##############################################################################
###                                                                        ###
###        Electronic paper (Acta Crystallographica Section E)             ###
###                                                                        ###
##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section E. It conforms to the requirements of Notes      #
# for Authors for Section E, and has been peer reviewed under the auspices   #
# of the IUCr Commission on Journals.                                        #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.1.    #
#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
# this CIF.  For information consult the CIF home page http://www.iucr.org/  #
# cif/home.html                                                              #
#                                                                            #
#            Copyright International Union of Crystallography                #
#                                                                            #
##############################################################################
                                             
data_General
_audit_creation_method     'by teXsan'
_journal_date_recd_electronic     2003-09-01
_journal_date_accepted     2003-09-08
_journal_name_full     'Acta Crystallographica, Section E'
_journal_year     2003
_journal_volume     59
_journal_issue     10
_journal_page_first     o1476
_journal_page_last     o1477
_journal_paper_category     EO
_publ_contact_author_name     'Professor Shigeru Ohba'
_publ_contact_author_address
;
Department of Chemistry
Keio University
Hiyoshi 4-1-1, Kohoku-ku
Yokohama 223-8521
Japan
;
_publ_contact_author_email     'ohba@flet.keio.ac.jp'
_publ_contact_author_fax     '(81) 45 566 1314'
_publ_contact_author_phone     '(81) 45 566 1308'
_publ_section_title
;
(+)-(1S,2S,4S,4aR,5R,6S,9S,10S)-4-Benzyloxy-9,10-(carbonyldioxy)-
1-methoxymethoxy-4a,6,8,8-tetramethyl-7-methylenedodecahydro-
6,9-ethanobenzocyclooctene-5-ol
;
loop_
    _publ_author_name
    _publ_author_address
    'Ohba, Shigeru'
;
Department of Chemistry
Keio University
Hiyoshi 4-1-1, Kohoku-ku
Yokohama 223-8521
Japan
;
    'Chinen, Ayako'
;
Department of Applied Chemistry
Faculty of Science and Technology
Keio University
Hiyoshi 3-14-1, Kohoku-ku
Yokohama 223-8522
Japan
;
    'Matsumoto, Yuki'
;
Department of Applied Chemistry
Faculty of Science and Technology
Keio University
Hiyoshi 3-14-1, Kohoku-ku
Yokohama 223-8522
Japan
;
    'Chida, Noritaka'
;
Department of Applied Chemistry
Faculty of Science and Technology
Keio University
Hiyoshi 3-14-1, Kohoku-ku
Yokohama 223-8522
Japan
;
data_I
_chemical_formula_moiety     'C29 H40 O7 '
_chemical_formula_sum     'C29 H40 O7 '
_chemical_formula_weight     500.63
_chemical_melting_point     '427-430'
_symmetry_cell_setting     orthorhombic
_symmetry_space_group_name_H-M     'P 21 21 21   '
loop_
    _symmetry_equiv_pos_as_xyz
    x,y,z
    1/2-x,-y,1/2+z
    1/2+x,1/2-y,-z
    -x,1/2+y,1/2-z
_cell_length_a     13.754(2)
_cell_length_b     21.026(7)
_cell_length_c     9.1287(10)
_cell_angle_alpha     90
_cell_angle_beta     90
_cell_angle_gamma     90
_cell_volume     2639.9(10)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     25
_cell_measurement_theta_min     10.0
_cell_measurement_theta_max     11.2
_cell_measurement_temperature     297
_exptl_crystal_description     'prismatic'
_exptl_crystal_colour     'colourless'
_exptl_crystal_size_max     0.50
_exptl_crystal_size_mid     0.40
_exptl_crystal_size_min     0.40
_exptl_crystal_size_rad     ?
_exptl_crystal_density_diffrn     1.260
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     1080
_exptl_absorpt_coefficient_mu     0.089
_exptl_absorpt_correction_type     none
_diffrn_radiation_type     'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_measurement_device_type     'Rigaku AFC7R'
_diffrn_measurement_method     ω
_diffrn_reflns_number     4059
_diffrn_reflns_av_R_equivalents     0.016
_diffrn_reflns_theta_min     ?
