##############################################################################
#                                                                            #
# This CIF contains the data for a data article accepted for                 #
# publication in IUCrData. It conforms to the requirements of                #
# Notes for Authors for IUCrData, and has been                               #
# peer reviewed under the auspices of IUCrData.                              #
#                                                                            #
# 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.                                       #
#                                                                            #
# Software is freely available for graphical display of the structure(s)     #
# in this CIF. For information consult the CIF software page                 #
# http://www.iucr.org/resources/cif/software.                                #
#                                                                            #
# This file may be used for bona fide research purposes within the           #
# scientific community so long as proper attribution is given to the data    # 
# article from which it was obtained.                                        #
#                                                                            #
##############################################################################
data_I
_audit_creation_method     'SHELXL-2014/7'
_journal_date_recd_electronic     2019-07-10
_journal_date_accepted     2019-07-16
_journal_name_full     'IUCrData'
_journal_year     2019
_journal_volume     4
_journal_issue      7
_journal_page_first     0
_journal_page_last     0
_journal_paper_category     HO
_journal_paper_doi     10.1107/S2414314619010186
_journal_coeditor_code     HB4307
_publ_contact_author_name     'Amely Täufer'
_publ_contact_author_address
;
Leibniz-Institut für Katalyse e. V. an der Universität Rostock
Albert-Einstein-Str. 29a
18059 Rostock
Germany
;
_publ_contact_author_email     'amely.taeufer@catalysis.de'
_publ_contact_author_fax     '+49 381 1281 5000'
_publ_contact_author_phone     '+493811281188'
_publ_section_title
;\
8,13-Diisopropyl-10,11-dimethyl-bis([1,3]dioxolo[4',5':6,7]naphtho)\
[1,2-d;2,1-f][1,3]dioxepine
;
loop_
    _publ_author_name
    _publ_author_footnote
    _publ_author_address
    'Täufer, Amely' .
;
Leibniz-Institut für Katalyse e. V. an der Universität Rostock
Albert-Einstein-Str. 29a
18059 Rostock
Germany
;
    'Köckritz, Angela' .
;
Leibniz-Institut für Katalyse e. V. an der Universität Rostock
Albert-Einstein-Str. 29a
18059 Rostock
Germany
;
    'Quint, Stephan' .
;
Chiracon GmbH
Im Biotechnologiepark 9
14943 Luckenwalde
Germany
;
    'Spannenberg, Anke' .
;
Leibniz-Institut für Katalyse e. V. an der Universität Rostock
Albert-Einstein-Str. 29a
18059 Rostock
Germany
;
_publ_section_synopsis
;
The title compound C₃₁H₃₀O₆ contains a bridging dioxepine unit which
hinders the rotation around the 2,2'-internaphthyl bond.
;
_database_code_depnum_ccdc_archive     'CCDC 1940900'
_chemical_name_systematic
;\
8,13-Diisopropyl-10,11-dimethyl-bis([1,3]dioxolo[4',5':6,7]naphtho)\
[1,2-d;2,1-f][1,3]dioxepine
;
_chemical_name_common     ?
_chemical_formula_moiety     'C31 H30 O6'
_chemical_formula_sum     'C31 H30 O6'
_chemical_formula_iupac     'C31 H30 O6'
_chemical_formula_weight     498.55
_chemical_melting_point     ?
_space_group_crystal_system     triclinic
_space_group_name_H-M_alt     'P -1'
_space_group_name_Hall     '-P 1'
loop_
    _space_group_symop_operation_xyz
    'x, y, z'
    '-x, -y, -z'
_cell_length_a     9.7053(6)
_cell_length_b     11.0901(7)
_cell_length_c     12.4156(8)
_cell_angle_alpha     68.0282(16)
_cell_angle_beta     81.7012(16)
_cell_angle_gamma     86.4672(16)
_cell_volume     1226.25(13)
_cell_formula_units_Z     2
_cell_measurement_reflns_used     9929
_cell_measurement_theta_min     2.82
_cell_measurement_theta_max     30.56
_cell_measurement_temperature     150(2)
_exptl_crystal_description     'part of a plate'
_exptl_crystal_colour     orange
_exptl_crystal_size_max     0.460
_exptl_crystal_size_mid     0.325
_exptl_crystal_size_min     0.184
_exptl_crystal_density_diffrn     1.350
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     ?
