5) Uani 1 1 d . . .
H18A H 0.3470 -0.0443 0.7421 0.024 Uiso 1 1 calc R . .
C19 C 0.1829(3) 0.0786(2) 0.73249(6) 0.0220(6) Uani 1 1 d . . .
C20 C 0.1016(3) -0.0216(3) 0.71762(7) 0.0258(6) Uani 1 1 d . . .
H20A H 0.1379 -0.1060 0.7162 0.031 Uiso 1 1 calc R . .
C21 C -0.0329(3) 0.0027(3) 0.70483(7) 0.0311(7) Uani 1 1 d . . .
H21A H -0.0861 -0.0655 0.6953 0.037 Uiso 1 1 calc R . .
C22 C -0.0875(3) 0.1281(3) 0.70620(7) 0.0313(7) Uani 1 1 d . . .
H22A H -0.1772 0.1449 0.6976 0.038 Uiso 1 1 calc R . .
C23 C -0.0074(3) 0.2281(3) 0.72046(7) 0.0310(7) Uani 1 1 d . . .
H23A H -0.0434 0.3128 0.7214 0.037 Uiso 1 1 calc R . .
C24 C 0.1264(3) 0.2036(3) 0.73346(7) 0.0277(6) Uani 1 1 d . . .
H24A H 0.1790 0.2722 0.7430 0.033 Uiso 1 1 calc R . .
C25 C 0.5717(3) 0.1077(2) 0.76049(6) 0.0221(6) Uani 1 1 d . . .
C26 C 0.4447(3) 0.1350(2) 0.73701(6) 0.0202(5) Uani 1 1 d . . .
H26A H 0.4166 0.2266 0.7403 0.024 Uiso 1 1 calc R . .
C27 C 0.4879(3) 0.1146(2) 0.69767(6) 0.0210(6) Uani 1 1 d . . .
C28 C 0.5293(3) -0.0087(3) 0.68530(7) 0.0278(6) Uani 1 1 d . . .
H28A H 0.5229 -0.0810 0.7005 0.033 Uiso 1 1 calc R . .
C29 C 0.5801(3) -0.0240(3) 0.65020(7) 0.0331(7) Uani 1 1 d . . .
H29A H 0.6087 -0.1061 0.6422 0.040 Uiso 1 1 calc R . .
C30 C 0.5882(3) 0.0829(3) 0.62737(7) 0.0349(7) Uani 1 1 d . . .
H30A H 0.6229 0.0728 0.6040 0.042 Uiso 1 1 calc R . .
C31 C 0.5445(3) 0.2051(3) 0.63920(7) 0.0333(7) Uani 1 1 d . . .
H31A H 0.5480 0.2767 0.6236 0.040 Uiso 1 1 calc R . .
C32 C 0.8859(4) 0.6136(4) 0.93896(9) 0.0549(10) Uani 1 1 d . . .
H32A H 0.8904 0.6803 0.9576 0.066 Uiso 1 1 calc R . .
H32B H 0.8502 0.5334 0.9496 0.066 Uiso 1 1 calc R . .
C33 C 0.7936(4) 0.6576(4) 0.90845(8) 0.0504(9) Uani 1 1 d . . .
H33A H 0.7934 0.7523 0.9064 0.060 Uiso 1 1 calc R . .
H33B H 0.6983 0.6272 0.9118 0.060 Uiso 1 1 calc R . .
C34 C 0.8596(3) 0.5950(3) 0.87574(8) 0.0424(8) Uani 1 1 d . . .
H34A H 0.8299 0.5046 0.8730 0.051 Uiso 1 1 calc R . .
H34B H 0.8376 0.6431 0.8538 0.051 Uiso 1 1 calc R . .
C35 C 1.0122(4) 0.6038(4) 0.88467(8) 0.0444(8) Uani 1 1 d . . .
H35A H 1.0637 0.5336 0.8730 0.053 Uiso 1 1 calc R . .
H35B H 1.0504 0.6870 0.8767 0.053 Uiso 1 1 calc R . .
O1 O 0.3258(2) 0.14002(19) 0.87906(5) 0.0355(5) Uani 1 1 d . . .
O2 O 0.1939(2) -0.0399(2) 0.87363(5) 0.0343(5) Uani 1 1 d . . .
O3 O 0.1753(2) 0.3977(2) 0.94518(6) 0.0406(6) Uani 1 1 d . . .
O4 O 0.0501(2) 0.2531(2) 0.91313(6) 0.0413(5) Uani 1 1 d . . .
O5 O 0.3424(2) 0.15075(18) 0.80706(5) 0.0334(5) Uani 1 1 d . . .
O6 O 0.2522(2) -0.05077(17) 0.80473(5) 0.0284(4) Uani 1 1 d . . .
O7 O 0.6489(2) 0.21290(17) 0.76601(5) 0.0271(4) Uani 1 1 d . . .
O8 O 0.5994(2) 0.00032(17) 0.77246(5) 0.0319(5) Uani 1 1 d . . .
O9 O 1.0213(2) 0.59213(19) 0.92355(5) 0.0347(5) Uani 1 1 d . . .
O10 O 0.8345(2) 0.17584(18) 0.81618(5) 0.0351(5) Uani 1 1 d . . .
C39 C 0.7615(5) 0.1783(4) 0.85004(9) 0.0614(11) Uani 1 1 d . . .
H39A H 0.6657 0.2068 0.8465 0.074 Uiso 1 1 calc R . .
H39B H 0.8068 0.2385 0.8666 0.074 Uiso 1 1 calc R . .
C37 C 0.8496(4) -0.0345(4) 0.84139(10) 0.0585(11) Uani 1 1 d . . .
H37A H 0.7927 -0.0990 0.8289 0.070 Uiso 1 1 calc R . .
H37B H 0.9208 -0.0796 0.8554 0.070 Uiso 1 1 calc R . .
C36 C 0.9146(4) 0.0580(4) 0.81519(10) 0.0538(10) Uani 1 1 d . . .
H36A H 1.0109 0.0755 0.8219 0.065 Uiso 1 1 calc R . .
H36B H 0.9134 0.0209 0.7910 0.065 Uiso 1 1 calc R . .
C38 C 0.7641(9) 0.0473(5) 0.86454(14) 0.150(3) Uani 1 1 d . . .
H38A H 0.6697 0.0125 0.8657 0.181 Uiso 1 1 calc R . .
H38B H 0.8024 0.0483 0.8888 0.181 Uiso 1 1 calc R . .
C40 C 0.4954(3) 0.2208(3) 0.67436(7) 0.0265(6) Uani 1 1 d . . .
H40A H 0.4675 0.3032 0.6823 0.032 Uiso 1 1 calc R . .
H1O H 0.118(4) 0.458(4) 0.9377(9) 0.059(12) Uiso 1 1 d . . .
H2O H 0.325(6) 0.149(6) 0.8387(17) 0.16(2) Uiso 1 1 d . . .
H3O H 0.230(6) -0.039(6) 0.8467(16) 0.17(2) Uiso 1 1 d . . .
H4O H 0.719(5) 0.188(4) 0.7819(11) 0.082(14) Uiso 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 1.254(3) . ?
C1 O2 1.269(3) . ?
C1 C2 1.521(3) . ?
C2 C3 1.523(4) . ?
C2 C10 1.538(4) . ?
C2 H2A 0.9800 . ?
C3 C4 1.387(4) . ?
C3 C8 1.389(4) . ?
C4 C5 1.385(4) . ?
C4 H4A 0.9300 . ?
C5 C6 1.384(5) . ?
C5 H5A 0.9300 . ?
C6 C7 1.380(5) . ?
C6 H6A 0.9300 . ?
C7 C8 1.382(4) . ?
C7 H7A 0.9300 . ?
C8 H8A 0.9300 . ?
C9 O4 1.203(3) . ?
C9 O3 1.328(4) . ?
C9 C10 1.515(4) . ?
C10 C11 1.535(4) . ?
C10 H10A 0.9800 . ?
C11 C12 1.366(4) . ?
C11 C16 1.382(4) . ?
C12 C13 1.384(4) . ?
C12 H12A 0.9300 . ?
C13 C14 1.355(5) . ?
C13 H13A 0.9300 . ?
C14 C15 1.381(5) . ?
C14 H14A 0.9300 . ?
C15 C16 1.390(5) . ?
C15 H15A 0.9300 . ?
C16 H16A 0.9300 . ?
C17 O6 1.258(3) . ?
C17 O5 1.278(3) . ?
C17 C18 1.509(3) . ?
C18 C19 1.515(4) . ?
C18 C26 1.541(3) . ?
C18 H18A 0.9800 . ?
C19 C24 1.386(4) . ?
C19 C20 1.397(3) . ?
C20 C21 1.391(4) . ?
C20 H20A 0.9300 . ?
C21 C22 1.383(4) . ?
C21 H21A 0.9300 . ?
C22 C23 1.380(4) . ?
C22 H22A 0.9300 . ?
C23 C24 1.389(4) . ?
C23 H23A 0.9300 . ?
C24 H24A 0.9300 . ?
C25 O8 1.211(3) . ?
C25 O7 1.318(3) . ?
C25 C26 1.518(3) . ?
C26 C27 1.526(3) . ?
C26 H26A 0.9800 . ?
C27 C40 1.386(3) . ?
C27 C28 1.396(4) . ?
C28 C29 1.394(3) . ?
C28 H28A 0.9300 . ?
C29 C30 1.381(4) . ?
C29 H29A 0.9300 . ?
C30 C31 1.386(4) . ?
C30 H30A 0.9300 . ?
C31 C40 1.391(4) . ?
C31 H31A 0.9300 . ?
C32 O9 1.431(4) . ?
C32 C33 1.500(5) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C34 1.506(4) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.498(5) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 O9 1.445(3) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
O2 H3O 1.05(6) . ?
O3 H1O 0.87(4) . ?
O5 H2O 1.18(6) . ?
O7 H4O 0.93(4) . ?
O10 C36 1.426(4) . ?
O10 C39 1.433(4) . ?
C39 C38 1.440(6) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C37 C38 1.448(6) . ?
C37 C36 1.488(5) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C40 H40A 0.9300 . ?