_diffrn_reflns_theta_max     27.5
_diffrn_reflns_theta_full     27.5
_diffrn_measured_fraction_theta_max     1.0
_diffrn_measured_fraction_theta_full     1.0
_diffrn_reflns_limit_h_min     -7
_diffrn_reflns_limit_h_max     17
_diffrn_reflns_limit_k_min     0
_diffrn_reflns_limit_k_max     27
_diffrn_reflns_limit_l_min     -11
_diffrn_reflns_limit_l_max     4
_diffrn_standards_number     3
_diffrn_standards_interval_count     150
_diffrn_standards_decay_%     0.8
_refine_special_details
;
Refinement using reflections with F² > 0.0 sigma(F²). The weighted
R-factor
(wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to
zero
for negative F. The threshold expression of F² > 2.0 sigma(F²) is used
only
for calculating R-factor (gt).
;
_reflns_number_total     3419
_reflns_number_gt     2443
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_R_factor_gt     0.0422
_refine_ls_wR_factor_ref     0.1258
_refine_ls_goodness_of_fit_ref     1.017
_refine_ls_number_reflns     3419
_refine_ls_number_parameters     326
_refine_ls_hydrogen_treatment     noref
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
         'w = 1/[σ²(Fo²) + (0.0632P)²+0.271P] where P = (Fo²+2Fc²)/3'
_refine_ls_shift/su_max     0.002
_refine_diff_density_max     0.20
_refine_diff_density_min     -0.17
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
_refine_ls_abs_structure_details     'see text'
_refine_ls_abs_structure_Flack     ?
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'C' 'C' 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
    'H' 'H' 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
    'O' 'O' 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
_computing_data_collection
; WinAFC Diffractometer Control Software (Rigaku, 1999)
;
_computing_cell_refinement
; WinAFC Diffractometer Control Software
;
_computing_data_reduction
;TEXSAN (Molecular Structure Corporation, 2001)
;
_computing_structure_solution
;SIR92 (Altomare et al., 1994)
;
_computing_structure_refinement
;SHELXL97 (Sheldrick, 1997)
;
_computing_molecular_graphics     'ORTEPII (Johnson, 1976)'
_computing_publication_material     'TEXSAN'
loop_
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    O1 0.4180(2) 0.28200(10)
                           0.3995(3) 0.0664(6) Uani d . 1.00 . . O
    O2 0.4702(2) 0.18330(10)
                           0.3851(2) 0.0613(6) Uani d . 1.00 . . O
    O3 0.3901(2) 0.2148(2) 0.5844(3) 0.0860(8) Uani d . 1.00 . . O
    O4 0.6455(2) 0.23270(10)
                           -0.1698(3) 0.0588(6) Uani d . 1.00 . . O
    O5 0.59920(10)
                 0.10974(9) -0.2254(2) 0.0433(4) Uani d . 1.00 . . O
    O6 0.33860(10)
                 0.11548(9) 0.2367(2) 0.0520(5) Uani d . 1.00 . . O
    O7 0.2929(2) 0.01400(10)
                           0.3211(3) 0.0724(7) Uani d . 1.00 . . O
    C8 0.4230(3) 0.2259(2) 0.4671(4) 0.0622(8) Uani d . 1.00 . . C
    C9 0.4620(2) 0.27950(10)
                           0.2537(3) 0.0491(6) Uani d . 1.00 . . C
    C10 0.4998(2) 0.20980(10)