_exptl_crystal_F_000     528
_exptl_absorpt_coefficient_mu     0.093
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_absorpt_correction_T_min     0.95
_exptl_absorpt_correction_T_max     0.98
_diffrn_ambient_temperature     150(2)
_diffrn_source     'fine-focus sealed tube'
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type     'Bruker APEXII CCD'
_diffrn_measurement_method     'φ and ω scans'
_diffrn_detector_area_resol_mean     8.3333
_diffrn_reflns_number     43308
_diffrn_reflns_av_R_equivalents     0.0231
_diffrn_reflns_av_unetI/netI     0.0135
_diffrn_reflns_theta_min     1.784
_diffrn_reflns_theta_max     27.999
_diffrn_reflns_theta_full     25.242
_diffrn_measured_fraction_theta_max     1.000
_diffrn_measured_fraction_theta_full     1.000
_diffrn_reflns_limit_h_min     -12
_diffrn_reflns_limit_h_max     12
_diffrn_reflns_limit_k_min     -14
_diffrn_reflns_limit_k_max     14
_diffrn_reflns_limit_l_min     -16
_diffrn_reflns_limit_l_max     16
_refine_special_details
;
All H atoms were placed in idealized positions with d(C---H) =
0.95--1.00 Å (CH), 0.99 (CH₂), 0.98 Å (CH₃) and refined using a riding
model with Uiso(H) fixed at 1.2 Ueq(C) for CH, CH₂ and 1.5
Ueq(C) for CH₃.
;
_reflns_number_total     5923
_reflns_number_gt     4941
_reflns_threshold_expression     'I > 2σ(I)'
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all     0.0539
_refine_ls_R_factor_gt     0.0454
_refine_ls_wR_factor_gt     0.1272
_refine_ls_wR_factor_ref     0.1375
_refine_ls_goodness_of_fit_ref     1.052
_refine_ls_restrained_S_all     1.052
_refine_ls_number_reflns     5923
_refine_ls_number_parameters     340
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
              'w=1/[σ²(Fo²)+(0.0747P)²+0.4119P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary     ?
_refine_ls_shift/su_max     0.000
_refine_ls_shift/su_mean     0.000
_refine_diff_density_max     0.503
_refine_diff_density_min     -0.237
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     .
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'
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014/7 (Sheldrick, 2015)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
loop_
    _atom_site_type_symbol
    _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_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    C C1 0.82699(13) 0.25631(12) 0.23443(11) 0.0250(3) Uani d 1 . .
    C C2 0.76549(13) 0.22345(11) 0.34917(11) 0.0241(2) Uani d 1 . .
    C C3 0.61762(13) 0.21611(12) 0.37149(11) 0.0261(3) Uani d 1 . .
    C C4 0.54302(13) 0.23621(12) 0.27978(11) 0.0264(3) Uani d 1 . .
    H H4 0.4443 0.2325 0.2958 0.032 Uiso calc 1 . .
    C C5 0.60517(13) 0.26203(12) 0.16310(11) 0.0252(3) Uani d 1 . .
    C C6 0.52512(14) 0.27466(12) 0.06984(12) 0.0279(3) Uani d 1 . .
    C C7 0.60147(14) 0.29242(13) -0.03592(12) 0.0310(3) Uani d 1 . .
    C C8 0.74758(15) 0.30407(14) -0.05803(12) 0.0316(3) Uani d 1 . .
    C C9 0.82598(14) 0.29600(13) 0.02588(11) 0.0288(3) Uani d 1 . .