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 124.9(2) . . ?
O1 C1 C2 120.2(2) . . ?
O2 C1 C2 114.8(2) . . ?
C1 C2 C3 107.4(2) . . ?
C1 C2 C10 113.4(2) . . ?
C3 C2 C10 112.6(2) . . ?
C1 C2 H2A 107.7 . . ?
C3 C2 H2A 107.7 . . ?
C10 C2 H2A 107.7 . . ?
C4 C3 C8 118.6(3) . . ?
C4 C3 C2 121.3(2) . . ?
C8 C3 C2 120.0(3) . . ?
C5 C4 C3 120.5(3) . . ?
C5 C4 H4A 119.7 . . ?
C3 C4 H4A 119.7 . . ?
C6 C5 C4 120.2(3) . . ?
C6 C5 H5A 119.9 . . ?
C4 C5 H5A 119.9 . . ?
C7 C6 C5 119.8(3) . . ?
C7 C6 H6A 120.1 . . ?
C5 C6 H6A 120.1 . . ?
C6 C7 C8 119.9(3) . . ?
C6 C7 H7A 120.0 . . ?
C8 C7 H7A 120.0 . . ?
C7 C8 C3 121.0(3) . . ?
C7 C8 H8A 119.5 . . ?
C3 C8 H8A 119.5 . . ?
O4 C9 O3 124.3(3) . . ?
O4 C9 C10 124.7(3) . . ?
O3 C9 C10 111.1(2) . . ?
C9 C10 C11 108.4(2) . . ?
C9 C10 C2 111.4(2) . . ?
C11 C10 C2 112.0(2) . . ?
C9 C10 H10A 108.3 . . ?
C11 C10 H10A 108.3 . . ?
C2 C10 H10A 108.3 . . ?
C12 C11 C16 117.9(3) . . ?
C12 C11 C10 123.0(3) . . ?
C16 C11 C10 118.9(3) . . ?
C11 C12 C13 121.6(3) . . ?
C11 C12 H12A 119.2 . . ?
C13 C12 H12A 119.2 . . ?
C14 C13 C12 120.3(3) . . ?
C14 C13 H13A 119.8 . . ?
C12 C13 H13A 119.8 . . ?
C13 C14 C15 119.5(3) . . ?
C13 C14 H14A 120.2 . . ?
C15 C14 H14A 120.2 . . ?
C14 C15 C16 119.8(4) . . ?
C14 C15 H15A 120.1 . . ?
C16 C15 H15A 120.1 . . ?
C11 C16 C15 120.8(4) . . ?
C11 C16 H16A 119.6 . . ?
C15 C16 H16A 119.6 . . ?
O6 C17 O5 123.1(2) . . ?
O6 C17 C18 118.1(2) . . ?
O5 C17 C18 118.7(2) . . ?
C17 C18 C19 107.5(2) . . ?
C17 C18 C26 111.4(2) . . ?
C19 C18 C26 114.62(19) . . ?
C17 C18 H18A 107.7 . . ?
C19 C18 H18A 107.7 . . ?
C26 C18 H18A 107.7 . . ?
C24 C19 C20 117.9(2) . . ?
C24 C19 C18 122.6(2) . . ?
C20 C19 C18 119.4(2) . . ?
C21 C20 C19 121.1(3) . . ?
C21 C20 H20A 119.4 . . ?
C19 C20 H20A 119.4 . . ?
C22 C21 C20 120.1(3) . . ?
C22 C21 H21A 120.0 . . ?
C20 C21 H21A 120.0 . . ?
C23 C22 C21 119.3(3) . . ?
C23 C22 H22A 120.4 . . ?
C21 C22 H22A 120.4 . . ?
C22 C23 C24 120.6(3) . . ?
C22 C23 H23A 119.7 . . ?
C24 C23 H23A 119.7 . . ?
C19 C24 C23 121.0(3) . . ?
C19 C24 H24A 119.5 . . ?
C23 C24 H24A 119.5 . . ?
O8 C25 O7 124.0(2) . . ?
O8 C25 C26 123.3(2) . . ?
O7 C25 C26 112.7(2) . . ?
C25 C26 C27 107.6(2) . . ?
C25 C26 C18 109.02(19) . . ?
C27 C26 C18 113.57(19) . . ?
C25 C26 H26A 108.8 . . ?
C27 C26 H26A 108.8 . . ?
C18 C26 H26A 108.8 . . ?
C40 C27 C28 119.1(2) . . ?
C40 C27 C26 120.0(2) . . ?
C28 C27 C26 120.8(2) . . ?
C29 C28 C27 120.3(2) . . ?
C29 C28 H28A 119.9 . . ?
C27 C28 H28A 119.9 . . ?
C30 C29 C28 120.0(3) . . ?
C30 C29 H29A 120.0 . . ?
C28 C29 H29A 120.0 . . ?
C29 C30 C31 120.1(2) . . ?
C29 C30 H30A 120.0 . . ?
C31 C30 H30A 120.0 . . ?
C30 C31 C40 120.0(3) . . ?
C30 C31 H31A 120.0 . . ?
C40 C31 H31A 120.0 . . ?
O9 C32 C33 106.1(3) . . ?
O9 C32 H32A 110.5 . . ?
C33 C32 H32A 110.5 . . ?
O9 C32 H32B 110.5 . . ?
C33 C32 H32B 110.5 . . ?
H32A C32 H32B 108.7 . . ?
C32 C33 C34 103.3(3) . . ?
C32 C33 H33A 111.1 . . ?
C34 C33 H33A 111.1 . . ?
C32 C33 H33B 111.1 . . ?
C34 C33 H33B 111.1 . . ?
H33A C33 H33B 109.1 . . ?
C35 C34 C33 101.9(3) . . ?
C35 C34 H34A 111.4 . . ?
C33 C34 H34A 111.4 . . ?
C35 C34 H34B 111.4 . . ?
C33 C34 H34B 111.4 . . ?
H34A C34 H34B 109.3 . . ?
O9 C35 C34 105.8(2) . . ?
O9 C35 H35A 110.6 . . ?
C34 C35 H35A 110.6 . . ?
O9 C35 H35B 110.6 . . ?
C34 C35 H35B 110.6 . . ?
H35A C35 H35B 108.7 . . ?
C1 O2 H3O 111(3) . . ?
C9 O3 H1O 114(2) . . ?
C17 O5 H2O 116(3) . . ?
C25 O7 H4O 106(3) . . ?
C32 O9 C35 109.2(2) . . ?
C36 O10 C39 107.3(2) . . ?
O10 C39 C38 107.5(3) . . ?
O10 C39 H39A 110.2 . . ?
C38 C39 H39A 110.2 . . ?
O10 C39 H39B 110.2 . . ?
C38 C39 H39B 110.2 . . ?
H39A C39 H39B 108.5 . . ?
C38 C37 C36 104.8(3) . . ?
C38 C37 H37A 110.8 . . ?
C36 C37 H37A 110.8 . . ?
C38 C37 H37B 110.8 . . ?
C36 C37 H37B 110.8 . . ?
H37A C37 H37B 108.9 . . ?
O10 C36 C37 107.1(3) . . ?
O10 C36 H36A 110.3 . . ?
C37 C36 H36A 110.3 . . ?
O10 C36 H36B 110.3 . . ?
C37 C36 H36B 110.3 . . ?
H36A C36 H36B 108.5 . . ?
C39 C38 C37 108.9(3) . . ?
C39 C38 H38A 109.9 . . ?
C37 C38 H38A 109.9 . . ?
C39 C38 H38B 109.9 . . ?
C37 C38 H38B 109.9 . . ?
H38A C38 H38B 108.3 . . ?
C27 C40 C31 120.6(3) . . ?
C27 C40 H40A 119.7 . . ?
C31 C40 H40A 119.7 . . ?

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 -97.7(3) . . . . ?
O2 C1 C2 C3 79.6(3) . . . . ?
O1 C1 C2 C10 27.4(4) . . . . ?
O2 C1 C2 C10 -155.3(2) . . . . ?
C1 C2 C3 C4 79.2(3) . . . . ?
C10 C2 C3 C4 -46.4(3) . . . . ?
C1 C2 C3 C8 -98.2(3) . . . . ?
C10 C2 C3 C8 136.2(2) . . . . ?
C8 C3 C4 C5 -0.4(4) . . . . ?
C2 C3 C4 C5 -177.8(3) . . . . ?
C3 C4 C5 C6 -0.1(5) . . . . ?
C4 C5 C6 C7 0.0(5) . . . . ?
C5 C6 C7 C8 0.4(4) . . . . ?
C6 C7 C8 C3 -0.8(4) . . . . ?
C4 C3 C8 C7 0.8(4) . . . . ?
C2 C3 C8 C7 178.2(2) . . . . ?
O4 C9 C10 C11 -109.7(3) . . . . ?
O3 C9 C10 C11 70.9(3) . . . . ?
O4 C9 C10 C2 14.0(4) . . . . ?
O3 C9 C10 C2 -165.4(2) . . . . ?
C1 C2 C10 C9 53.4(3) . . . . ?
C3 C2 C10 C9 175.6(2) . . . . ?
C1 C2 C10 C11 175.0(2) . . . . ?
C3 C2 C10 C11 -62.8(3) . . . . ?
C9 C10 C11 C12 79.6(3) . . . . ?
C2 C10 C11 C12 -43.8(4) . . . . ?
C9 C10 C11 C16 -96.0(4) . . . . ?
C2 C10 C11 C16 140.7(3) . . . . ?
C16 C11 C12 C13 0.1(5) . . . . ?
C10 C11 C12 C13 -175.4(3) . . . . ?
C11 C12 C13 C14 -0.7(5) . . . . ?
C12 C13 C14 C15 1.4(5) . . . . ?
C13 C14 C15 C16 -1.5(7) . . . . ?
C12 C11 C16 C15 -0.2(6) . . . . ?
C10 C11 C16 C15 175.6(4) . . . . ?
C14 C15 C16 C11 0.9(7) . . . . ?
O6 C17 C18 C19 80.2(3) . . . . ?
O5 C17 C18 C19 -98.3(3) . . . . ?
O6 C17 C18 C26 -153.5(2) . . . . ?
O5 C17 C18 C26 28.0(3) . . . . ?
C17 C18 C19 C24 72.2(3) . . . . ?
C26 C18 C19 C24 -52.2(3) . . . . ?
C17 C18 C19 C20 -103.4(3) . . . . ?
C26 C18 C19 C20 132.2(2) . . . . ?
C24 C19 C20 C21 -1.2(4) . . . . ?
C18 C19 C20 C21 174.5(2) . . . . ?
C19 C20 C21 C22 1.0(4) . . . . ?
C20 C21 C22 C23 -0.2(4) . . . . ?
C21 C22 C23 C24 -0.2(4) . . . . ?
C20 C19 C24 C23 0.8(4) . . . . ?
C18 C19 C24 C23 -174.9(2) . . . . ?
C22 C23 C24 C19 -0.1(4) . . . . ?
O8 C25 C26 C27 -89.9(3) . . . . ?
O7 C25 C26 C27 89.4(2) . . . . ?
O8 C25 C26 C18 33.7(3) . . . . ?
O7 C25 C26 C18 -147.0(2) . . . . ?
C17 C18 C26 C25 47.6(3) . . . . ?
C19 C18 C26 C25 169.9(2) . . . . ?
C17 C18 C26 C27 167.6(2) . . . . ?
C19 C18 C26 C27 -70.1(3) . . . . ?
C25 C26 C27 C40 -111.7(3) . . . . ?
C18 C26 C27 C40 127.5(3) . . . . ?
C25 C26 C27 C28 63.9(3) . . . . ?
C18 C26 C27 C28 -56.9(3) . . . . ?
C40 C27 C28 C29 1.3(4) . . . . ?
C26 C27 C28 C29 -174.4(3) . . . . ?
C27 C28 C29 C30 -0.8(4) . . . . ?
C28 C29 C30 C31 -0.6(5) . . . . ?
C29 C30 C31 C40 1.4(5) . . . . ?
O9 C32 C33 C34 27.7(4) . . . . ?
C32 C33 C34 C35 -36.3(4) . . . . ?
C33 C34 C35 O9 32.4(4) . . . . ?
C33 C32 O9 C35 -7.5(4) . . . . ?
C34 C35 O9 C32 -15.9(4) . . . . ?
C36 O10 C39 C38 -16.7(5) . . . . ?
C39 O10 C36 C37 21.6(4) . . . . ?
C38 C37 C36 O10 -18.0(5) . . . . ?
O10 C39 C38 C37 5.2(7) . . . . ?
C36 C37 C38 C39 7.7(7) . . . . ?
C28 C27 C40 C31 -0.5(4) . . . . ?
C26 C27 C40 C31 175.3(3) . . . . ?
C30 C31 C40 C27 -0.9(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O5 H2O O1 1.18(6) 1.49(6) 2.668(3) 171(5) .
O2 H3O O6 1.05(6) 1.57(6) 2.609(2) 167(6) .
O7 H4O O10 0.93(4) 1.69(4) 2.593(3) 166(4) .

_diffrn_measured_fraction_theta_max 0.957
_diffrn_reflns_theta_full        28.30
_diffrn_measured_fraction_theta_full 0.957
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.065

# Attachment 'xtal4.cif'

data_xtal4
_database_code_depnum_ccdc_archive 'CCDC 706646'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C68 H66 O17'
_chemical_formula_weight         1155.21

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           tetragonal
_symmetry_space_group_name_H-M   P4(1)

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x, z+1/4'
'y, -x, z+3/4'

_cell_length_a                   16.249(6)
_cell_length_b                   16.249(6)
_cell_length_c                   22.540(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5951(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2440
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_correction_T_min  
;
Ratio of minimum to maximum apparent transmission: 0.767208
;
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(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  'Bruker APEX CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19315
_diffrn_reflns_av_R_equivalents  0.1032
_diffrn_reflns_av_sigmaI/netI    0.1040
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.25
_diffrn_reflns_theta_max         20.81
_reflns_number_total             5945
_reflns_number_gt                3069
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  'Bruker XCIF'

_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.