                            0.2455(3) 0.0443(6) Uani d . 1.00 . . C
    C11 0.5534(2) 0.22930(10)
                            -0.0973(3) 0.0424(6) Uani d . 1.00 . . C
    C12 0.5327(2) 0.29770(10)
                            -0.0357(3) 0.0468(6) Uani d . 1.00 . . C
    C13 0.4212(2) 0.30630(10)
                            -0.0075(4) 0.0540(7) Uani d . 1.00 . . C
    C14 0.3824(2) 0.29480(10)
                            0.1479(4) 0.0530(7) Uani d . 1.00 . . C
    C15 0.5961(2) 0.31570(10)
                            0.0968(4) 0.0530(7) Uani d . 1.00 . . C
    C16 0.5471(2) 0.3270(2) 0.2451(4) 0.0627(8) Uani d . 1.00 . . C
    C17 0.5548(3) 0.3438(2) -0.1628(4) 0.0699(10) Uani d . 1.00 . . C
    C18 0.6917(2) 0.3225(2) 0.0812(5) 0.0790(10)
                                               Uani d . 1.00 . . C
    C19 0.5090(3) 0.3966(2) 0.2480(6) 0.0910(10)
                                               Uani d . 1.00 . . C
    C20 0.6153(3) 0.3187(3) 0.3753(5) 0.0950(10)
                                               Uani d . 1.00 . . C
    C21 0.4679(2) 0.16780(10)
                            0.1152(3) 0.0363(5) Uani d . 1.00 . . C
    C22 0.4318(2) 0.10250(10)
                            0.1712(3) 0.0437(6) Uani d . 1.00 . . C
    C23 0.4185(2) 0.05340(10)
                            0.0515(3) 0.0488(7) Uani d . 1.00 . . C
    C24 0.5082(2) 0.04920(10)
                            -0.0441(3) 0.0477(6) Uani d . 1.00 . . C
    C25 0.5237(2) 0.11310(10)
                            -0.1149(3) 0.0399(5) Uani d . 1.00 . . C
    C26 0.5502(2) 0.16600(10)
                            -0.0034(3) 0.0368(5) Uani d . 1.00 . . C
    C27 0.6497(2) 0.1502(2) 0.0652(3) 0.0487(7) Uani d . 1.00 . . C
    C28 0.5638(2) 0.0862(2) -0.3620(3) 0.0586(8) Uani d . 1.00 . . C
    C29 0.6463(2) 0.07910(10)
                            -0.4679(3) 0.0477(6) Uani d . 1.00 . . C
    C30 0.6585(3) 0.0233(2) -0.5438(4) 0.0707(10) Uani d . 1.00 . . C
    C31 0.7316(4) 0.0159(2) -0.6453(5) 0.0880(10)
                                                Uani d . 1.00 . . C
    C32 0.7953(3) 0.0644(2) -0.6707(4) 0.0770(10)
                                                Uani d . 1.00 . . C
    C33 0.7848(3) 0.1201(2) -0.5976(4) 0.0780(10)
                                                Uani d . 1.00 . . C
    C34 0.7105(3) 0.1276(2) -0.4969(4) 0.0647(9) Uani d . 1.00 . . C
    C35 0.3150(3) 0.0771(2) 0.3575(4) 0.0696(10) Uani d . 1.00 . . C
    C36 0.2085(3) 0.0077(2) 0.2331(6) 0.0850(10)
                                               Uani d . 1.00 . . C
    H4 0.6572 0.1986 -0.2095 0.0588 Uiso calc . 1.00 . . H
    H10 0.5689 0.2115 0.2450 0.0530 Uiso calc . 1.00 . . H
    H11 0.5072 0.2231 -0.1732 0.0502 Uiso calc . 1.00 . . H
    H13A 0.4053 0.3489 -0.0331 0.0641 Uiso calc . 1.00 . . H
    H13B 0.3882 0.2778 -0.0708 0.0641 Uiso calc . 1.00 . . H
    H14A 0.3378 0.2603 0.1455 0.0626 Uiso calc . 1.00 . . H
    H14B 0.3498 0.3321 0.1805 0.0626 Uiso calc . 1.00 . . H
    H17A 0.6221 0.3415 -0.1866 0.0835 Uiso calc . 1.00 . . H