    H H9 0.9243 0.3051 0.0098 0.035 Uiso calc 1 . .
    C C10 0.75335(13) 0.27314(11) 0.13981(11) 0.0248(3) Uani d 1 . .
    C C11 0.94951(13) 0.31227(12) 0.41291(11) 0.0241(2) Uani d 1 . .
    C C12 0.85840(13) 0.21138(12) 0.43837(11) 0.0240(2) Uani d 1 . .
    C C13 0.86743(13) 0.10115(12) 0.54305(11) 0.0258(3) Uani d 1 . .
    C C14 0.96098(14) 0.10164(12) 0.61658(11) 0.0272(3) Uani d 1 . .
    H H14 0.9651 0.0277 0.6866 0.033 Uiso calc 1 . .
    C C15 1.05123(13) 0.20650(12) 0.59326(11) 0.0249(3) Uani d 1 . .
    C C16 1.14992(14) 0.20510(12) 0.67065(11) 0.0265(3) Uani d 1 . .
    C C17 1.22813(13) 0.31411(12) 0.63546(11) 0.0266(3) Uani d 1 . .
    C C18 1.22056(13) 0.42122(12) 0.53020(12) 0.0261(3) Uani d 1 . .
    C C19 1.13326(13) 0.42565(12) 0.45361(11) 0.0265(3) Uani d 1 . .
    H H19 1.1302 0.4978 0.3821 0.032 Uiso calc 1 . .
    C C20 1.04574(13) 0.31570(12) 0.48625(11) 0.0239(2) Uani d 1 . .
    C C21 0.67417(17) 0.2882(2) -0.21373(14) 0.0475(4) Uani d 1 . .
    H H21A 0.6668 0.3455 -0.2959 0.057 Uiso calc 1 . .
    H H21B 0.6843 0.1971 -0.2094 0.057 Uiso calc 1 . .
    C C22 1.01188(14) 0.39371(14) 0.21042(12) 0.0324(3) Uani d 1 . .
    H H22A 1.1140 0.3928 0.2104 0.039 Uiso calc 1 . .
    H H22B 0.9894 0.4647 0.1381 0.039 Uiso calc 1 . .
    C C23 1.36283(15) 0.47149(13) 0.63326(13) 0.0329(3) Uani d 1 . .
    H H23A 1.4647 0.4831 0.6241 0.039 Uiso calc 1 . .
    H H23B 1.3167 0.5232 0.6784 0.039 Uiso calc 1 . .
    C C24 0.53967(15) 0.19488(15) 0.49121(12) 0.0334(3) Uani d 1 . .
    H H24A 0.4524 0.2450 0.4830 0.050 Uiso calc 1 . .
    H H24B 0.5969 0.2237 0.5358 0.050 Uiso calc 1 . .
    H H24C 0.5190 0.1022 0.5326 0.050 Uiso calc 1 . .
    C C25 0.36832(14) 0.25869(15) 0.08976(13) 0.0337(3) Uani d 1 . .
    H H25 0.3333 0.2680 0.1661 0.040 Uiso calc 1 . .
    C C26 0.33202(18) 0.12209(17) 0.10137(15) 0.0454(4) Uani d 1 . .
    H H26A 0.3637 0.1103 0.0273 0.068 Uiso calc 1 . .
    H H26B 0.2310 0.1104 0.1201 0.068 Uiso calc 1 . .
    H H26C 0.3781 0.0578 0.1641 0.068 Uiso calc 1 . .
    C C27 0.29569(16) 0.36318(17) -0.00509(15) 0.0431(4) Uani d 1 . .
    H H27A 0.3218 0.4495 -0.0107 0.065 Uiso calc 1 . .
    H H27B 0.1946 0.3532 0.0152 0.065 Uiso calc 1 . .
    H H27C 0.3242 0.3538 -0.0806 0.065 Uiso calc 1 . .
