# Electronic Supplementary Material (ESI) for Catalysis Science & Technology.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Sam2
_database_code_depnum_ccdc_archive 'CCDC 1409564'
_audit_update_record             
;
2015-06-29 deposited with the CCDC.
2016-11-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H30 O4, H2 O'
_chemical_formula_sum            'C46 H32 O5'
_chemical_formula_weight         664.71

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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.
;

loop_
_space_group_symop_operation_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                   9.6965(4)
_cell_length_b                   17.3653(7)
_cell_length_c                   19.2464(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3240.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    8084
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      26.72

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_F_000             1392
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.088
_shelx_estimated_absorpt_T_min   0.983
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.969
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            44815
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_av_R_equivalents  0.0669
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.116
_diffrn_reflns_theta_max         30.575
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9922
_reflns_number_gt                7141
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.805
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0846P)²+0.0074P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2621 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0(4)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         9922
_refine_ls_number_parameters     460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0539
_refine_ls_wR_factor_ref         0.1457
_refine_ls_wR_factor_gt          0.1281
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 1.1396(2) 0.28881(10) 0.67516(10) 0.0245(4) Uani 1 1 d . . . . .
H1O H 1.0784 0.3141 0.7020 0.037 Uiso 1 1 d R U . . .
O2 O 0.91823(19) 0.30873(10) 0.75308(10) 0.0242(4) Uani 1 1 d . . . . .
H2O H 0.8809 0.3433 0.7823 0.036 Uiso 1 1 d R U . . .
O3 O 0.6226(2) 0.24564(11) 0.75578(10) 0.0255(4) Uani 1 1 d . . . . .
H3O H 0.5367 0.2514 0.7390 0.038 Uiso 1 1 d R U . . .
O4 O 0.3664(2) 0.28402(11) 0.75834(11) 0.0301(4) Uani 1 1 d . . . . .
H4O H 0.2942 0.2958 0.7309 0.045 Uiso 1 1 d R U . . .
C1 C 0.8508(3) 0.20792(14) 0.83203(13) 0.0205(5) Uani 1 1 d . . . . .
C2 C 0.9273(3) 0.23399(15) 0.77660(13) 0.0206(5) Uani 1 1 d . . . . .
C3 C 1.0185(3) 0.18495(15) 0.73800(13) 0.0212(5) Uani 1 1 d . . . . .
C4 C 1.0359(3) 0.11077(15) 0.76089(14) 0.0230(5) Uani 1 1 d . . . . .
H4 H 1.0973 0.0778 0.7366 0.028 Uiso 1 1 calc R U . . .
C4A C 0.9646(3) 0.08186(15) 0.81985(13) 0.0222(5) Uani 1 1 d . . . . .
C5 C 0.9825(3) 0.00375(16) 0.84186(14) 0.0275(6) Uani 1 1 d . . . . .
H5 H 1.0462 -0.0286 0.8184 0.033 Uiso 1 1 calc R U . . .
C6 C 0.9082(3) -0.02429(16) 0.89658(15) 0.0307(7) Uani 1 1 d . . . . .
H6 H 0.9198 -0.0764 0.9104 0.037 Uiso 1 1 calc R U . . .
C7 C 0.8143(3) 0.02316(16) 0.93286(16) 0.0291(6) Uani 1 1 d . . . . .
H7 H 0.7651 0.0033 0.9716 0.035 Uiso 1 1 calc R U . . .
C8 C 0.7941(3) 0.09836(16) 0.91212(14) 0.0250(6) Uani 1 1 d . . . . .
H8 H 0.7291 0.1295 0.9361 0.030 Uiso 1 1 calc R U . . .
C8A C 0.8693(3) 0.12987(15) 0.85521(14) 0.0222(5) Uani 1 1 d . . . . .
C9 C 0.7419(3) 0.25942(14) 0.86156(13) 0.0204(5) Uani 1 1 d . . . . .
C10 C 0.6292(3) 0.27793(15) 0.82029(13) 0.0206(5) Uani 1 1 d . . . . .
C11 C 0.5241(3) 0.32962(14) 0.84380(14) 0.0215(5) Uani 1 1 d . . . . .
C12 C 0.5350(3) 0.36071(15) 0.90910(15) 0.0235(5) Uani 1 1 d . . . . .
H12 H 0.4662 0.3955 0.9249 0.028 Uiso 1 1 calc R U . . .
C12A C 0.6463(3) 0.34218(15) 0.95346(13) 0.0214(5) Uani 1 1 d . . . . .