    H17B 0.5173 0.3322 -0.2459 0.0835 Uiso calc . 1.00 . . H
    H17C 0.5390 0.3859 -0.1340 0.0835 Uiso calc . 1.00 . . H
    H18A 0.7305 0.3345 0.1631 0.0949 Uiso calc . 1.00 . . H
    H18B 0.7214 0.3153 -0.0111 0.0949 Uiso calc . 1.00 . . H
    H19A 0.5618 0.4250 0.2331 0.1083 Uiso calc . 1.00 . . H
    H19B 0.4625 0.4022 0.1722 0.1083 Uiso calc . 1.00 . . H
    H19C 0.4797 0.4050 0.3400 0.1083 Uiso calc . 1.00 . . H
    H20A 0.6414 0.2768 0.3748 0.1136 Uiso calc . 1.00 . . H
    H20B 0.6669 0.3486 0.3692 0.1136 Uiso calc . 1.00 . . H
    H20C 0.5803 0.3252 0.4640 0.1136 Uiso calc . 1.00 . . H
    H21 0.4136 0.1882 0.0716 0.0430 Uiso calc . 1.00 . . H
    H22 0.4753 0.0868 0.2436 0.0522 Uiso calc . 1.00 . . H
    H23A 0.4070 0.0131 0.0951 0.0582 Uiso calc . 1.00 . . H
    H23B 0.3646 0.0650 -0.0074 0.0582 Uiso calc . 1.00 . . H
    H24A 0.5632 0.0382 0.0138 0.0570 Uiso calc . 1.00 . . H
    H24B 0.4990 0.0176 -0.1176 0.0570 Uiso calc . 1.00 . . H
    H25 0.4649 0.1249 -0.1617 0.0480 Uiso calc . 1.00 . . H
    H27A 0.6458 0.1104 0.1144 0.0580 Uiso calc . 1.00 . . H
    H27B 0.6975 0.1479 -0.0095 0.0580 Uiso calc . 1.00 . . H
    H27C 0.6669 0.1824 0.1333 0.0580 Uiso calc . 1.00 . . H
    H28A 0.5336 0.0461 -0.3473 0.0701 Uiso calc . 1.00 . . H
    H28B 0.5175 0.1153 -0.4008 0.0701 Uiso calc . 1.00 . . H
    H30 0.6154 -0.0112 -0.5254 0.0844 Uiso calc . 1.00 . . H
    H31 0.7375 -0.0228 -0.6982 0.1046 Uiso calc . 1.00 . . H
    H32 0.8471 0.0590 -0.7387 0.0920 Uiso calc . 1.00 . . H
    H33 0.8286 0.1540 -0.6154 0.0932 Uiso calc . 1.00 . . H
    H34 0.7037 0.1670 -0.4468 0.0776 Uiso calc . 1.00 . . H
    H35A 0.3690 0.0769 0.4228 0.0828 Uiso calc . 1.00 . . H
    H35B 0.2603 0.0951 0.4054 0.0828 Uiso calc . 1.00 . . H
    H36A 0.1538 0.0239 0.2848 0.1031 Uiso calc . 1.00 . . H
    H36B 0.2169 0.0311 0.1449 0.1031 Uiso calc . 1.00 . . H
    H36C 0.1981 -0.0358 0.2106 0.1031 Uiso calc . 1.00 . . H
_geom_special_details
;
 ?
;
loop_
    _geom_bond_atom_site_label_1
    _geom_bond_atom_site_label_2
    _geom_bond_site_symmetry_1
    _geom_bond_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    O1 C8 . . 1.333(4) ?
    O1 C9 . . 1.462(4) ?
    O2 C8 . . 1.334(4) ?
    O2 C10 . . 1.449(4) ?
    O3 C8 . . 1.186(4) ?
    O4 C11 . . 1.431(3) ?
    O4 H4 . . 0.820 no
    O5 C25 . . 1.449(3) ?
    O5 C28 . . 1.427(4) ?
    O6 C22 . . 1.441(3) ?
    O6 C35 . . 1.405(4) ?
    O7 C35 . . 1.400(5) ?
    O7 C36 . . 1.418(5) ?
    C9 C10 . . 1.556(4) yes
    C9 C14 . . 1.495(4) yes
    C9 C16 . . 1.542(4) yes
    C10 C21 . . 1.545(4) yes
    C10 H10 . . 0.951 no
    C11 C12 . . 1.571(4) yes
    C11 C26 . . 1.582(4) yes
    C11 H11 . . 0.949 no
    C12 C13 . . 1.566(4) yes
    C12 C15 . . 1.538(4) yes
    C12 C17 . . 1.542(5) ?
    C13 C14 . . 1.535(5) yes
    C13 H13A . . 0.950 no
    C13 H13B . . 0.948 no
    C14 H14A . . 0.950 no
    C14 H14B . . 0.950 no
    C15 C16 . . 1.531(5) yes
    C15 C18 . . 1.331(4) ?
    C16 C19 . . 1.554(5) ?
    C16 C20 . . 1.525(6) ?