    C C28 0.78370(15) -0.01978(13) 0.57202(12) 0.0321(3) Uani d 1 . .
    H H28A 0.8394 -0.0967 0.6103 0.048 Uiso calc 1 . .
    H H28B 0.7583 -0.0236 0.4998 0.048 Uiso calc 1 . .
    H H28C 0.6990 -0.0176 0.6248 0.048 Uiso calc 1 . .
    C C29 1.16247(16) 0.09451(13) 0.78629(12) 0.0340(3) Uani d 1 . .
    H H29 1.1097 0.0188 0.7884 0.041 Uiso calc 1 . .
    C C30 1.31337(18) 0.05092(15) 0.80179(14) 0.0426(4) Uani d 1 . .
    H H30A 1.3551 0.0262 0.7362 0.064 Uiso calc 1 . .
    H H30B 1.3154 -0.0238 0.8755 0.064 Uiso calc 1 . .
    H H30C 1.3662 0.1225 0.8036 0.064 Uiso calc 1 . .
    C C31 1.09481(18) 0.13534(19) 0.88678(14) 0.0481(4) Uani d 1 . .
    H H31A 1.1403 0.2137 0.8828 0.072 Uiso calc 1 . .
    H H31B 1.1052 0.0649 0.9618 0.072 Uiso calc 1 . .
    H H31C 0.9956 0.1535 0.8801 0.072 Uiso calc 1 . .
    O O1 0.55313(11) 0.30220(11) -0.13812(9) 0.0404(3) Uani d 1 . .
    O O2 0.79134(11) 0.32419(12) -0.17393(9) 0.0414(3) Uani d 1 . .
    O O3 0.97105(9) 0.27298(9) 0.20978(8) 0.0295(2) Uani d 1 . .
    O O4 0.94521(9) 0.41888(8) 0.30849(8) 0.0278(2) Uani d 1 . .
    O O5 1.31535(10) 0.51336(9) 0.52047(9) 0.0330(2) Uani d 1 . .
    O O6 1.32875(11) 0.33807(9) 0.69250(9) 0.0336(2) Uani d 1 . .
_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_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    C1 C2 . 1.3825(18) ?
    C1 O3 . 1.3959(15) ?
    C1 C10 . 1.4098(17) ?
    C2 C3 . 1.4233(17) ?
    C2 C12 . 1.4900(16) ?
    C3 C4 . 1.3779(17) ?
    C3 C24 . 1.5075(18) ?
    C4 C5 . 1.4152(18) ?
    C4 H4 . 0.9500 ?
    C5 C10 . 1.4290(17) ?
    C5 C6 . 1.4453(17) ?
    C6 C7 . 1.362(2) ?
    C6 C25 . 1.5167(18) ?
    C7 O1 . 1.3801(16) ?
    C7 C8 . 1.4094(19) ?
    C8 C9 . 1.3502(18) ?
    C8 O2 . 1.3769(16) ?
    C9 C10 . 1.4241(18) ?
    C9 H9 . 0.9500 ?
    C11 C12 . 1.3821(17) ?
    C11 O4 . 1.3939(14) ?
    C11 C20 . 1.4066(17) ?
    C12 C13 . 1.4219(17) ?
    C13 C14 . 1.3789(17) ?
    C13 C28 . 1.5091(17) ?
    C14 C15 . 1.4155(17) ?
    C14 H14 . 0.9500 ?
    C15 C20 . 1.4293(17) ?
    C15 C16 . 1.4470(17) ?
    C16 C17 . 1.3604(18) ?
    C16 C29 . 1.5149(18) ?
    C17 O6 . 1.3777(15) ?
    C17 C18 . 1.4070(18) ?
    C18 C19 . 1.3479(18) ?
    C18 O5 . 1.3771(15) ?
    C19 C20 . 1.4252(17) ?
    C19 H19 . 0.9500 ?
    C21 O1 . 1.433(2) ?
    C21 O2 . 1.4362(19) ?