C13 C 0.6539(3) 0.37241(15) 1.02248(14) 0.0248(6) Uani 1 1 d . . . . .
H13 H 0.5842 0.4065 1.0385 0.030 Uiso 1 1 calc R U . . .
C14 C 0.7582(3) 0.35328(17) 1.06495(15) 0.0303(6) Uani 1 1 d . . . . .
H14 H 0.7597 0.3723 1.1112 0.036 Uiso 1 1 calc R U . . .
C15 C 0.8657(3) 0.30513(17) 1.04127(15) 0.0301(6) Uani 1 1 d . . . . .
H15 H 0.9411 0.2938 1.0711 0.036 Uiso 1 1 calc R U . . .
C16 C 0.8623(3) 0.27449(16) 0.97563(14) 0.0255(6) Uani 1 1 d . . . . .
H16 H 0.9348 0.2416 0.9606 0.031 Uiso 1 1 calc R U . . .
C16A C 0.7515(3) 0.29143(15) 0.92986(14) 0.0212(5) Uani 1 1 d . . . . .
C17 C 1.0782(3) 0.21245(15) 0.66885(13) 0.0226(5) Uani 1 1 d . . . . .
C17A C 0.9672(3) 0.21061(16) 0.61118(14) 0.0263(6) Uani 1 1 d . . . . .
C18 C 0.8347(3) 0.24102(19) 0.61090(17) 0.0338(7) Uani 1 1 d . . . . .
H18 H 0.8016 0.2696 0.6496 0.041 Uiso 1 1 calc R U . . .
C19 C 0.7510(4) 0.2289(2) 0.55295(19) 0.0434(8) Uani 1 1 d . . . . .
H19 H 0.6598 0.2489 0.5525 0.052 Uiso 1 1 calc R U . . .
C20 C 0.7989(4) 0.1884(2) 0.49636(18) 0.0446(9) Uani 1 1 d . . . . .
H20 H 0.7413 0.1822 0.4569 0.054 Uiso 1 1 calc R U . . .
C21 C 0.9294(4) 0.15669(19) 0.49618(16) 0.0391(8) Uani 1 1 d . . . . .
H21 H 0.9615 0.1284 0.4572 0.047 Uiso 1 1 calc R U . . .
C21A C 1.0141(3) 0.16700(17) 0.55468(15) 0.0300(6) Uani 1 1 d . . . . .
C21B C 1.1510(3) 0.13709(17) 0.57048(15) 0.0290(6) Uani 1 1 d . . . . .
C22 C 1.2390(4) 0.0911(2) 0.53030(17) 0.0404(8) Uani 1 1 d . . . . .
H22 H 1.2119 0.0737 0.4856 0.049 Uiso 1 1 calc R U . . .
C23 C 1.3663(4) 0.0719(2) 0.55754(18) 0.0427(8) Uani 1 1 d . . . . .
H23 H 1.4282 0.0418 0.5306 0.051 Uiso 1 1 calc R U . . .
C24 C 1.4054(4) 0.09574(19) 0.62364(17) 0.0382(8) Uani 1 1 d . . . . .
H24 H 1.4935 0.0820 0.6413 0.046 Uiso 1 1 calc R U . . .
C25 C 1.3154(3) 0.14009(17) 0.66451(16) 0.0300(6) Uani 1 1 d . . . . .
H25 H 1.3408 0.1555 0.7101 0.036 Uiso 1 1 calc R U . . .
C25A C 1.1900(3) 0.16075(16) 0.63716(14) 0.0248(6) Uani 1 1 d . . . . .
C26 C 0.4054(3) 0.35278(15) 0.79511(15) 0.0254(6) Uani 1 1 d . . . . .
C26A C 0.2846(3) 0.38947(16) 0.83402(15) 0.0272(6) Uani 1 1 d . . . . .
C27 C 0.1970(3) 0.35624(19) 0.88161(18) 0.0345(7) Uani 1 1 d . . . . .
H27 H 0.2024 0.3028 0.8919 0.041 Uiso 1 1 calc R U . . .
C28 C 0.0999(3) 0.4032(2) 0.91441(19) 0.0414(8) Uani 1 1 d . . . . .
H28 H 0.0372 0.3813 0.9468 0.050 Uiso 1 1 calc R U . . .
C29 C 0.0940(4) 0.4812(2) 0.9001(2) 0.0430(8) Uani 1 1 d . . . . .
H29 H 0.0292 0.5125 0.9241 0.052 Uiso 1 1 calc R U . . .