Due to the weak intensities, anisotropic thermal parameters of many carbon
atoms were non-positive definite or unreasonable ellipsoids. Therefore,
a soft restraint of ISOR instruction was applied to all the carbons atoms.
As the number of carbons atoms in the asymmetric unit were 68, total number
of restraints were 408 (=68 x 8 thermal parameters per atom). The remaining
ones are related to both geometry restraints for hydrogen atoms, and
disordered ether molecule.
;

_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)+(0.1453P)²+29.8751P] 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     SHELXL
_refine_ls_extinction_coef       0.0005(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   
;
chirality based on the configuration at the chiral center of the molecule:1(4)
;
_refine_ls_number_reflns         5945
_refine_ls_number_parameters     673
_refine_ls_number_restraints     498
_refine_ls_R_factor_all          0.1952
_refine_ls_R_factor_gt           0.1143
_refine_ls_wR_factor_ref         0.3441
_refine_ls_wR_factor_gt          0.2863
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.048
_refine_ls_shift/su_mean         0.003

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 0.4874(6) 0.7578(7) -0.0268(5) 0.042(3) Uani 1 1 d D . .
H1 H 0.5325 0.7824 -0.0196 0.051 Uiso 1 1 calc RD . .
O2 O 0.4704(6) 0.7786(6) 0.0699(5) 0.041(3) Uani 1 1 d D . .
O3 O 0.3028(6) 0.8790(5) -0.0043(5) 0.027(3) Uani 1 1 d D . .
O4 O 0.2819(6) 0.8882(6) 0.0940(5) 0.041(3) Uani 1 1 d D . .
H4 H 0.2888 0.9393 0.0876 0.049 Uiso 1 1 calc RD . .
C1 C 0.4452(9) 0.7516(8) 0.0217(7) 0.026(4) Uani 1 1 d DU . .
C2 C 0.3596(8) 0.7129(8) 0.0140(7) 0.028(4) Uani 1 1 d U . .
H2A H 0.3426 0.7199 -0.0283 0.033 Uiso 1 1 calc R . .
C3 C 0.3688(7) 0.6255(4) 0.0256(5) 0.029(4) Uani 1 1 d GU . .
C4 C 0.3778(8) 0.6022(6) 0.0831(4) 0.075(6) Uani 1 1 d GU . .
H4A H 0.3715 0.6412 0.1142 0.090 Uiso 1 1 calc R . .
C5 C 0.3968(9) 0.5186(7) 0.0964(5) 0.101(8) Uani 1 1 d GU . .
H5A H 0.4088 0.5000 0.1354 0.121 Uiso 1 1 calc R . .
C6 C 0.3963(8) 0.4607(4) 0.0419(6) 0.065(5) Uani 1 1 d GU . .
H6A H 0.3981 0.4031 0.0492 0.078 Uiso 1 1 calc R . .
C7 C 0.3938(7) 0.4837(5) -0.0106(6) 0.066(6) Uani 1 1 d GU . .
H7A H 0.4055 0.4483 -0.0430 0.079 Uiso 1 1 calc R . .
C8 C 0.3728(6) 0.5637(6) -0.0173(4) 0.040(4) Uani 1 1 d GU . .
H8A H 0.3589 0.5799 -0.0565 0.048 Uiso 1 1 calc R . .
C9 C 0.2946(8) 0.8473(8) 0.0452(7) 0.022(4) Uani 1 1 d DU . .
C10 C 0.2956(8) 0.7547(7) 0.0531(7) 0.021(3) Uani 1 1 d U . .
H10A H 0.3111 0.7434 0.0952 0.025 Uiso 1 1 calc R . .
C11 C 0.2075(4) 0.7235(5) 0.0446(4) 0.023(3) Uani 1 1 d GU . .
C12 C 0.1553(6) 0.7038(5) 0.0897(3) 0.035(4) Uani 1 1 d GU . .
H12A H 0.1769 0.7021 0.1289 0.042 Uiso 1 1 calc R . .
C13 C 0.0747(6) 0.6865(5) 0.0823(4) 0.038(4) Uani 1 1 d GU . .
H13A H 0.0399 0.6809 0.1159 0.046 Uiso 1 1 calc R . .
C14 C 0.0448(4) 0.6777(5) 0.0297(5) 0.031(4) Uani 1 1 d GU . .
H14A H -0.0112 0.6618 0.0254 0.037 Uiso 1 1 calc R . .
C15 C 0.0949(6) 0.6914(6) -0.0237(4) 0.053(5) Uani 1 1 d GU . .
H15A H 0.0730 0.6835 -0.0623 0.064 Uiso 1 1 calc R . .
C16 C 0.1741(5) 0.7161(6) -0.0152(4) 0.034(4) Uani 1 1 d GU . .
H16A H 0.2079 0.7284 -0.0484 0.041 Uiso 1 1 calc R . .
O5 O 0.6284(6) 0.7904(6) 0.0938(5) 0.038(3) Uani 1 1 d D . .
H5 H 0.5779 0.7829 0.0854 0.045 Uiso 1 1 calc RD . .
O6 O 0.6397(6) 0.8129(6) -0.0050(5) 0.031(3) Uani 1 1 d D . .
O7 O 0.7440(6) 0.9783(6) 0.0700(5) 0.037(3) Uani 1 1 d D . .
O8 O 0.7613(6) 0.9985(6) -0.0260(5) 0.039(3) Uani 1 1 d D . .
H8 H 0.7322 1.0407 -0.0185 0.047 Uiso 1 1 calc RD . .
C17 C 0.6702(8) 0.8048(7) 0.0443(7) 0.019(2) Uani 1 1 d DU . .
C18 C 0.7599(8) 0.8082(7) 0.0528(6) 0.015(3) Uani 1 1 d U . .
H18A H 0.7704 0.8235 0.0951 0.018 Uiso 1 1 calc R . .
C19 C 0.7939(6) 0.7184(4) 0.0431(5) 0.028(4) Uani 1 1 d GU . .
C20 C 0.8027(6) 0.6830(5) -0.0146(4) 0.038(4) Uani 1 1 d GU . .
H20A H 0.7922 0.7168 -0.0481 0.046 Uiso 1 1 calc R . .
C21 C 0.8253(6) 0.6031(5) -0.0241(4) 0.039(4) Uani 1 1 d GU . .
H21A H 0.8307 0.5826 -0.0634 0.046 Uiso 1 1 calc R . .
C22 C 0.8397(6) 0.5535(4) 0.0227(5) 0.037(4) Uani 1 1 d GU . .
H22A H 0.8512 0.4967 0.0172 0.044 Uiso 1 1 calc R . .
C23 C 0.8375(7) 0.5869(6) 0.0779(4) 0.054(5) Uani 1 1 d GU . .
H23A H 0.8546 0.5536 0.1103 0.065 Uiso 1 1 calc R . .
C24 C 0.8117(7) 0.6669(6) 0.0901(4) 0.051(5) Uani 1 1 d GU . .
H24A H 0.8064 0.6856 0.1299 0.062 Uiso 1 1 calc R . .
C25 C 0.7658(8) 0.9502(8) 0.0231(7) 0.019(2) Uani 1 1 d DU . .
C26 C 0.8050(8) 0.8704(8) 0.0137(7) 0.029(4) Uani 1 1 d U . .
H26A H 0.7949 0.8544 -0.0285 0.035 Uiso 1 1 calc R . .
C27 C 0.8923(5) 0.8806(6) 0.0208(5) 0.029(4) Uani 1 1 d GU . .
C28 C 0.9509(7) 0.8762(6) -0.0199(4) 0.059(5) Uani 1 1 d GU . .
H28A H 0.9370 0.8629 -0.0597 0.071 Uiso 1 1 calc R . .
C29 C 1.0353(6) 0.8914(7) -0.0045(5) 0.046(5) Uani 1 1 d GU . .
H29A H 1.0754 0.8848 -0.0349 0.055 Uiso 1 1 calc R . .
C30 C 1.0609(5) 0.9131(6) 0.0468(6) 0.060(5) Uani 1 1 d GU . .
H30A H 1.1169 0.9277 0.0533 0.072 Uiso 1 1 calc R . .
C31 C 1.0058(8) 0.9146(7) 0.0914(5) 0.075(6) Uani 1 1 d GU . .
H31A H 1.0259 0.9249 0.1303 0.091 Uiso 1 1 calc R . .
C32 C 0.9227(7) 0.9022(7) 0.0847(4) 0.070(6) Uani 1 1 d GU . .
H32A H 0.8857 0.9066 0.1172 0.084 Uiso 1 1 calc R . .
O9 O 0.7256(6) 0.1349(6) 0.0929(4) 0.032(3) Uani 1 1 d D . .
H9 H 0.7449 0.0880 0.0837 0.038 Uiso 1 1 calc RD . .
O10 O 0.7081(7) 0.1498(6) -0.0050(5) 0.040(3) Uani 1 1 d D . .
O11 O 0.5424(6) 0.2521(7) 0.0706(6) 0.048(3) Uani 1 1 d D . .
O12 O 0.5211(6) 0.2718(7) -0.0259(5) 0.044(3) Uani 1 1 d D . .
H12 H 0.4720 0.2584 -0.0172 0.053 Uiso 1 1 calc RD . .
C33 C 0.7154(8) 0.1794(8) 0.0443(7) 0.025(4) Uani 1 1 d DU . .
C34 C 0.7128(8) 0.2732(7) 0.0547(7) 0.021(3) Uani 1 1 d U . .
H34A H 0.6979 0.2856 0.0968 0.025 Uiso 1 1 calc R . .
C35 C 0.8002(4) 0.3016(5) 0.0414(4) 0.022(3) Uani 1 1 d GU . .
C36 C 0.8313(5) 0.3045(6) -0.0117(4) 0.032(4) Uani 1 1 d GU . .
H36A H 0.7974 0.2887 -0.0442 0.038 Uiso 1 1 calc R . .
C37 C 0.9120(6) 0.3296(6) -0.0237(4) 0.045(4) Uani 1 1 d GU . .
H37A H 0.9303 0.3335 -0.0636 0.054 Uiso 1 1 calc R . .
C38 C 0.9623(4) 0.3476(6) 0.0191(5) 0.044(4) Uani 1 1 d GU . .
H38A H 1.0183 0.3604 0.0115 0.053 Uiso 1 1 calc R . .
C39 C 0.9295(5) 0.3473(6) 0.0790(4) 0.051(5) Uani 1 1 d GU . .
H39A H 0.9638 0.3647 0.1107 0.061 Uiso 1 1 calc R . .
C40 C 0.8506(6) 0.3228(5) 0.0911(3) 0.032(4) Uani 1 1 d GU . .
H40A H 0.8304 0.3199 0.1306 0.038 Uiso 1 1 calc R . .
C41 C 0.5654(8) 0.2744(9) 0.0226(7) 0.027(4) Uani 1 1 d DU . .
C42 C 0.6489(8) 0.3117(7) 0.0117(7) 0.024(4) Uani 1 1 d U . .
H42A H 0.6662 0.3030 -0.0304 0.028 Uiso 1 1 calc R . .
C43 C 0.6375(7) 0.4065(4) 0.0250(5) 0.030(4) Uani 1 1 d GU . .
C44 C 0.6368(7) 0.4583(6) -0.0225(4) 0.052(5) Uani 1 1 d GU . .
H44A H 0.6436 0.4400 -0.0623 0.062 Uiso 1 1 calc R . .
C45 C 0.6250(7) 0.5423(5) -0.0071(5) 0.054(5) Uani 1 1 d GU . .
H45A H 0.6286 0.5817 -0.0382 0.064 Uiso 1 1 calc R . .
C46 C 0.6086(8) 0.5724(5) 0.0504(6) 0.065(6) Uani 1 1 d GU . .
H46A H 0.5933 0.6282 0.0566 0.079 Uiso 1 1 calc R . .
C47 C 0.6148(8) 0.5220(7) 0.0941(5) 0.077(6) Uani 1 1 d GU . .
H47A H 0.6087 0.5398 0.1339 0.092 Uiso 1 1 calc R . .
C48 C 0.6308(8) 0.4417(6) 0.0805(4) 0.052(5) Uani 1 1 d GU . .
H48A H 0.6381 0.4057 0.1133 0.062 Uiso 1 1 calc R . .
O13 O 0.2466(7) 0.0303(6) -0.0261(5) 0.046(3) Uani 1 1 d D . .
H13 H 0.2581 -0.0195 -0.0180 0.055 Uiso 1 1 calc RD . .
O14 O 0.2696(6) 0.0489(6) 0.0707(5) 0.036(3) Uani 1 1 d D . .
O15 O 0.3702(7) 0.2171(7) -0.0041(6) 0.050(3) Uani 1 1 d D . .
O16 O 0.3808(6) 0.2364(6) 0.0918(5) 0.040(3) Uani 1 1 d D . .
H16 H 0.4315 0.2288 0.0843 0.048 Uiso 1 1 calc RD . .
C49 C 0.2456(9) 0.0735(9) 0.0225(8) 0.035(4) Uani 1 1 d DU . .
C50 C 0.2044(8) 0.1591(8) 0.0139(7) 0.026(4) Uani 1 1 d U . .
H50A H 0.2097 0.1768 -0.0285 0.031 Uiso 1 1 calc R . .
C51 C 0.1118(5) 0.1515(6) 0.0307(5) 0.034(4) Uani 1 1 d GU . .
C52 C 0.0824(7) 0.1442(6) 0.0824(4) 0.043(4) Uani 1 1 d GU . .
H52A H 0.1182 0.1446 0.1158 0.051 Uiso 1 1 calc R . .
C53 C 0.0032(7) 0.1362(6) 0.0903(4) 0.064(5) Uani 1 1 d GU . .
H53A H -0.0133 0.1407 0.1306 0.076 Uiso 1 1 calc R . .
C54 C -0.0535(5) 0.1242(7) 0.0563(6) 0.060(5) Uani 1 1 d GU . .
H54A H -0.1086 0.1160 0.0690 0.072 Uiso 1 1 calc R . .
C55 C -0.0275(6) 0.1235(7) -0.0090(5) 0.066(5) Uani 1 1 d GU . .
H55A H -0.0660 0.1131 -0.0398 0.080 Uiso 1 1 calc R . .
C56 C 0.0592(6) 0.1394(7) -0.0217(4) 0.042(4) Uani 1 1 d GU . .
H56A H 0.0802 0.1419 -0.0610 0.050 Uiso 1 1 calc R . .
C57 C 0.3365(9) 0.2244(8) 0.0421(8) 0.029(4) Uani 1 1 d DU . .
C58 C 0.2449(8) 0.2236(7) 0.0549(7) 0.021(4) Uani 1 1 d U . .
H58A H 0.2348 0.2091 0.0975 0.026 Uiso 1 1 calc R . .
C59 C 0.2125(6) 0.3099(4) 0.0420(4) 0.026(4) Uani 1 1 d GU . .
C60 C 0.1966(6) 0.3623(5) 0.0908(4) 0.035(4) Uani 1 1 d GU . .
H60A H 0.2043 0.3412 0.1298 0.042 Uiso 1 1 calc R . .
C61 C 0.1701(7) 0.4434(5) 0.0845(4) 0.045(4) Uani 1 1 d GU . .
H61A H 0.1542 0.4759 0.1177 0.054 Uiso 1 1 calc R . .
C62 C 0.1682(6) 0.4746(4) 0.0259(5) 0.048(5) Uani 1 1 d GU . .
H62A H 0.1554 0.5309 0.0192 0.058 Uiso 1 1 calc R . .
C63 C 0.1856(6) 0.4216(6) -0.0235(4) 0.042(4) Uani 1 1 d GU . .
H63A H 0.1811 0.4412 -0.0630 0.050 Uiso 1 1 calc R . .
C64 C 0.2092(6) 0.3409(5) -0.0121(4) 0.039(4) Uani 1 1 d GU . .
H64A H 0.2236 0.3066 -0.0446 0.046 Uiso 1 1 calc R . .
O1G O 0.5290(18) 0.027(2) 0.0234(19) 0.31(2) Uani 1 1 d D . .
C1G C 0.524(2) 0.003(2) -0.0648(17) 0.184(17) Uani 1 1 d DU . .
H1GA H 0.4996 0.0074 -0.1044 0.221 Uiso 1 1 calc R . .
H1GB H 0.5306 -0.0548 -0.0541 0.221 Uiso 1 1 calc R . .
H1GC H 0.5781 0.0302 -0.0648 0.221 Uiso 1 1 calc R . .
C2G C 0.471(2) 0.044(2) -0.0218(15) 0.22(2) Uani 1 1 d DU . .
H2GA H 0.4624 0.1029 -0.0296 0.269 Uiso 1 1 calc R . .
H2GB H 0.4175 0.0152 -0.0159 0.269 Uiso 1 1 calc R . .