    C21 H21A . 0.9900 ?
    C21 H21B . 0.9900 ?
    C22 O4 . 1.4085(17) ?
    C22 O3 . 1.4226(17) ?
    C22 H22A . 0.9900 ?
    C22 H22B . 0.9900 ?
    C23 O6 . 1.4197(17) ?
    C23 O5 . 1.4362(17) ?
    C23 H23A . 0.9900 ?
    C23 H23B . 0.9900 ?
    C24 H24A . 0.9800 ?
    C24 H24B . 0.9800 ?
    C24 H24C . 0.9800 ?
    C25 C26 . 1.526(2) ?
    C25 C27 . 1.531(2) ?
    C25 H25 . 1.0000 ?
    C26 H26A . 0.9800 ?
    C26 H26B . 0.9800 ?
    C26 H26C . 0.9800 ?
    C27 H27A . 0.9800 ?
    C27 H27B . 0.9800 ?
    C27 H27C . 0.9800 ?
    C28 H28A . 0.9800 ?
    C28 H28B . 0.9800 ?
    C28 H28C . 0.9800 ?
    C29 C30 . 1.530(2) ?
    C29 C31 . 1.530(2) ?
    C29 H29 . 1.0000 ?
    C30 H30A . 0.9800 ?
    C30 H30B . 0.9800 ?
    C30 H30C . 0.9800 ?
    C31 H31A . 0.9800 ?
    C31 H31B . 0.9800 ?
    C31 H31C . 0.9800 ?
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_3
    _geom_angle
    _geom_angle_publ_flag
    C2 C1 O3 . . 118.53(11) ?
    C2 C1 C10 . . 124.07(11) ?
    O3 C1 C10 . . 117.40(11) ?
    C1 C2 C3 . . 117.75(11) ?
    C1 C2 C12 . . 117.17(11) ?
    C3 C2 C12 . . 124.79(11) ?
    C4 C3 C2 . . 119.11(11) ?
    C4 C3 C24 . . 118.90(12) ?
    C2 C3 C24 . . 121.90(11) ?
    C3 C4 C5 . . 123.69(12) ?
    C3 C4 H4 . . 118.2 ?
    C5 C4 H4 . . 118.2 ?
    C4 C5 C10 . . 117.31(11) ?
    C4 C5 C6 . . 122.60(12) ?
    C10 C5 C6 . . 120.08(12) ?
    C7 C6 C5 . . 115.21(12) ?
    C7 C6 C25 . . 121.96(12) ?
    C5 C6 C25 . . 122.65(12) ?
    C6 C7 O1 . . 127.54(13) ?
    C6 C7 C8 . . 124.16(12) ?
    O1 C7 C8 . . 108.30(12) ?
    C9 C8 O2 . . 128.09(13) ?
    C9 C8 C7 . . 122.49(12) ?
    O2 C8 C7 . . 109.42(12) ?
    C8 C9 C10 . . 116.41(12) ?
    C8 C9 H9 . . 121.8 ?
    C10 C9 H9 . . 121.8 ?
    C1 C10 C9 . . 120.48(11) ?
    C1 C10 C5 . . 117.89(11) ?
    C9 C10 C5 . . 121.59(11) ?
    C12 C11 O4 . . 118.23(11) ?
    C12 C11 C20 . . 124.36(11) ?
    O4 C11 C20 . . 117.41(10) ?
    C11 C12 C13 . . 117.62(11) ?
    C11 C12 C2 . . 116.91(11) ?
    C13 C12 C2 . . 125.32(11) ?
    C14 C13 C12 . . 119.25(11) ?
    C14 C13 C28 . . 119.01(11) ?
    C12 C13 C28 . . 121.62(11) ?
    C13 C14 C15 . . 123.47(11) ?
    C13 C14 H14 . . 118.3 ?
    C15 C14 H14 . . 118.3 ?
    C14 C15 C20 . . 117.46(11) ?