C30 C 0.1803(3) 0.51445(19) 0.85184(19) 0.0381(8) Uani 1 1 d . . . . .
H30 H 0.1755 0.5681 0.8424 0.046 Uiso 1 1 calc R U . . .
C30A C 0.2752(3) 0.46767(17) 0.81697(16) 0.0297(6) Uani 1 1 d . . . . .
C30B C 0.3756(3) 0.48556(17) 0.76331(16) 0.0312(6) Uani 1 1 d . . . . .
C31 C 0.4030(4) 0.55416(18) 0.72892(19) 0.0390(8) Uani 1 1 d . . . . .
H31 H 0.3523 0.5994 0.7397 0.047 Uiso 1 1 calc R U . . .
C32 C 0.5037(4) 0.5556(2) 0.67953(19) 0.0446(9) Uani 1 1 d . . . . .
H32 H 0.5225 0.6024 0.6557 0.053 Uiso 1 1 calc R U . . .
C33 C 0.5801(4) 0.4895(2) 0.66319(17) 0.0399(8) Uani 1 1 d . . . . .
H33 H 0.6498 0.4919 0.6286 0.048 Uiso 1 1 calc R U . . .
C34 C 0.5545(3) 0.42043(18) 0.69725(16) 0.0334(7) Uani 1 1 d . . . . .
H34 H 0.6061 0.3755 0.6864 0.040 Uiso 1 1 calc R U . . .
C34A C 0.4517(3) 0.41856(16) 0.74746(15) 0.0273(6) Uani 1 1 d . . . . .
O5 O 0.8141(3) 0.43984(14) 0.81144(14) 0.0467(6) Uani 1 1 d . . . . .
H5A H 0.7227 0.4378 0.8196 0.070 Uiso 1 1 d R U . . .
H5B H 0.8574 0.4538 0.8508 0.070 Uiso 1 1 d R U . . .


_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 C17 1.458(3) . ?
O1 H1O 0.9001 . ?
O2 C2 1.377(3) . ?
O2 H2O 0.8988 . ?
O3 C10 1.364(3) . ?
O3 H3O 0.8992 . ?
O4 C26 1.439(3) . ?
O4 H4O 0.9007 . ?
C1 C2 1.376(4) . ?
C1 C8A 1.438(4) . ?
C1 C9 1.496(4) . ?
C2 C3 1.435(4) . ?
C3 C4 1.372(4) . ?
C3 C17 1.528(4) . ?
C4 C4A 1.420(4) . ?
C4 H4 0.9500 . ?
C4A C8A 1.418(4) . ?
C4A C5 1.432(4) . ?
C5 C6 1.366(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.413(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.379(4) . ?
C7 H7 0.9500 . ?
C8 C8A 1.426(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.389(4) . ?
C9 C16A 1.430(4) . ?
C10 C11 1.431(4) . ?
C11 C12 1.372(4) . ?
C11 C26 1.538(4) . ?
C12 C12A 1.413(4) . ?
C12 H12 0.9500 . ?
C12A C16A 1.422(4) . ?
C12A C13 1.430(4) . ?
C13 C14 1.342(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.412(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.371(4) . ?
C15 H15 0.9500 . ?
C16 C16A 1.421(4) . ?
C16 H16 0.9500 . ?
C17 C25A 1.535(4) . ?
C17 C17A 1.546(4) . ?
C17A C18 1.389(4) . ?
C17A C21A 1.401(4) . ?
C18 C19 1.395(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.378(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.380(6) . ?
C20 H20 0.9500 . ?
C21 C21A 1.405(4) . ?
C21 H21 0.9500 . ?
C21A C21B 1.457(5) . ?
C21B C25A 1.400(4) . ?
C21B C22 1.401(5) . ?
C22 C23 1.382(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.391(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.405(4) . ?
C24 H24 0.9500 . ?
C25 C25A 1.373(4) . ?
C25 H25 0.9500 . ?
C26 C26A 1.530(4) . ?
C26 C34A 1.532(4) . ?
C26A C27 1.376(5) . ?
C26A C30A 1.400(4) . ?
C27 C28 1.396(5) . ?
C27 H27 0.9500 . ?
C28 C29 1.384(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.378(5) . ?
C29 H29 0.9500 . ?
C30 C30A 1.399(4) . ?
C30 H30 0.9500 . ?
C30A C30B 1.453(5) . ?
C30B C31 1.389(4) . ?
C30B C34A 1.411(4) . ?
C31 C32 1.363(5) . ?
C31 H31 0.9500 . ?
C32 C33 1.402(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.389(5) . ?