C3G C 0.496(3) -0.001(3) 0.0765(14) 0.188(18) Uani 1 1 d DU . .
H3GA H 0.5174 -0.0583 0.0763 0.225 Uiso 1 1 calc R . .
H3GB H 0.4376 -0.0069 0.0651 0.225 Uiso 1 1 calc R . .
C4G C 0.4876(19) 0.012(2) 0.1409(14) 0.160(13) Uani 1 1 d DU . .
H4GA H 0.4923 -0.0403 0.1617 0.192 Uiso 1 1 calc R . .
H4GB H 0.4336 0.0369 0.1491 0.192 Uiso 1 1 calc R . .
H4GC H 0.5310 0.0497 0.1545 0.192 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 C1 1.293(16) . ?
O1 H1 0.8501 . ?
O2 C1 1.241(16) . ?
O3 C9 1.237(16) . ?
O4 C9 1.301(16) . ?
O4 H4 0.8501 . ?
C1 C2 1.536(19) . ?
C2 C3 1.451(15) . ?
C2 C10 1.523(19) . ?
C2 H2A 1.0000 . ?
C3 C4 1.3597 . ?
C3 C8 1.3955 . ?
C4 C5 1.4248 . ?
C4 H4A 0.9500 . ?
C5 C6 1.5475 . ?
C5 H5A 0.9500 . ?
C6 C7 1.2413 . ?
C6 H6A 0.9500 . ?
C7 C8 1.3525 . ?
C7 H7A 0.9500 . ?
C8 H8A 0.9500 . ?
C9 C10 1.516(18) . ?
C10 C11 1.530(13) . ?
C10 H10A 1.0000 . ?
C11 C12 1.3639 . ?
C11 C16 1.4567 . ?
C12 C13 1.3496 . ?
C12 H12A 0.9500 . ?
C13 C14 1.2879 . ?
C13 H13A 0.9500 . ?
C14 C15 1.4700 . ?
C14 H14A 0.9500 . ?
C15 C16 1.3622 . ?
C15 H15A 0.9500 . ?
C16 H16A 0.9500 . ?
O5 C17 1.327(16) . ?
O5 H5 0.8501 . ?
O6 C17 1.223(15) . ?
O7 C25 1.206(15) . ?
O8 C25 1.359(16) . ?
O8 H8 0.8501 . ?
C17 C18 1.471(18) . ?
C18 C26 1.528(18) . ?
C18 C19 1.575(13) . ?
C18 H18A 1.0000 . ?
C19 C24 1.3814 . ?
C19 C20 1.4285 . ?
C20 C21 1.3664 . ?
C20 H20A 0.9500 . ?
C21 C22 1.3465 . ?
C21 H21A 0.9500 . ?
C22 C23 1.3593 . ?
C22 H22A 0.9500 . ?
C23 C24 1.3923 . ?
C23 H23A 0.9500 . ?
C24 H24A 0.9500 . ?
C25 C26 1.461(19) . ?
C26 C27 1.437(15) . ?
C26 H26A 1.0000 . ?
C27 C28 1.3241 . ?
C27 C32 1.5636 . ?
C28 C29 1.4368 . ?
C28 H28A 0.9500 . ?
C29 C30 1.2795 . ?
C29 H29A 0.9500 . ?
C30 C31 1.3467 . ?
C30 H30A 0.9500 . ?
C31 C32 1.3734 . ?
C31 H31A 0.9500 . ?
C32 H32A 0.9500 . ?
O9 C33 1.324(16) . ?
O9 H9 0.8501 . ?
O10 C33 1.217(16) . ?
O11 C41 1.202(16) . ?
O12 C41 1.308(16) . ?
O12 H12 0.8501 . ?
C33 C34 1.542(17) . ?
C34 C35 1.524(14) . ?
C34 C42 1.551(18) . ?
C34 H34A 1.0000 . ?
C35 C36 1.3017 . ?
C35 C40 1.4284 . ?
C36 C37 1.4004 . ?
C36 H36A 0.9500 . ?
C37 C38 1.2972 . ?
C37 H37A 0.9500 . ?
C38 C39 1.4502 . ?
C38 H38A 0.9500 . ?
C39 C40 1.3708 . ?
C39 H39A 0.9500 . ?
C40 H40A 0.9500 . ?
C41 C42 1.507(19) . ?
C42 C43 1.581(14) . ?
C42 H42A 1.0000 . ?
C43 C44 1.3615 . ?
C43 C48 1.3808 . ?
C44 C45 1.4224 . ?
C44 H44A 0.9500 . ?
C45 C46 1.4091 . ?
C45 H45A 0.9500 . ?
C46 C47 1.2845 . ?
C46 H46A 0.9500 . ?
C47 C48 1.3640 . ?
C47 H47A 0.9500 . ?
C48 H48A 0.9500 . ?
O13 C49 1.302(17) . ?
O13 H13 0.8501 . ?
O14 C49 1.220(17) . ?
O15 C57 1.182(16) . ?
O16 C57 1.346(17) . ?
O16 H16 0.8501 . ?
C49 C50 1.56(2) . ?
C50 C58 1.546(18) . ?
C50 C51 1.555(15) . ?
C50 H50A 1.0000 . ?
C51 C52 1.2663 . ?
C51 C56 1.4705 . ?
C52 C53 1.3047 . ?
C52 H52A 0.9500 . ?
C53 C54 1.2138 . ?
C53 H53A 0.9500 . ?
C54 C55 1.5312 . ?
C54 H54A 0.9500 . ?
C55 C56 1.4608 . ?
C55 H55A 0.9500 . ?
C56 H56A 0.9500 . ?
C57 C58 1.516(19) . ?
C58 C59 1.525(14) . ?
C58 H58A 1.0000 . ?
C59 C64 1.3193 . ?
C59 C60 1.4168 . ?
C60 C61 1.3935 . ?
C60 H60A 0.9500 . ?
C61 C62 1.4163 . ?
C61 H61A 0.9500 . ?
C62 C63 1.4350 . ?
C62 H62A 0.9500 . ?
C63 C64 1.3891 . ?
C63 H63A 0.9500 . ?
C64 H64A 0.9500 . ?
O1G C3G 1.390(19) . ?
O1G C2G 1.415(19) . ?
C1G C2G 1.456(19) . ?
C1G H1GA 0.9800 . ?
C1G H1GB 0.9800 . ?
C1G H1GC 0.9800 . ?
C2G H2GA 0.9900 . ?
C2G H2GB 0.9900 . ?
C3G C4G 1.474(19) . ?
C3G H3GA 0.9900 . ?
C3G H3GB 0.9900 . ?
C4G H4GA 0.9800 . ?
C4G H4GB 0.9800 . ?
C4G H4GC 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
C1 O1 H1 109.5 . . ?
C9 O4 H4 109.5 . . ?
O2 C1 O1 122.5(12) . . ?
O2 C1 C2 122.8(13) . . ?
O1 C1 C2 114.7(13) . . ?
C3 C2 C10 113.8(11) . . ?
C3 C2 C1 106.7(11) . . ?
C10 C2 C1 111.8(11) . . ?
C3 C2 H2A 108.1 . . ?
C10 C2 H2A 108.1 . . ?
C1 C2 H2A 108.1 . . ?
C4 C3 C8 117.1 . . ?
C4 C3 C2 117.0(9) . . ?
C8 C3 C2 125.8(9) . . ?
C3 C4 C5 119.3 . . ?
C3 C4 H4A 120.3 . . ?
C5 C4 H4A 120.3 . . ?
C4 C5 C6 114.3 . . ?
C4 C5 H5A 122.8 . . ?
C6 C5 H5A 122.8 . . ?
C7 C6 C5 125.0 . . ?
C7 C6 H6A 117.5 . . ?
C5 C6 H6A 117.5 . . ?
C6 C7 C8 113.9 . . ?
C6 C7 H7A 123.1 . . ?
C8 C7 H7A 123.1 . . ?
C7 C8 C3 128.7 . . ?
C7 C8 H8A 115.6 . . ?
C3 C8 H8A 115.6 . . ?
O3 C9 O4 124.6(12) . . ?
O3 C9 C10 121.2(13) . . ?
O4 C9 C10 114.2(13) . . ?
C9 C10 C2 112.5(11) . . ?
C9 C10 C11 107.7(10) . . ?
C2 C10 C11 114.8(10) . . ?
C9 C10 H10A 107.2 . . ?
C2 C10 H10A 107.2 . . ?
C11 C10 H10A 107.2 . . ?
C12 C11 C16 116.0 . . ?
C12 C11 C10 124.5(8) . . ?
C16 C11 C10 119.4(8) . . ?
C13 C12 C11 124.0 . . ?
C13 C12 H12A 118.0 . . ?
C11 C12 H12A 118.0 . . ?
C14 C13 C12 120.3 . . ?
C14 C13 H13A 119.9 . . ?
C12 C13 H13A 119.9 . . ?
C13 C14 C15 121.8 . . ?
C13 C14 H14A 119.1 . . ?
C15 C14 H14A 119.1 . . ?
C16 C15 C14 117.0 . . ?
C16 C15 H15A 121.5 . . ?
C14 C15 H15A 121.5 . . ?
C15 C16 C11 120.4 . . ?
C15 C16 H16A 119.8 . . ?
C11 C16 H16A 119.8 . . ?
C17 O5 H5 109.5 . . ?
C25 O8 H8 109.5 . . ?
O6 C17 O5 125.1(12) . . ?
O6 C17 C18 121.1(13) . . ?
O5 C17 C18 113.8(13) . . ?
C17 C18 C26 115.1(11) . . ?
C17 C18 C19 107.2(9) . . ?
C26 C18 C19 111.4(10) . . ?
C17 C18 H18A 107.6 . . ?
C26 C18 H18A 107.6 . . ?
C19 C18 H18A 107.6 . . ?
C24 C19 C20 115.7 . . ?
C24 C19 C18 121.9(8) . . ?
C20 C19 C18 122.3(8) . . ?
C21 C20 C19 123.5 . . ?
C21 C20 H20A 118.3 . . ?
C19 C20 H20A 118.3 . . ?
C22 C21 C20 119.5 . . ?
C22 C21 H21A 120.2 . . ?
C20 C21 H21A 120.2 . . ?
C21 C22 C23 118.3 . . ?
C21 C22 H22A 120.9 . . ?
C23 C22 H22A 120.9 . . ?
C22 C23 C24 124.2 . . ?
C22 C23 H23A 117.9 . . ?
C24 C23 H23A 117.9 . . ?
C19 C24 C23 118.5 . . ?
C19 C24 H24A 120.8 . . ?
C23 C24 H24A 120.8 . . ?
O7 C25 O8 118.7(12) . . ?
O7 C25 C26 126.3(14) . . ?
O8 C25 C26 114.7(13) . . ?
C27 C26 C25 108.2(11) . . ?
C27 C26 C18 119.1(12) . . ?
C25 C26 C18 107.1(11) . . ?
C27 C26 H26A 107.3 . . ?
C25 C26 H26A 107.3 . . ?
C18 C26 H26A 107.3 . . ?
C28 C27 C26 128.8(10) . . ?
C28 C27 C32 115.1 . . ?
C26 C27 C32 116.1(10) . . ?
C27 C28 C29 120.6 . . ?
C27 C28 H28A 119.7 . . ?
C29 C28 H28A 119.7 . . ?
C30 C29 C28 125.2 . . ?
C30 C29 H29A 117.4 . . ?
C28 C29 H29A 117.4 . . ?
C29 C30 C31 117.6 . . ?
C29 C30 H30A 121.2 . . ?
C31 C30 H30A 121.2 . . ?
C30 C31 C32 124.7 . . ?
C30 C31 H31A 117.7 . . ?
C32 C31 H31A 117.7 . . ?
C31 C32 C27 116.4 . . ?
C31 C32 H32A 121.8 . . ?
C27 C32 H32A 121.8 . . ?
C33 O9 H9 109.5 . . ?
C41 O12 H12 109.5 . . ?
O10 C33 O9 123.5(12) . . ?
O10 C33 C34 121.9(14) . . ?
O9 C33 C34 114.6(13) . . ?
C35 C34 C33 104.1(10) . . ?
C35 C34 C42 112.2(10) . . ?
C33 C34 C42 108.7(11) . . ?
C35 C34 H34A 110.5 . . ?
C33 C34 H34A 110.5 . . ?
C42 C34 H34A 110.5 . . ?
C36 C35 C40 119.4 . . ?
C36 C35 C34 123.6(8) . . ?
C40 C35 C34 117.0(8) . . ?
C35 C36 C37 123.4 . . ?
C35 C36 H36A 118.3 . . ?
C37 C36 H36A 118.3 . . ?
C38 C37 C36 120.8 . . ?
C38 C37 H37A 119.6 . . ?
C36 C37 H37A 119.6 . . ?
C37 C38 C39 117.4 . . ?
C37 C38 H38A 121.3 . . ?
C39 C38 H38A 121.3 . . ?
C40 C39 C38 122.0 . . ?
C40 C39 H39A 119.0 . . ?
C38 C39 H39A 119.0 . . ?
C39 C40 C35 116.7 . . ?
C39 C40 H40A 121.6 . . ?
C35 C40 H40A 121.6 . . ?
O11 C41 O12 124.9(13) . . ?
O11 C41 C42 123.2(14) . . ?
O12 C41 C42 111.9(14) . . ?
C41 C42 C34 109.8(12) . . ?
C41 C42 C43 104.8(10) . . ?
C34 C42 C43 110.7(10) . . ?
C41 C42 H42A 110.5 . . ?
C34 C42 H42A 110.5 . . ?
C43 C42 H42A 110.5 . . ?
C44 C43 C48 117.2 . . ?
C44 C43 C42 117.0(9) . . ?
C48 C43 C42 125.8(9) . . ?
C43 C44 C45 113.7 . . ?
C43 C44 H44A 123.2 . . ?
C45 C44 H44A 123.2 . . ?
C46 C45 C44 125.7 . . ?
C46 C45 H45A 117.2 . . ?
C44 C45 H45A 117.2 . . ?
C47 C46 C45 117.9 . . ?
C47 C46 H46A 121.0 . . ?
C45 C46 H46A 121.0 . . ?
C46 C47 C48 116.9 . . ?
C46 C47 H47A 121.5 . . ?
C48 C47 H47A 121.5 . . ?
C47 C48 C43 127.9 . . ?
C47 C48 H48A 116.1 . . ?
C43 C48 H48A 116.1 . . ?
C49 O13 H13 109.5 . . ?
C57 O16 H16 109.5 . . ?
O14 C49 O13 124.7(14) . . ?
O14 C49 C50 122.7(15) . . ?
O13 C49 C50 112.4(14) . . ?
C58 C50 C51 108.6(11) . . ?
C58 C50 C49 110.4(12) . . ?
C51 C50 C49 108.3(10) . . ?
C58 C50 H50A 109.8 . . ?
C51 C50 H50A 109.8 . . ?
C49 C50 H50A 109.8 . . ?
C52 C51 C56 120.5 . . ?
C52 C51 C50 126.7(9) . . ?
C56 C51 C50 112.1(9) . . ?
C51 C52 C53 120.4 . . ?
C51 C52 H52A 119.8 . . ?
C53 C52 H52A 119.8 . . ?
C54 C53 C52 132.8 . . ?
C54 C53 H53A 113.6 . . ?
C52 C53 H53A 113.6 . . ?
C53 C54 C55 113.4 . . ?
C53 C54 H54A 123.3 . . ?
C55 C54 H54A 123.3 . . ?
C56 C55 C54 117.0 . . ?
C56 C55 H55A 121.5 . . ?
C54 C55 H55A 121.5 . . ?
C55 C56 C51 115.3 . . ?
C55 C56 H56A 122.4 . . ?
C51 C56 H56A 122.4 . . ?
O15 C57 O16 119.9(14) . . ?
O15 C57 C58 128.5(15) . . ?
O16 C57 C58 111.6(14) . . ?
C57 C58 C59 107.2(10) . . ?
C57 C58 C50 108.0(11) . . ?
C59 C58 C50 111.2(10) . . ?
C57 C58 H58A 110.1 . . ?
C59 C58 H58A 110.1 . . ?
C50 C58 H58A 110.1 . . ?
C64 C59 C60 118.7 . . ?
C64 C59 C58 122.8(8) . . ?
C60 C59 C58 117.8(8) . . ?
C61 C60 C59 123.1 . . ?
C61 C60 H60A 118.5 . . ?
C59 C60 H60A 118.5 . . ?
C60 C61 C62 116.1 . . ?
C60 C61 H61A 121.9 . . ?
C62 C61 H61A 121.9 . . ?
C61 C62 C63 120.3 . . ?
C61 C62 H62A 119.9 . . ?
C63 C62 H62A 119.9 . . ?
C64 C63 C62 118.6 . . ?
C64 C63 H63A 120.7 . . ?
C62 C63 H63A 120.7 . . ?
C59 C64 C63 122.8 . . ?
C59 C64 H64A 118.6 . . ?
C63 C64 H64A 118.6 . . ?
C3G O1G C2G 115(2) . . ?
C2G C1G H1GA 109.4 . . ?
C2G C1G H1GB 109.5 . . ?
H1GA C1G H1GB 109.5 . . ?
C2G C1G H1GC 109.4 . . ?
H1GA C1G H1GC 109.5 . . ?
H1GB C1G H1GC 109.5 . . ?
O1G C2G C1G 90(3) . . ?
O1G C2G H2GA 113.8 . . ?
C1G C2G H2GA 113.7 . . ?
O1G C2G H2GB 113.6 . . ?
C1G C2G H2GB 113.6 . . ?
H2GA C2G H2GB 110.9 . . ?
O1G C3G C4G 146(4) . . ?
O1G C3G H3GA 100.2 . . ?
C4G C3G H3GA 100.2 . . ?
O1G C3G H3GB 100.2 . . ?
C4G C3G H3GB 100.3 . . ?
H3GA C3G H3GB 104.3 . . ?
C3G C4G H4GA 109.5 . . ?
C3G C4G H4GB 109.5 . . ?
H4GA C4G H4GB 109.5 . . ?
C3G C4G H4GC 109.4 . . ?
H4GA C4G H4GC 109.5 . . ?
H4GB C4G H4GC 109.5 . . ?