    C14 C15 C16 . . 122.87(11) ?
    C20 C15 C16 . . 119.64(11) ?
    C17 C16 C15 . . 115.30(11) ?
    C17 C16 C29 . . 121.16(11) ?
    C15 C16 C29 . . 123.47(11) ?
    C16 C17 O6 . . 127.12(12) ?
    C16 C17 C18 . . 124.26(12) ?
    O6 C17 C18 . . 108.60(11) ?
    C19 C18 O5 . . 127.98(12) ?
    C19 C18 C17 . . 122.69(11) ?
    O5 C18 C17 . . 109.32(11) ?
    C18 C19 C20 . . 116.05(11) ?
    C18 C19 H19 . . 122.0 ?
    C20 C19 H19 . . 122.0 ?
    C11 C20 C19 . . 120.23(11) ?
    C11 C20 C15 . . 117.76(11) ?
    C19 C20 C15 . . 122.01(11) ?
    O1 C21 O2 . . 106.62(12) ?
    O1 C21 H21A . . 110.4 ?
    O2 C21 H21A . . 110.4 ?
    O1 C21 H21B . . 110.4 ?
    O2 C21 H21B . . 110.4 ?
    H21A C21 H21B . . 108.6 ?
    O4 C22 O3 . . 112.29(10) ?
    O4 C22 H22A . . 109.1 ?
    O3 C22 H22A . . 109.1 ?
    O4 C22 H22B . . 109.1 ?
    O3 C22 H22B . . 109.1 ?
    H22A C22 H22B . . 107.9 ?
    O6 C23 O5 . . 107.43(10) ?
    O6 C23 H23A . . 110.2 ?
    O5 C23 H23A . . 110.2 ?
    O6 C23 H23B . . 110.2 ?
    O5 C23 H23B . . 110.2 ?
    H23A C23 H23B . . 108.5 ?
    C3 C24 H24A . . 109.5 ?
    C3 C24 H24B . . 109.5 ?
    H24A C24 H24B . . 109.5 ?
    C3 C24 H24C . . 109.5 ?
    H24A C24 H24C . . 109.5 ?
    H24B C24 H24C . . 109.5 ?
    C6 C25 C26 . . 110.01(12) ?
    C6 C25 C27 . . 112.64(12) ?
    C26 C25 C27 . . 111.63(12) ?
    C6 C25 H25 . . 107.4 ?
    C26 C25 H25 . . 107.4 ?
    C27 C25 H25 . . 107.4 ?
    C25 C26 H26A . . 109.5 ?
    C25 C26 H26B . . 109.5 ?
    H26A C26 H26B . . 109.5 ?
    C25 C26 H26C . . 109.5 ?
    H26A C26 H26C . . 109.5 ?
    H26B C26 H26C . . 109.5 ?
    C25 C27 H27A . . 109.5 ?
    C25 C27 H27B . . 109.5 ?
    H27A C27 H27B . . 109.5 ?
    C25 C27 H27C . . 109.5 ?
    H27A C27 H27C . . 109.5 ?
    H27B C27 H27C . . 109.5 ?
    C13 C28 H28A . . 109.5 ?
    C13 C28 H28B . . 109.5 ?
    H28A C28 H28B . . 109.5 ?
    C13 C28 H28C . . 109.5 ?
    H28A C28 H28C . . 109.5 ?
    H28B C28 H28C . . 109.5 ?
    C16 C29 C30 . . 112.64(12) ?
    C16 C29 C31 . . 109.28(12) ?
    C30 C29 C31 . . 110.71(12) ?
    C16 C29 H29 . . 108.0 ?
    C30 C29 H29 . . 108.0 ?
    C31 C29 H29 . . 108.0 ?
    C29 C30 H30A . . 109.5 ?
    C29 C30 H30B . . 109.5 ?
    H30A C30 H30B . . 109.5 ?
    C29 C30 H30C . . 109.5 ?