    C17 H17A . . 0.951 no
    C17 H17B . . 0.949 no
    C17 H17C . . 0.950 no
    C18 H18A . . 0.952 no
    C18 H18B . . 0.948 no
    C19 H19A . . 0.950 no
    C19 H19B . . 0.950 no
    C19 H19C . . 0.949 no
    C20 H20A . . 0.952 no
    C20 H20B . . 0.949 no
    C20 H20C . . 0.951 no
    C21 C22 . . 1.545(4) yes
    C21 C26 . . 1.567(3) yes
    C21 H21 . . 0.950 no
    C22 C23 . . 1.515(4) yes
    C22 H22 . . 0.951 no
    C23 C24 . . 1.514(4) yes
    C23 H23A . . 0.948 no
    C23 H23B . . 0.948 no
    C24 C25 . . 1.507(4) yes
    C24 H24A . . 0.950 no
    C24 H24B . . 0.952 no
    C25 C26 . . 1.552(4) yes
    C25 H25 . . 0.948 no
    C26 C27 . . 1.542(4) ?
    C27 H27A . . 0.950 no
    C27 H27B . . 0.948 no
    C27 H27C . . 0.950 no
    C28 C29 . . 1.498(4) ?
    C28 H28A . . 0.950 no
    C28 H28B . . 0.951 no
    C29 C30 . . 1.374(4) ?
    C29 C34 . . 1.375(5) ?
    C30 C31 . . 1.376(6) ?
    C30 H30 . . 0.951 no
    C31 C32 . . 1.363(7) ?
    C31 H31 . . 0.951 no
    C32 C33 . . 1.356(7) ?
    C32 H32 . . 0.952 no
    C33 C34 . . 1.384(5) ?
    C33 H33 . . 0.948 no
    C34 H34 . . 0.949 no
    C35 H35A . . 0.952 no
    C35 H35B . . 0.949 no
    C36 H36A . . 0.951 no
    C36 H36B . . 0.950 no
    C36 H36C . . 0.950 no
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_2
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    C8 O1 C9 . . . 111.6(2) ?
    C8 O2 C10 . . . 111.8(2) ?
    C11 O4 H4 . . . 109.5 no
    C25 O5 C28 . . . 112.4(2) ?
    C22 O6 C35 . . . 115.1(2) ?
    C35 O7 C36 . . . 113.6(3) ?
    O1 C8 O2 . . . 111.0(3) ?
    O1 C8 O3 . . . 124.9(4) ?
    O2 C8 O3 . . . 124.1(4) ?
    O1 C9 C10 . . . 102.5(2) ?
    O1 C9 C14 . . . 106.1(2) ?
    O1 C9 C16 . . . 109.7(3) ?
    C10 C9 C14 . . . 114.6(2) ?
    C10 C9 C16 . . . 110.7(2) ?
    C14 C9 C16 . . . 112.5(3) ?
    O2 C10 C9 . . . 103.0(2) ?
    O2 C10 C21 . . . 112.1(2) ?
    O2 C10 H10 . . . 107.4 no
    C9 C10 C21 . . . 118.7(2) ?
    C9 C10 H10 . . . 107.4 no
    C21 C10 H10 . . . 107.5 no
    O4 C11 C12 . . . 106.2(2) ?
    O4 C11 C26 . . . 108.6(2) ?
    O4 C11 H11 . . . 105.2 no
    C12 C11 C26 . . . 124.8(2) ?
    C12 C11 H11 . . . 105.3 no
    C26 C11 H11 . . . 105.2 no
    C11 C12 C13 . . . 110.0(2) ?
    C11 C12 C15 . . . 113.8(2) ?
    C11 C12 C17 . . . 105.7(2) ?
    C13 C12 C15 . . . 113.4(3) ?
    C13 C12 C17 . . . 104.2(3) ?
    C15 C12 C17 . . . 109.0(2) ?
    C12 C13 C14 . . . 118.3(3) ?
    C12 C13 H13A . . . 107.1 no
    C12 C13 H13B . . . 107.2 no
    C14 C13 H13A . . . 107.2 no
    C14 C13 H13B . . . 107.3 no
    H13A C13 H13B . . . 109.6 no
    C9 C14 C13 . . . 112.1(2) ?
    C9 C14 H14A . . . 108.8 no
    C9 C14 H14B . . . 108.8 no
    C13 C14 H14A . . . 108.8 no
    C13 C14 H14B . . . 108.9 no
    H14A C14 H14B . . . 109.4 no
    C12 C15 C16 . . . 118.9(3) ?