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 C1 C2 C3 -89.9(15) . . . . ?
O1 C1 C2 C3 93.4(14) . . . . ?
O2 C1 C2 C10 35.1(18) . . . . ?
O1 C1 C2 C10 -141.5(12) . . . . ?
C10 C2 C3 C4 -48.8(13) . . . . ?
C1 C2 C3 C4 75.0(13) . . . . ?
C10 C2 C3 C8 134.1(10) . . . . ?
C1 C2 C3 C8 -102.1(12) . . . . ?
C8 C3 C4 C5 4.8 . . . . ?
C2 C3 C4 C5 -172.6(10) . . . . ?
C3 C4 C5 C6 -6.0 . . . . ?
C4 C5 C6 C7 11.8 . . . . ?
C5 C6 C7 C8 -14.2 . . . . ?
C6 C7 C8 C3 13.0 . . . . ?
C4 C3 C8 C7 -8.4 . . . . ?
C2 C3 C8 C7 168.7(11) . . . . ?
O3 C9 C10 C2 39.7(17) . . . . ?
O4 C9 C10 C2 -142.4(12) . . . . ?
O3 C9 C10 C11 -87.7(14) . . . . ?
O4 C9 C10 C11 90.1(13) . . . . ?
C3 C2 C10 C9 173.1(12) . . . . ?
C1 C2 C10 C9 52.1(16) . . . . ?
C3 C2 C10 C11 -63.2(15) . . . . ?
C1 C2 C10 C11 175.8(11) . . . . ?
C9 C10 C11 C12 -100.4(12) . . . . ?
C2 C10 C11 C12 133.5(10) . . . . ?
C9 C10 C11 C16 77.6(12) . . . . ?
C2 C10 C11 C16 -48.6(13) . . . . ?
C16 C11 C12 C13 -6.8 . . . . ?
C10 C11 C12 C13 171.2(9) . . . . ?
C11 C12 C13 C14 8.9 . . . . ?
C12 C13 C14 C15 -4.3 . . . . ?
C13 C14 C15 C16 -1.6 . . . . ?
C14 C15 C16 C11 3.3 . . . . ?
C12 C11 C16 C15 0.6 . . . . ?
C10 C11 C16 C15 -177.5(9) . . . . ?
O6 C17 C18 C26 37.1(17) . . . . ?
O5 C17 C18 C26 -144.7(12) . . . . ?
O6 C17 C18 C19 -87.4(14) . . . . ?
O5 C17 C18 C19 90.9(12) . . . . ?
C17 C18 C19 C24 -99.2(11) . . . . ?
C26 C18 C19 C24 134.1(10) . . . . ?
C17 C18 C19 C20 76.2(12) . . . . ?
C26 C18 C19 C20 -50.5(12) . . . . ?
C24 C19 C20 C21 1.4 . . . . ?
C18 C19 C20 C21 -174.2(9) . . . . ?
C19 C20 C21 C22 0.6 . . . . ?
C20 C21 C22 C23 -5.1 . . . . ?
C21 C22 C23 C24 8.0 . . . . ?
C20 C19 C24 C23 1.1 . . . . ?
C18 C19 C24 C23 176.7(9) . . . . ?
C22 C23 C24 C19 -5.9 . . . . ?
O7 C25 C26 C27 -87.4(16) . . . . ?
O8 C25 C26 C27 86.4(14) . . . . ?
O7 C25 C26 C18 42.2(18) . . . . ?
O8 C25 C26 C18 -144.0(11) . . . . ?
C17 C18 C26 C27 177.3(12) . . . . ?
C19 C18 C26 C27 -60.5(16) . . . . ?
C17 C18 C26 C25 54.2(15) . . . . ?
C19 C18 C26 C25 176.5(10) . . . . ?
C25 C26 C27 C28 -111.1(12) . . . . ?
C18 C26 C27 C28 126.4(11) . . . . ?
C25 C26 C27 C32 67.1(13) . . . . ?
C18 C26 C27 C32 -55.5(14) . . . . ?
C26 C27 C28 C29 177.7(12) . . . . ?
C32 C27 C28 C29 -0.5 . . . . ?
C27 C28 C29 C30 -3.1 . . . . ?
C28 C29 C30 C31 6.5 . . . . ?
C29 C30 C31 C32 -6.6 . . . . ?
C30 C31 C32 C27 3.2 . . . . ?
C28 C27 C32 C31 0.4 . . . . ?
C26 C27 C32 C31 -178.1(10) . . . . ?
O10 C33 C34 C35 -83.2(15) . . . . ?
O9 C33 C34 C35 97.2(13) . . . . ?
O10 C33 C34 C42 36.6(17) . . . . ?
O9 C33 C34 C42 -143.0(12) . . . . ?
C33 C34 C35 C36 71.9(12) . . . . ?
C42 C34 C35 C36 -45.6(12) . . . . ?
C33 C34 C35 C40 -105.4(11) . . . . ?
C42 C34 C35 C40 137.1(9) . . . . ?
C40 C35 C36 C37 -1.8 . . . . ?
C34 C35 C36 C37 -179.1(9) . . . . ?
C35 C36 C37 C38 3.7 . . . . ?
C36 C37 C38 C39 -5.0 . . . . ?
C37 C38 C39 C40 5.2 . . . . ?
C38 C39 C40 C35 -3.4 . . . . ?
C36 C35 C40 C39 1.8 . . . . ?
C34 C35 C40 C39 179.2(8) . . . . ?
O11 C41 C42 C34 32.7(18) . . . . ?
O12 C41 C42 C34 -149.2(12) . . . . ?
O11 C41 C42 C43 -86.2(16) . . . . ?
O12 C41 C42 C43 91.8(13) . . . . ?
C35 C34 C42 C41 173.8(10) . . . . ?
C33 C34 C42 C41 59.2(15) . . . . ?
C35 C34 C42 C43 -70.9(13) . . . . ?
C33 C34 C42 C43 174.4(10) . . . . ?
C41 C42 C43 C44 -107.1(11) . . . . ?
C34 C42 C43 C44 134.6(10) . . . . ?
C41 C42 C43 C48 75.2(13) . . . . ?
C34 C42 C43 C48 -43.2(13) . . . . ?
C48 C43 C44 C45 -2.9 . . . . ?
C42 C43 C44 C45 179.1(10) . . . . ?
C43 C44 C45 C46 -5.0 . . . . ?
C44 C45 C46 C47 9.5 . . . . ?
C45 C46 C47 C48 -5.0 . . . . ?
C46 C47 C48 C43 -3.2 . . . . ?
C44 C43 C48 C47 7.5 . . . . ?
C42 C43 C48 C47 -174.8(11) . . . . ?
O14 C49 C50 C58 36.3(18) . . . . ?
O13 C49 C50 C58 -147.6(12) . . . . ?
O14 C49 C50 C51 -82.5(16) . . . . ?
O13 C49 C50 C51 93.5(13) . . . . ?
C58 C50 C51 C52 -47.0(13) . . . . ?
C49 C50 C51 C52 72.9(13) . . . . ?
C58 C50 C51 C56 142.7(9) . . . . ?
C49 C50 C51 C56 -97.4(12) . . . . ?
C56 C51 C52 C53 -8.6 . . . . ?
C50 C51 C52 C53 -178.2(10) . . . . ?
C51 C52 C53 C54 10.2 . . . . ?
C52 C53 C54 C55 -4.4 . . . . ?
C53 C54 C55 C56 -1.8 . . . . ?
C54 C55 C56 C51 2.1 . . . . ?
C52 C51 C56 C55 3.1 . . . . ?
C50 C51 C56 C55 174.1(9) . . . . ?
O15 C57 C58 C59 -82.2(18) . . . . ?
O16 C57 C58 C59 96.7(13) . . . . ?
O15 C57 C58 C50 38(2) . . . . ?
O16 C57 C58 C50 -143.5(12) . . . . ?
C51 C50 C58 C57 174.6(11) . . . . ?
C49 C50 C58 C57 55.9(15) . . . . ?
C51 C50 C58 C59 -68.1(14) . . . . ?
C49 C50 C58 C59 173.2(10) . . . . ?
C57 C58 C59 C64 68.1(12) . . . . ?
C50 C58 C59 C64 -49.7(13) . . . . ?
C57 C58 C59 C60 -102.7(11) . . . . ?
C50 C58 C59 C60 139.5(9) . . . . ?
C64 C59 C60 C61 6.2 . . . . ?
C58 C59 C60 C61 177.3(9) . . . . ?
C59 C60 C61 C62 -6.7 . . . . ?
C60 C61 C62 C63 5.6 . . . . ?
C61 C62 C63 C64 -4.0 . . . . ?
C60 C59 C64 C63 -4.3 . . . . ?
C58 C59 C64 C63 -174.9(9) . . . . ?
C62 C63 C64 C59 3.3 . . . . ?
C3G O1G C2G C1G -136(4) . . . . ?
C2G O1G C3G C4G -122(6) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O6 0.85 1.84 2.677(12) 167.5 .
O4 H4 O14 0.85 1.85 2.672(13) 162.6 1_565
O5 H5 O2 0.85 1.78 2.630(12) 173.8 .
O8 H8 O10 0.85 1.84 2.648(14) 158.2 1_565
O9 H9 O7 0.85 1.81 2.613(13) 157.2 1_545
O12 H12 O15 0.85 1.81 2.654(14) 172.3 .
O13 H13 O3 0.85 1.83 2.668(14) 169.1 1_545
O16 H16 O11 0.85 1.87 2.681(14) 159.9 .