    H30A C30 H30C . . 109.5 ?
    H30B C30 H30C . . 109.5 ?
    C29 C31 H31A . . 109.5 ?
    C29 C31 H31B . . 109.5 ?
    H31A C31 H31B . . 109.5 ?
    C29 C31 H31C . . 109.5 ?
    H31A C31 H31C . . 109.5 ?
    H31B C31 H31C . . 109.5 ?
    C7 O1 C21 . . 105.23(11) ?
    C8 O2 C21 . . 104.42(11) ?
    C1 O3 C22 . . 112.20(10) ?
    C11 O4 C22 . . 112.54(10) ?
    C18 O5 C23 . . 105.17(10) ?
    C17 O6 C23 . . 106.00(10) ?
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
    O3 C1 C2 C3 . . . . 175.54(10) ?
    C10 C1 C2 C3 . . . . -5.07(19) ?
    O3 C1 C2 C12 . . . . 1.47(17) ?
    C10 C1 C2 C12 . . . . -179.13(11) ?
    C1 C2 C3 C4 . . . . 2.77(18) ?
    C12 C2 C3 C4 . . . . 176.34(11) ?
    C1 C2 C3 C24 . . . . -173.52(12) ?
    C12 C2 C3 C24 . . . . 0.05(19) ?
    C2 C3 C4 C5 . . . . 1.10(19) ?
    C24 C3 C4 C5 . . . . 177.50(12) ?
    C3 C4 C5 C10 . . . . -2.82(18) ?
    C3 C4 C5 C6 . . . . 176.00(12) ?
    C4 C5 C6 C7 . . . . -176.55(12) ?
    C10 C5 C6 C7 . . . . 2.23(18) ?
    C4 C5 C6 C25 . . . . -1.22(19) ?
    C10 C5 C6 C25 . . . . 177.56(12) ?
    C5 C6 C7 O1 . . . . 177.26(12) ?
    C25 C6 C7 O1 . . . . 1.9(2) ?
    C5 C6 C7 C8 . . . . -2.8(2) ?
    C25 C6 C7 C8 . . . . -178.14(13) ?
    C6 C7 C8 C9 . . . . 1.3(2) ?
    O1 C7 C8 C9 . . . . -178.72(13) ?
    C6 C7 C8 O2 . . . . -178.55(13) ?
    O1 C7 C8 O2 . . . . 1.42(16) ?
    O2 C8 C9 C10 . . . . -179.36(13) ?
    C7 C8 C9 C10 . . . . 0.8(2) ?
    C2 C1 C10 C9 . . . . -174.57(12) ?
    O3 C1 C10 C9 . . . . 4.83(17) ?
    C2 C1 C10 C5 . . . . 3.33(19) ?
    O3 C1 C10 C5 . . . . -177.27(10) ?
    C8 C9 C10 C1 . . . . 176.59(12) ?
    C8 C9 C10 C5 . . . . -1.23(19) ?
    C4 C5 C10 C1 . . . . 0.65(17) ?
    C6 C5 C10 C1 . . . . -178.19(11) ?
    C4 C5 C10 C9 . . . . 178.53(11) ?
    C6 C5 C10 C9 . . . . -0.31(18) ?
    O4 C11 C12 C13 . . . . 177.72(11) ?
    C20 C11 C12 C13 . . . . -3.15(19) ?
    O4 C11 C12 C2 . . . . 1.94(17) ?
    C20 C11 C12 C2 . . . . -178.93(11) ?
    C1 C2 C12 C11 . . . . 49.07(16) ?
    C3 C2 C12 C11 . . . . -124.53(13) ?
    C1 C2 C12 C13 . . . . -126.35(13) ?
    C3 C2 C12 C13 . . . . 60.04(18) ?
    C11 C12 C13 C14 . . . . 2.84(18) ?
    C2 C12 C13 C14 . . . . 178.23(12) ?
    C11 C12 C13 C28 . . . . -173.25(12) ?