    C12 C15 C18 . . . 120.2(3) ?
    C16 C15 C18 . . . 120.8(3) ?
    C9 C16 C15 . . . 106.2(3) ?
    C9 C16 C19 . . . 110.7(3) ?
    C9 C16 C20 . . . 110.7(3) ?
    C15 C16 C19 . . . 108.0(3) ?
    C15 C16 C20 . . . 113.6(3) ?
    C19 C16 C20 . . . 107.6(3) ?
    C12 C17 H17A . . . 109.4 no
    C12 C17 H17B . . . 109.5 no
    C12 C17 H17C . . . 109.4 no
    H17A C17 H17B . . . 109.5 no
    H17A C17 H17C . . . 109.4 no
    H17B C17 H17C . . . 109.6 no
    C15 C18 H18A . . . 119.9 no
    C15 C18 H18B . . . 120.1 no
    H18A C18 H18B . . . 120.0 no
    C16 C19 H19A . . . 109.4 no
    C16 C19 H19B . . . 109.3 no
    C16 C19 H19C . . . 109.5 no
    H19A C19 H19B . . . 109.5 no
    H19A C19 H19C . . . 109.6 no
    H19B C19 H19C . . . 109.6 no
    C16 C20 H20A . . . 109.5 no
    C16 C20 H20B . . . 109.8 no
    C16 C20 H20C . . . 109.6 no
    H20A C20 H20B . . . 109.4 no
    H20A C20 H20C . . . 109.2 no
    H20B C20 H20C . . . 109.4 no
    C10 C21 C22 . . . 110.2(2) ?
    C10 C21 C26 . . . 109.9(2) ?
    C10 C21 H21 . . . 106.7 no
    C22 C21 C26 . . . 116.1(2) ?
    C22 C21 H21 . . . 106.7 no
    C26 C21 H21 . . . 106.8 no
    O6 C22 C21 . . . 104.8(2) ?
    O6 C22 C23 . . . 108.7(2) ?
    O6 C22 H22 . . . 109.7 no
    C21 C22 C23 . . . 114.0(2) ?
    C21 C22 H22 . . . 109.7 no
    C23 C22 H22 . . . 109.8 no
    C22 C23 C24 . . . 110.9(2) ?
    C22 C23 H23A . . . 109.1 no
    C22 C23 H23B . . . 109.0 no
    C24 C23 H23A . . . 109.0 no
    C24 C23 H23B . . . 109.0 no
    H23A C23 H23B . . . 109.7 no
    C23 C24 C25 . . . 108.1(2) ?
    C23 C24 H24A . . . 110.0 no
    C23 C24 H24B . . . 109.7 no
    C25 C24 H24A . . . 110.0 no
    C25 C24 H24B . . . 109.8 no
    H24A C24 H24B . . . 109.3 no
    O5 C25 C24 . . . 110.9(2) ?
    O5 C25 C26 . . . 108.9(2) ?
    O5 C25 H25 . . . 108.1 no
    C24 C25 C26 . . . 113.1(2) ?
    C24 C25 H25 . . . 107.9 no
    C26 C25 H25 . . . 107.9 no
    C11 C26 C21 . . . 112.0(2) ?
    C11 C26 C25 . . . 104.7(2) ?
    C11 C26 C27 . . . 112.1(2) ?
    C21 C26 C25 . . . 107.5(2) ?
    C21 C26 C27 . . . 111.4(2) ?
    C25 C26 C27 . . . 108.6(2) ?
    C26 C27 H27A . . . 109.4 no
    C26 C27 H27B . . . 109.5 no
    C26 C27 H27C . . . 109.4 no
    H27A C27 H27B . . . 109.6 no
    H27A C27 H27C . . . 109.4 no
    H27B C27 H27C . . . 109.6 no
    O5 C28 C29 . . . 109.9(2) ?
    O5 C28 H28A . . . 109.4 no
    O5 C28 H28B . . . 109.3 no
    C29 C28 H28A . . . 109.4 no
    C29 C28 H28B . . . 109.4 no
    H28A C28 H28B . . . 109.3 no
    C28 C29 C30 . . . 120.2(3) ?
    C28 C29 C34 . . . 122.4(3) ?
    C30 C29 C34 . . . 117.3(3) ?
    C29 C30 C31 . . . 121.7(3) ?