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        20.81
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.085

# Attachment 'xtal5.cif'

data_xtal5
_database_code_depnum_ccdc_archive 'CCDC 706647'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C68 H64 O17'
_chemical_formula_weight         1153.19

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           tetragonal
_symmetry_space_group_name_H-M   I4

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

_cell_length_a                   16.3890(3)
_cell_length_b                   16.3890(3)
_cell_length_c                   11.3011(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3035.47(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1216
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_correction_T_min  
;
Ratio of minimum to maximum apparent transmission: 0.782538
;
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298(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  'Bruker APEX CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13122
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.76
_diffrn_reflns_theta_max         28.30
_reflns_number_total             3493
_reflns_number_gt                1801
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  'Bruker XCIF'

_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.

We used two DFIX restraints for O1-H1O and O4-H4O bonds, AFIX restraints
for the H atoms attached to C atoms, and ISOR restraints for five
non-hydrogen atoms of the guest molecule. As the guest molecule sits on
the four-fold axis, some of them must follow symmetric restrictions.
;

_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)+(0.0877P)²+0.0000P] 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     SHELXL
_refine_ls_extinction_coef       0.0010(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.2(18)
_refine_ls_number_reflns         3493
_refine_ls_number_parameters     221
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.1193
_refine_ls_R_factor_gt           0.0525
_refine_ls_wR_factor_ref         0.1693
_refine_ls_wR_factor_gt          0.1363
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_restrained_S_all      0.983
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.002