    C2 C12 C13 C28 . . . . 2.1(2) ?
    C12 C13 C14 C15 . . . . -0.7(2) ?
    C28 C13 C14 C15 . . . . 175.52(12) ?
    C13 C14 C15 C20 . . . . -1.35(19) ?
    C13 C14 C15 C16 . . . . -179.34(12) ?
    C14 C15 C16 C17 . . . . -179.62(12) ?
    C20 C15 C16 C17 . . . . 2.43(18) ?
    C14 C15 C16 C29 . . . . -2.7(2) ?
    C20 C15 C16 C29 . . . . 179.38(12) ?
    C15 C16 C17 O6 . . . . 179.85(12) ?
    C29 C16 C17 O6 . . . . 2.8(2) ?
    C15 C16 C17 C18 . . . . -2.0(2) ?
    C29 C16 C17 C18 . . . . -179.06(12) ?
    C16 C17 C18 C19 . . . . 0.2(2) ?
    O6 C17 C18 C19 . . . . 178.63(12) ?
    C16 C17 C18 O5 . . . . -178.74(12) ?
    O6 C17 C18 O5 . . . . -0.33(15) ?
    O5 C18 C19 C20 . . . . 179.94(12) ?
    C17 C18 C19 C20 . . . . 1.19(19) ?
    C12 C11 C20 C19 . . . . -178.50(12) ?
    O4 C11 C20 C19 . . . . 0.63(17) ?
    C12 C11 C20 C15 . . . . 1.13(19) ?
    O4 C11 C20 C15 . . . . -179.73(11) ?
    C18 C19 C20 C11 . . . . 178.95(12) ?
    C18 C19 C20 C15 . . . . -0.67(18) ?
    C14 C15 C20 C11 . . . . 1.14(18) ?
    C16 C15 C20 C11 . . . . 179.20(11) ?
    C14 C15 C20 C19 . . . . -179.23(11) ?
    C16 C15 C20 C19 . . . . -1.18(19) ?
    C7 C6 C25 C26 . . . . 76.33(16) ?
    C5 C6 C25 C26 . . . . -98.68(15) ?
    C7 C6 C25 C27 . . . . -48.91(18) ?
    C5 C6 C25 C27 . . . . 136.07(14) ?
    C17 C16 C29 C30 . . . . -50.79(18) ?
    C15 C16 C29 C30 . . . . 132.44(14) ?
    C17 C16 C29 C31 . . . . 72.70(17) ?
    C15 C16 C29 C31 . . . . -104.07(15) ?
    C6 C7 O1 C21 . . . . -166.34(15) ?
    C8 C7 O1 C21 . . . . 13.69(16) ?
    O2 C21 O1 C7 . . . . -23.43(17) ?
    C9 C8 O2 C21 . . . . 164.34(16) ?
    C7 C8 O2 C21 . . . . -15.81(16) ?
    O1 C21 O2 C8 . . . . 24.11(17) ?
    C2 C1 O3 C22 . . . . -76.37(14) ?
    C10 C1 O3 C22 . . . . 104.20(12) ?
    O4 C22 O3 C1 . . . . 46.28(14) ?
    C12 C11 O4 C22 . . . . -77.59(14) ?
    C20 C11 O4 C22 . . . . 103.22(13) ?
    O3 C22 O4 C11 . . . . 47.28(14) ?
    C19 C18 O5 C23 . . . . 170.18(13) ?
    C17 C18 O5 C23 . . . . -10.94(14) ?
    O6 C23 O5 C18 . . . . 18.06(14) ?
    C16 C17 O6 C23 . . . . -170.02(14) ?
    C18 C17 O6 C23 . . . . 11.63(14) ?
    O5 C23 O6 C17 . . . . -18.38(14) ?
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    C23 H23A O5 2_866 0.99 2.58 3.3956(18) 140
    C23 H23B O4 2_766 0.99 2.58 3.2442(18) 124
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