    C29 C30 H30 . . . 119.1 no
    C31 C30 H30 . . . 119.3 no
    C30 C31 C32 . . . 120.0(4) ?
    C30 C31 H31 . . . 120.0 no
    C32 C31 H31 . . . 119.9 no
    C31 C32 C33 . . . 119.5(4) ?
    C31 C32 H32 . . . 120.3 no
    C33 C32 H32 . . . 120.2 no
    C32 C33 C34 . . . 120.4(4) ?
    C32 C33 H33 . . . 119.8 no
    C34 C33 H33 . . . 119.8 no
    C29 C34 C33 . . . 121.1(3) ?
    C29 C34 H34 . . . 119.4 no
    C33 C34 H34 . . . 119.5 no
    O6 C35 O7 . . . 114.1(3) ?
    O6 C35 H35A . . . 108.2 no
    O6 C35 H35B . . . 108.3 no
    O7 C35 H35A . . . 108.4 no
    O7 C35 H35B . . . 108.5 no
    H35A C35 H35B . . . 109.3 no
    O7 C36 H36A . . . 109.4 no
    O7 C36 H36B . . . 109.5 no
    O7 C36 H36C . . . 109.5 no
    H36A C36 H36B . . . 109.4 no
    H36A C36 H36C . . . 109.4 no
    H36B C36 H36C . . . 109.5 no
loop_
    _geom_torsion_atom_site_label_1
    _geom_torsion_atom_site_label_2
    _geom_torsion_atom_site_label_3
    _geom_torsion_atom_site_label_4
    _geom_torsion_site_symmetry_1
    _geom_torsion_site_symmetry_2
    _geom_torsion_site_symmetry_3
    _geom_torsion_site_symmetry_4
    _geom_torsion
    _geom_torsion_publ_flag
    O1 C8 O2 C10 . . . . -1.5(4) ?
    O1 C9 C10 O2 . . . . 1.1(3) ?
    O1 C9 C10 C21 . . . . 125.7(2) ?
    O1 C9 C14 C13 . . . . 169.3(2) ?
    O1 C9 C16 C15 . . . . 173.4(2) ?
    O1 C9 C16 C19 . . . . -69.6(4) ?
    O1 C9 C16 C20 . . . . 49.6(4) ?
    O2 C8 O1 C9 . . . . 2.3(4) ?
    O2 C10 C9 C14 . . . . -113.4(3) ?
    O2 C10 C9 C16 . . . . 118.0(3) ?
    O2 C10 C21 C22 . . . . -11.5(3) ?
    O2 C10 C21 C26 . . . . -140.7(2) ?
    O3 C8 O1 C9 . . . . -177.6(3) ?
    O3 C8 O2 C10 . . . . 178.4(3) ?
    O4 C11 C12 C13 . . . . 158.9(2) ?
    O4 C11 C12 C15 . . . . -72.6(3) ?
    O4 C11 C12 C17 . . . . 47.0(3) ?
    O4 C11 C26 C21 . . . . 162.6(2) ?
    O4 C11 C26 C25 . . . . -81.2(2) ?
    O4 C11 C26 C27 . . . . 36.4(3) ?
    O5 C25 C24 C23 . . . . -171.0(2) ?
    O5 C25 C26 C11 . . . . 61.4(2) ?
    O5 C25 C26 C21 . . . . -179.3(2) ?
    O5 C25 C26 C27 . . . . -58.6(3) ?
    O5 C28 C29 C30 . . . . 130.1(3) ?
    O5 C28 C29 C34 . . . . -51.9(4) ?
    O6 C22 C21 C10 . . . . 73.2(2) ?
    O6 C22 C21 C26 . . . . -161.2(2) ?
    O6 C22 C23 C24 . . . . 166.8(2) ?
    O6 C35 O7 C36 . . . . -64.1(4) no
    O7 C35 O6 C22 . . . . -71.9(3) no
    C8 O1 C9 C10 . . . . -2.0(3) ?
    C8 O1 C9 C14 . . . . 118.5(3) ?
    C8 O1 C9 C16 . . . . -119.7(3) ?
    C8 O2 C10 C9 . . . . 0.2(3) ?
    C8 O2 C10 C21 . . . . -128.6(3) ?
    C9 C10 C21 C22 . . . . -131.6(2) ?