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 0.77678(16) 0.12585(13) 0.2813(2) 0.0751(7) Uani 1 1 d D . .
H1O H 0.777(2) 0.0728(12) 0.293(4) 0.090 Uiso 1 1 d D . .
O2 O 0.79821(16) 0.13612(13) 0.4747(2) 0.0745(7) Uani 1 1 d . . .
O3 O 0.96637(14) 0.24212(16) 0.3243(2) 0.0799(8) Uani 1 1 d . . .
O4 O 0.98461(14) 0.25373(17) 0.5182(2) 0.0796(7) Uani 1 1 d D . .
H4O H 1.0312(15) 0.232(2) 0.503(4) 0.096 Uiso 1 1 d D . .
C1 C 0.79078(17) 0.16739(17) 0.3778(3) 0.0559(7) Uani 1 1 d . . .
C2 C 0.79360(17) 0.25880(15) 0.3600(3) 0.0540(7) Uani 1 1 d . . .
H2 H 0.8092 0.2700 0.2779 0.065 Uiso 1 1 calc R . .
C3 C 0.70789(17) 0.29120(15) 0.3804(3) 0.0562(7) Uani 1 1 d . . .
C4 C 0.6597(2) 0.3122(2) 0.2852(3) 0.0769(10) Uani 1 1 d . . .
H4 H 0.6808 0.3101 0.2089 0.092 Uiso 1 1 calc R . .
C5 C 0.5792(3) 0.3366(2) 0.3039(5) 0.0956(14) Uani 1 1 d . . .
H5 H 0.5467 0.3509 0.2397 0.115 Uiso 1 1 calc R . .
C6 C 0.5477(2) 0.3396(2) 0.4150(6) 0.0939(13) Uani 1 1 d . . .
H6 H 0.4935 0.3542 0.4270 0.113 Uiso 1 1 calc R . .
C7 C 0.5962(2) 0.3210(2) 0.5081(4) 0.0894(12) Uani 1 1 d . . .
H7 H 0.5757 0.3252 0.5846 0.107 Uiso 1 1 calc R . .
C8 C 0.67532(19) 0.2962(2) 0.4912(3) 0.0738(10) Uani 1 1 d . . .
H8 H 0.7072 0.2826 0.5564 0.089 Uiso 1 1 calc R . .
C9 C 0.94142(17) 0.26073(16) 0.4225(4) 0.0575(7) Uani 1 1 d . . .
C10 C 0.85739(16) 0.29751(16) 0.4426(3) 0.0537(7) Uani 1 1 d . . .
H10 H 0.8412 0.2867 0.5246 0.064 Uiso 1 1 calc R . .
C11 C 0.86589(16) 0.38918(18) 0.4267(4) 0.0623(8) Uani 1 1 d . . .
C12 C 0.8728(3) 0.4228(2) 0.3171(5) 0.1194(18) Uani 1 1 d . . .
H12 H 0.8696 0.3896 0.2505 0.143 Uiso 1 1 calc R . .
C13 C 0.8847(4) 0.5068(4) 0.3041(8) 0.152(2) Uani 1 1 d . . .
H13A H 0.8894 0.5281 0.2282 0.183 Uiso 1 1 calc R . .
C14 C 0.8893(3) 0.5554(3) 0.3921(10) 0.137(3) Uani 1 1 d . . .
H14 H 0.8981 0.6109 0.3803 0.164 Uiso 1 1 calc R . .
C15 C 0.8809(4) 0.5243(4) 0.5054(8) 0.147(3) Uani 1 1 d . . .
H15 H 0.8842 0.5588 0.5704 0.176 Uiso 1 1 calc R . .
C16 C 0.8671(3) 0.4395(3) 0.5221(5) 0.1026(14) Uani 1 1 d . . .
H16 H 0.8590 0.4187 0.5977 0.123 Uiso 1 1 calc R . .
O1G O 0.0578(13) 0.0438(14) 0.3712(19) 0.199(8) Uani 0.25 1 d PU . .
C1G C -0.016(12) 0.021(9) 0.548(2) 0.125(11) Uani 0.25 1 d PU . .
C2G C 0.0000 0.0000 0.436(3) 0.187(6) Uani 1 4 d SU . .
C3G C 0.0000 0.0000 0.316(2) 0.180(6) Uani 1 4 d SU . .
C4G C 0.021(5) 0.018(6) 0.2013(17) 0.117(11) Uani 0.25 1 d PU . .


_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 C1 1.306(4) . ?
O1 H1O 0.878(18) . ?
O2 C1 1.215(4) . ?
O3 C9 1.222(4) . ?
O4 C9 1.297(4) . ?
O4 H4O 0.859(19) . ?
C1 C2 1.512(4) . ?
C2 C3 1.519(4) . ?
C2 C10 1.539(4) . ?
C2 H2 0.9800 . ?
C3 C8 1.365(5) . ?
C3 C4 1.377(5) . ?
C4 C5 1.395(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.359(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.353(7) . ?
C6 H6 0.9300 . ?
C7 C8 1.372(5) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C10 1.520(4) . ?
C10 C11 1.519(4) . ?
C10 H10 0.9800 . ?
C11 C16 1.358(6) . ?
C11 C12 1.359(6) . ?
C12 C13 1.398(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.277(9) . ?
C13 H13A 0.9300 . ?
C14 C15 1.385(9) . ?
C14 H14 0.9300 . ?
C15 C16 1.420(8) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
O1G C2G 1.40(2) . ?
O1G C3G 1.34(2) . ?
O1G O1G 1.68(2) 4 ?
O1G O1G 1.68(2) 3 ?
C1G C1G 0.61(4) 3 ?
C1G C1G 0.61(4) 4 ?
C1G C1G 0.87(6) 2 ?
C1G C2G 1.34(3) . ?
C2G C3G 1.35(3) . ?
C2G O1G 1.40(2) 2 ?
C2G O1G 1.40(2) 4 ?
C2G O1G 1.40(2) 3 ?
C2G C1G 1.34(3) 4 ?
C2G C1G 1.34(3) 3 ?
C2G C1G 1.34(3) 2 ?
C3G O1G 1.34(2) 3 ?
C3G O1G 1.34(2) 4 ?
C3G O1G 1.34(2) 2 ?
C3G C4G 1.38(3) . ?
C3G C4G 1.38(3) 3 ?
C3G C4G 1.38(3) 2 ?
C3G C4G 1.38(3) 4 ?
C4G C4G 0.64(4) 3 ?
C4G C4G 0.64(4) 4 ?
C4G C4G 0.91(5) 2 ?

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
C1 O1 H1O 113(3) . . ?
C9 O4 H4O 111(3) . . ?
O2 C1 O1 123.4(3) . . ?
O2 C1 C2 122.3(3) . . ?
O1 C1 C2 114.3(3) . . ?
C1 C2 C3 107.3(2) . . ?
C1 C2 C10 110.4(3) . . ?
C3 C2 C10 113.1(2) . . ?
C1 C2 H2 108.6 . . ?
C3 C2 H2 108.6 . . ?
C10 C2 H2 108.6 . . ?
C8 C3 C4 118.5(3) . . ?
C8 C3 C2 121.5(3) . . ?
C4 C3 C2 119.9(3) . . ?
C3 C4 C5 119.7(4) . . ?
C3 C4 H4 120.1 . . ?
C5 C4 H4 120.1 . . ?
C6 C5 C4 120.6(4) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C7 C6 C5 119.2(4) . . ?
C7 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?
C6 C7 C8 120.9(5) . . ?
C6 C7 H7 119.5 . . ?
C8 C7 H7 119.5 . . ?
C3 C8 C7 121.0(4) . . ?
C3 C8 H8 119.5 . . ?
C7 C8 H8 119.5 . . ?
O3 C9 O4 123.5(3) . . ?
O3 C9 C10 122.5(3) . . ?
O4 C9 C10 113.9(3) . . ?
C9 C10 C11 106.9(2) . . ?
C9 C10 C2 111.2(2) . . ?
C11 C10 C2 113.5(2) . . ?
C9 C10 H10 108.4 . . ?
C11 C10 H10 108.4 . . ?
C2 C10 H10 108.4 . . ?
C16 C11 C12 118.4(3) . . ?
C16 C11 C10 120.5(4) . . ?
C12 C11 C10 121.0(3) . . ?
C11 C12 C13 120.4(6) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C14 C13 C12 122.7(7) . . ?
C14 C13 H13A 118.6 . . ?
C12 C13 H13A 118.6 . . ?
C13 C14 C15 118.9(6) . . ?
C13 C14 H14 120.5 . . ?
C15 C14 H14 120.5 . . ?
C14 C15 C16 120.0(5) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C11 C16 C15 119.4(6) . . ?
C11 C16 H16 120.3 . . ?
C15 C16 H16 120.3 . . ?
C2G O1G C3G 59.3(14) . . ?
C2G O1G O1G 53.0(6) . 4 ?
C3G O1G O1G 51.2(6) . 4 ?
C2G O1G O1G 53.0(6) . 3 ?
C3G O1G O1G 51.2(6) . 3 ?
O1G O1G O1G 90.000(3) 4 3 ?
C1G C1G C1G 90.00(3) 3 4 ?
C1G C1G C1G 45.000(9) 3 2 ?
C1G C1G C1G 45.00(3) 4 2 ?
C1G C1G C2G 76.8(9) 3 . ?
C1G C1G C2G 76.8(9) 4 . ?
C1G C1G C2G 71.1(13) 2 . ?
C3G C2G O1G 58.4(14) . . ?
C3G C2G O1G 58.4(14) . 2 ?
O1G C2G O1G 117(3) . 2 ?
C3G C2G O1G 58.4(14) . 4 ?
O1G C2G O1G 74.1(13) . 4 ?
O1G C2G O1G 74.1(13) 2 4 ?
C3G C2G O1G 58.4(14) . 3 ?
O1G C2G O1G 74.1(13) . 3 ?
O1G C2G O1G 74.1(13) 2 3 ?
O1G C2G O1G 117(3) 4 3 ?
C3G C2G C1G 161.1(13) . 4 ?
O1G C2G C1G 102.7(16) . 4 ?
O1G C2G C1G 141(2) 2 4 ?
O1G C2G C1G 120(10) 4 4 ?
O1G C2G C1G 119(10) 3 4 ?
C3G C2G C1G 161.1(13) . 3 ?
O1G C2G C1G 141(2) . 3 ?
O1G C2G C1G 102.7(16) 2 3 ?
O1G C2G C1G 119(10) 4 3 ?
O1G C2G C1G 120(10) 3 3 ?
C1G C2G C1G 38(3) 4 3 ?
C3G C2G C1G 161.1(13) . 2 ?
O1G C2G C1G 119(10) . 2 ?
O1G C2G C1G 120(10) 2 2 ?
O1G C2G C1G 102.7(16) 4 2 ?
O1G C2G C1G 141(2) 3 2 ?
C1G C2G C1G 26.5(18) 4 2 ?
C1G C2G C1G 26.5(18) 3 2 ?
C3G C2G C1G 161.1(13) . . ?
O1G C2G C1G 120(10) . . ?
O1G C2G C1G 119(10) 2 . ?
O1G C2G C1G 141(2) 4 . ?
O1G C2G C1G 102.7(16) 3 . ?
C1G C2G C1G 26.5(18) 4 . ?
C1G C2G C1G 26.5(18) 3 . ?
C1G C2G C1G 38(3) 2 . ?
C2G C3G O1G 62.4(14) . . ?
C2G C3G O1G 62.4(14) . 3 ?
O1G C3G O1G 77.6(11) . 3 ?
C2G C3G O1G 62.4(14) . 4 ?
O1G C3G O1G 77.6(11) . 4 ?
O1G C3G O1G 125(3) 3 4 ?
C2G C3G O1G 62.4(14) . 2 ?
O1G C3G O1G 125(3) . 2 ?
O1G C3G O1G 77.6(11) 3 2 ?
O1G C3G O1G 77.6(11) 4 2 ?
C2G C3G C4G 160.7(11) . . ?
O1G C3G C4G 98.4(15) . . ?
O1G C3G C4G 115(5) 3 . ?
O1G C3G C4G 117(5) 4 . ?
O1G C3G C4G 137(2) 2 . ?
C2G C3G C4G 160.7(11) . 3 ?
O1G C3G C4G 117(5) . 3 ?
O1G C3G C4G 98.4(15) 3 3 ?
O1G C3G C4G 137(2) 4 3 ?
O1G C3G C4G 115(5) 2 3 ?
C4G C3G C4G 27.0(15) . 3 ?
C2G C3G C4G 160.7(11) . 2 ?
O1G C3G C4G 137(2) . 2 ?
O1G C3G C4G 117(5) 3 2 ?
O1G C3G C4G 115(5) 4 2 ?
O1G C3G C4G 98.4(15) 2 2 ?
C4G C3G C4G 39(2) . 2 ?
C4G C3G C4G 27.0(15) 3 2 ?
C2G C3G C4G 160.7(11) . 4 ?
O1G C3G C4G 115(5) . 4 ?
O1G C3G C4G 137(2) 3 4 ?
O1G C3G C4G 98.4(15) 4 4 ?
O1G C3G C4G 117(5) 2 4 ?
C4G C3G C4G 27.0(15) . 4 ?
C4G C3G C4G 39(2) 3 4 ?
C4G C3G C4G 27.0(15) 2 4 ?
C4G C4G C4G 90.000(4) 3 4 ?
C4G C4G C4G 45.000(18) 3 2 ?
C4G C4G C4G 45.000(19) 4 2 ?
C4G C4G C3G 76.5(8) 3 . ?
C4G C4G C3G 76.5(8) 4 . ?
C4G C4G C3G 70.7(11) 2 . ?