    C9 C10 C21 C26 . . . . 99.3(3) no
    C9 C14 C13 C12 . . . . 2.8(4) yes
    C9 C16 C15 C12 . . . . 35.4(4) yes
    C9 C16 C15 C18 . . . . -146.0(3) ?
    C10 C9 C14 C13 . . . . -78.3(3) no
    C10 C9 C16 C15 . . . . 61.1(3) no
    C10 C9 C16 C19 . . . . 178.1(3) ?
    C10 C9 C16 C20 . . . . -62.7(4) ?
    C10 C21 C22 C23 . . . . -168.1(2) ?
    C10 C21 C26 C11 . . . . -76.8(2) no
    C10 C21 C26 C25 . . . . 168.7(2) ?
    C10 C21 C26 C27 . . . . 49.8(3) ?
    C11 C12 C13 C14 . . . . 96.0(3) no
    C11 C12 C15 C16 . . . . -115.4(3) no
    C11 C12 C15 C18 . . . . 66.1(4) ?
    C11 C26 C21 C22 . . . . 157.4(2) ?
    C11 C26 C25 C24 . . . . -174.9(2) ?
    C12 C11 C26 C21 . . . . 36.3(3) no
    C12 C11 C26 C25 . . . . 152.5(2) ?
    C12 C11 C26 C27 . . . . -89.9(3) ?
    C12 C15 C16 C19 . . . . -83.4(3) ?
    C12 C15 C16 C20 . . . . 157.4(3) ?
    C13 C12 C11 C26 . . . . -73.8(3) no
    C13 C12 C15 C16 . . . . 11.4(4) ?
    C13 C12 C15 C18 . . . . -167.1(3) ?
    C13 C14 C9 C16 . . . . 49.3(3) ?
    C14 C9 C10 C21 . . . . 11.2(4) no
    C14 C9 C16 C15 . . . . -68.7(3) ?
    C14 C9 C16 C19 . . . . 48.3(4) ?
    C14 C9 C16 C20 . . . . 167.5(3) ?
    C14 C13 C12 C15 . . . . -32.7(3) ?
    C14 C13 C12 C17 . . . . -151.1(3) ?
    C15 C12 C11 C26 . . . . 54.7(3) no
    C16 C9 C10 C21 . . . . -117.4(3) no
    C16 C15 C12 C17 . . . . 126.9(3) ?
    C17 C12 C11 C26 . . . . 174.3(2) ?
    C17 C12 C15 C18 . . . . -51.6(4) ?
    C18 C15 C16 C19 . . . . 95.2(4) ?
    C18 C15 C16 C20 . . . . -24.1(5) ?
    C21 C22 O6 C35 . . . . -147.2(2) ?
    C21 C22 C23 C24 . . . . 50.3(3) ?
    C21 C26 C25 C24 . . . . -55.6(3) ?
    C22 C21 C26 C25 . . . . 42.9(3) ?
    C22 C21 C26 C27 . . . . -76.0(3) ?
    C22 C23 C24 C25 . . . . -61.2(3) ?
    C23 C22 O6 C35 . . . . 90.6(3) ?
    C23 C22 C21 C26 . . . . -42.4(3) ?
    C23 C24 C25 C26 . . . . 66.4(3) ?
    C24 C25 O5 C28 . . . . 82.2(3) ?
    C24 C25 C26 C27 . . . . 65.1(3) ?
    C25 O5 C28 C29 . . . . -175.6(2) no
    C26 C25 O5 C28 . . . . -152.8(2) ?
    C28 C29 C30 C31 . . . . 177.8(4) ?
    C28 C29 C34 C33 . . . . -178.6(3) ?
    C29 C30 C31 C32 . . . . 1.3(6) ?
    C29 C34 C33 C32 . . . . 0.4(5) ?
    C30 C29 C34 C33 . . . . -0.6(5) ?
    C30 C31 C32 C33 . . . . -1.4(6) ?
    C31 C30 C29 C34 . . . . -0.3(5) ?
    C31 C32 C33 C34 . . . . 0.6(6) ?
    C31 C32 C33 C34 . . . . 0.6(6) ?
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_D
    _geom_hbond_site_symmetry_H
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    _geom_hbond_publ_flag
    O4 H4 O5 . . . 0.82 2.04 2.711(2) 139 yes