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 C1 C2 C3 -86.1(4) . . . . ?
O1 C1 C2 C3 91.6(3) . . . . ?
O2 C1 C2 C10 37.6(4) . . . . ?
O1 C1 C2 C10 -144.8(3) . . . . ?
C1 C2 C3 C8 73.6(4) . . . . ?
C10 C2 C3 C8 -48.4(4) . . . . ?
C1 C2 C3 C4 -102.9(3) . . . . ?
C10 C2 C3 C4 135.1(3) . . . . ?
C8 C3 C4 C5 -1.0(5) . . . . ?
C2 C3 C4 C5 175.6(3) . . . . ?
C3 C4 C5 C6 -0.2(6) . . . . ?
C4 C5 C6 C7 2.0(6) . . . . ?
C5 C6 C7 C8 -2.6(6) . . . . ?
C4 C3 C8 C7 0.4(5) . . . . ?
C2 C3 C8 C7 -176.1(3) . . . . ?
C6 C7 C8 C3 1.4(6) . . . . ?
O3 C9 C10 C11 -86.6(3) . . . . ?
O4 C9 C10 C11 91.2(3) . . . . ?
O3 C9 C10 C2 37.8(4) . . . . ?
O4 C9 C10 C2 -144.4(3) . . . . ?
C1 C2 C10 C9 57.4(3) . . . . ?
C3 C2 C10 C9 177.6(3) . . . . ?
C1 C2 C10 C11 178.0(3) . . . . ?
C3 C2 C10 C11 -61.8(3) . . . . ?
C9 C10 C11 C16 -103.9(4) . . . . ?
C2 C10 C11 C16 133.1(3) . . . . ?
C9 C10 C11 C12 75.8(4) . . . . ?
C2 C10 C11 C12 -47.1(4) . . . . ?
C16 C11 C12 C13 3.0(7) . . . . ?
C10 C11 C12 C13 -176.8(4) . . . . ?
C11 C12 C13 C14 -0.3(9) . . . . ?
C12 C13 C14 C15 -1.1(9) . . . . ?
C13 C14 C15 C16 -0.2(9) . . . . ?
C12 C11 C16 C15 -4.2(6) . . . . ?
C10 C11 C16 C15 175.6(4) . . . . ?
C14 C15 C16 C11 2.9(8) . . . . ?
O1G O1G C2G C3G -62.3(9) 4 . . . ?
O1G O1G C2G C3G 62.3(9) 3 . . . ?
C3G O1G C2G O1G 0.000(1) . . . 2 ?
O1G O1G C2G O1G -62.3(9) 4 . . 2 ?
O1G O1G C2G O1G 62.3(9) 3 . . 2 ?
C3G O1G C2G O1G 62.3(9) . . . 4 ?
O1G O1G C2G O1G 124.7(19) 3 . . 4 ?
C3G O1G C2G O1G -62.3(9) . . . 3 ?
O1G O1G C2G O1G -124.7(19) 4 . . 3 ?
C3G O1G C2G C1G -180(11) . . . 4 ?
O1G O1G C2G C1G 118(11) 4 . . 4 ?
O1G O1G C2G C1G -117(11) 3 . . 4 ?
C3G O1G C2G C1G 179(17) . . . 3 ?
O1G O1G C2G C1G 117(17) 4 . . 3 ?
O1G O1G C2G C1G -118(17) 3 . . 3 ?
C3G O1G C2G C1G 158(3) . . . 2 ?
O1G O1G C2G C1G 96(3) 4 . . 2 ?
O1G O1G C2G C1G -139(3) 3 . . 2 ?
C3G O1G C2G C1G -158(3) . . . . ?
O1G O1G C2G C1G 140(3) 4 . . . ?
O1G O1G C2G C1G -96(3) 3 . . . ?
C1G C1G C2G C3G 133.4(3) 3 . . . ?
C1G C1G C2G C3G -133.4(2) 4 . . . ?
C1G C1G C2G C3G 180.00(9) 2 . . . ?
C1G C1G C2G O1G -147(30) 3 . . . ?
C1G C1G C2G O1G -54(30) 4 . . . ?
C1G C1G C2G O1G -100(30) 2 . . . ?
C1G C1G C2G O1G 56(30) 3 . . 2 ?
C1G C1G C2G O1G 149(30) 4 . . 2 ?
C1G C1G C2G O1G 102(30) 2 . . 2 ?
C1G C1G C2G O1G -45(44) 3 . . 4 ?
C1G C1G C2G O1G 48(44) 4 . . 4 ?
C1G C1G C2G O1G 1(44) 2 . . 4 ?
C1G C1G C2G O1G 134(29) 3 . . 3 ?
C1G C1G C2G O1G -133(29) 4 . . 3 ?
C1G C1G C2G O1G -179(29) 2 . . 3 ?
C1G C1G C2G C1G -93.2(5) 3 . . 4 ?
C1G C1G C2G C1G -46.6(2) 2 . . 4 ?
C1G C1G C2G C1G 93.2(4) 4 . . 3 ?
C1G C1G C2G C1G 46.6(2) 2 . . 3 ?
C1G C1G C2G C1G -46.6(2) 3 . . 2 ?
C1G C1G C2G C1G 46.6(2) 4 . . 2 ?
O1G C2G C3G O1G 180.0 2 . . . ?
O1G C2G C3G O1G -90.000(3) 4 . . . ?
O1G C2G C3G O1G 90.000(4) 3 . . . ?
C1G C2G C3G O1G 1(33) 4 . . . ?
C1G C2G C3G O1G -179(33) 3 . . . ?
C1G C2G C3G O1G -89(33) 2 . . . ?
C1G C2G C3G O1G 91(33) . . . . ?
O1G C2G C3G O1G -90.000(3) . . . 3 ?
O1G C2G C3G O1G 90.000(3) 2 . . 3 ?
O1G C2G C3G O1G 180.000(3) 4 . . 3 ?
C1G C2G C3G O1G -89(33) 4 . . 3 ?
C1G C2G C3G O1G 91(33) 3 . . 3 ?
C1G C2G C3G O1G -179(33) 2 . . 3 ?
C1G C2G C3G O1G 1(33) . . . 3 ?
O1G C2G C3G O1G 90.000(2) . . . 4 ?
O1G C2G C3G O1G -90.000(2) 2 . . 4 ?
O1G C2G C3G O1G 180.000(3) 3 . . 4 ?
C1G C2G C3G O1G 91(33) 4 . . 4 ?
C1G C2G C3G O1G -89(33) 3 . . 4 ?
C1G C2G C3G O1G 1(33) 2 . . 4 ?
C1G C2G C3G O1G -179(33) . . . 4 ?
O1G C2G C3G O1G 180.0 . . . 2 ?
O1G C2G C3G O1G 90.000(3) 4 . . 2 ?
O1G C2G C3G O1G -90.000(4) 3 . . 2 ?
C1G C2G C3G O1G -179(33) 4 . . 2 ?
C1G C2G C3G O1G 1(33) 3 . . 2 ?
C1G C2G C3G O1G 91(33) 2 . . 2 ?
C1G C2G C3G O1G -89(33) . . . 2 ?
O1G C2G C3G C4G -3(16) . . . . ?
O1G C2G C3G C4G 177(16) 2 . . . ?
O1G C2G C3G C4G -93(16) 4 . . . ?
O1G C2G C3G C4G 87(16) 3 . . . ?
C1G C2G C3G C4G -2(38) 4 . . . ?
C1G C2G C3G C4G 178(38) 3 . . . ?
C1G C2G C3G C4G -92(38) 2 . . . ?
C1G C2G C3G C4G 88(38) . . . . ?
O1G C2G C3G C4G -93(16) . . . 3 ?
O1G C2G C3G C4G 87(16) 2 . . 3 ?
O1G C2G C3G C4G 177(16) 4 . . 3 ?
O1G C2G C3G C4G -3(16) 3 . . 3 ?
C1G C2G C3G C4G -92(38) 4 . . 3 ?
C1G C2G C3G C4G 88(38) 3 . . 3 ?
C1G C2G C3G C4G 178(38) 2 . . 3 ?
C1G C2G C3G C4G -2(38) . . . 3 ?
O1G C2G C3G C4G 177(16) . . . 2 ?
O1G C2G C3G C4G -3(16) 2 . . 2 ?
O1G C2G C3G C4G 87(16) 4 . . 2 ?
O1G C2G C3G C4G -93(16) 3 . . 2 ?
C1G C2G C3G C4G 178(38) 4 . . 2 ?
C1G C2G C3G C4G -2(38) 3 . . 2 ?
C1G C2G C3G C4G 88(38) 2 . . 2 ?
C1G C2G C3G C4G -92(38) . . . 2 ?
O1G C2G C3G C4G 87(16) . . . 4 ?
O1G C2G C3G C4G -93(16) 2 . . 4 ?
O1G C2G C3G C4G -3(16) 4 . . 4 ?
O1G C2G C3G C4G 177(16) 3 . . 4 ?
C1G C2G C3G C4G 88(38) 4 . . 4 ?
C1G C2G C3G C4G -92(38) 3 . . 4 ?
C1G C2G C3G C4G -2(38) 2 . . 4 ?
C1G C2G C3G C4G 178(38) . . . 4 ?
O1G O1G C3G C2G 65.1(10) 4 . . . ?
O1G O1G C3G C2G -65.1(10) 3 . . . ?
C2G O1G C3G O1G 65.1(10) . . . 3 ?
O1G O1G C3G O1G 130(2) 4 . . 3 ?
C2G O1G C3G O1G -65.1(10) . . . 4 ?
O1G O1G C3G O1G -130(2) 3 . . 4 ?
C2G O1G C3G O1G 0.000(1) . . . 2 ?
O1G O1G C3G O1G 65.1(10) 4 . . 2 ?
O1G O1G C3G O1G -65.1(10) 3 . . 2 ?
C2G O1G C3G C4G 179(5) . . . . ?
O1G O1G C3G C4G -116(5) 4 . . . ?
O1G O1G C3G C4G 114(5) 3 . . . ?
C2G O1G C3G C4G 158.3(15) . . . 3 ?
O1G O1G C3G C4G -137(2) 4 . . 3 ?
O1G O1G C3G C4G 93.2(14) 3 . . 3 ?
C2G O1G C3G C4G -179(7) . . . 2 ?
O1G O1G C3G C4G -114(8) 4 . . 2 ?
O1G O1G C3G C4G 116(8) 3 . . 2 ?
C2G O1G C3G C4G -158.6(18) . . . 4 ?
O1G O1G C3G C4G -93.5(17) 4 . . 4 ?
O1G O1G C3G C4G 136(2) 3 . . 4 ?
C2G C3G C4G C4G -133.3(2) . . . 3 ?
O1G C3G C4G C4G -136(14) . . . 3 ?
O1G C3G C4G C4G -56(14) 3 . . 3 ?
O1G C3G C4G C4G 144(14) 4 . . 3 ?
O1G C3G C4G C4G 43(20) 2 . . 3 ?
C4G C3G C4G C4G 46.66(18) 2 . . 3 ?
C4G C3G C4G C4G 93.3(4) 4 . . 3 ?
C2G C3G C4G C4G 133.34(18) . . . 4 ?
O1G C3G C4G C4G 131(14) . . . 4 ?
O1G C3G C4G C4G -149(14) 3 . . 4 ?
O1G C3G C4G C4G 51(14) 4 . . 4 ?
O1G C3G C4G C4G -50(20) 2 . . 4 ?
C4G C3G C4G C4G -93.3(4) 3 . . 4 ?
C4G C3G C4G C4G -46.66(19) 2 . . 4 ?
C2G C3G C4G C4G 180.00(4) . . . 2 ?
O1G C3G C4G C4G 178(14) . . . 2 ?
O1G C3G C4G C4G -102(14) 3 . . 2 ?
O1G C3G C4G C4G 97(14) 4 . . 2 ?
O1G C3G C4G C4G -4(20) 2 . . 2 ?
C4G C3G C4G C4G -46.66(19) 3 . . 2 ?
C4G C3G C4G C4G 46.66(19) 4 . . 2 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1O O3 0.878(18) 1.81(2) 2.676(3) 169(4) 3_645
O4 H4O O2 0.859(19) 1.82(2) 2.671(3) 172(4) 4_665

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.30
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.180
_refine_diff_density_min         -0.133
_refine_diff_density_rms         0.035