C33 H33 0.9500 . ?
C34 C34A 1.389(5) . ?
C34 H34 0.9500 . ?
O5 H5A 0.9001 . ?
O5 H5B 0.9001 . ?

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
C17 O1 H1O 102.8 . . ?
C2 O2 H2O 116.7 . . ?
C10 O3 H3O 109.0 . . ?
C26 O4 H4O 107.7 . . ?
C2 C1 C8A 118.9(2) . . ?
C2 C1 C9 118.6(2) . . ?
C8A C1 C9 122.3(2) . . ?
C1 C2 O2 122.0(2) . . ?
C1 C2 C3 122.6(2) . . ?
O2 C2 C3 115.4(2) . . ?
C4 C3 C2 117.8(2) . . ?
C4 C3 C17 121.8(2) . . ?
C2 C3 C17 119.9(2) . . ?
C3 C4 C4A 121.9(2) . . ?
C3 C4 H4 119.0 . . ?
C4A C4 H4 119.0 . . ?
C8A C4A C4 119.5(2) . . ?
C8A C4A C5 119.6(2) . . ?
C4 C4A C5 120.8(2) . . ?
C6 C5 C4A 120.1(3) . . ?
C6 C5 H5 119.9 . . ?
C4A C5 H5 119.9 . . ?
C5 C6 C7 120.9(3) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 H6 119.6 . . ?
C8 C7 C6 120.1(3) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C8 C8A 120.9(3) . . ?
C7 C8 H8 119.6 . . ?
C8A C8 H8 119.6 . . ?
C4A C8A C8 118.5(2) . . ?
C4A C8A C1 119.1(2) . . ?
C8 C8A C1 122.4(2) . . ?
C10 C9 C16A 119.1(2) . . ?
C10 C9 C1 118.5(2) . . ?
C16A C9 C1 122.4(2) . . ?
O3 C10 C9 117.5(2) . . ?
O3 C10 C11 120.8(2) . . ?
C9 C10 C11 121.6(2) . . ?
C12 C11 C10 118.8(2) . . ?
C12 C11 C26 120.9(2) . . ?
C10 C11 C26 120.3(2) . . ?
C11 C12 C12A 121.5(2) . . ?
C11 C12 H12 119.2 . . ?
C12A C12 H12 119.2 . . ?
C12 C12A C16A 119.7(2) . . ?
C12 C12A C13 121.1(2) . . ?
C16A C12A C13 119.2(2) . . ?
C14 C13 C12A 120.9(3) . . ?
C14 C13 H13 119.5 . . ?
C12A C13 H13 119.5 . . ?
C13 C14 C15 120.4(3) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
C16 C15 C14 120.6(3) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C15 C16 C16A 120.6(3) . . ?
C15 C16 H16 119.7 . . ?
C16A C16 H16 119.7 . . ?
C16 C16A C12A 118.2(2) . . ?
C16 C16A C9 122.6(2) . . ?
C12A C16A C9 119.2(2) . . ?
O1 C17 C3 111.5(2) . . ?
O1 C17 C25A 106.0(2) . . ?
C3 C17 C25A 115.5(2) . . ?
O1 C17 C17A 111.3(2) . . ?
C3 C17 C17A 110.8(2) . . ?
C25A C17 C17A 101.2(2) . . ?
C18 C17A C21A 120.2(3) . . ?
C18 C17A C17 129.7(3) . . ?
C21A C17A C17 110.0(3) . . ?
C17A C18 C19 119.0(3) . . ?
C17A C18 H18 120.5 . . ?
C19 C18 H18 120.5 . . ?
C20 C19 C18 120.8(3) . . ?
C20 C19 H19 119.6 . . ?
C18 C19 H19 119.6 . . ?
C19 C20 C21 121.0(3) . . ?
C19 C20 H20 119.5 . . ?
C21 C20 H20 119.5 . . ?
C20 C21 C21A 118.9(3) . . ?
C20 C21 H21 120.6 . . ?
C21A C21 H21 120.6 . . ?
C17A C21A C21 120.1(3) . . ?
C17A C21A C21B 109.1(2) . . ?
C21 C21A C21B 130.9(3) . . ?
C25A C21B C22 120.6(3) . . ?
C25A C21B C21A 109.4(3) . . ?
C22 C21B C21A 130.0(3) . . ?
C23 C22 C21B 118.2(3) . . ?
C23 C22 H22 120.9 . . ?
C21B C22 H22 120.9 . . ?
C22 C23 C24 121.2(3) . . ?
C22 C23 H23 119.4 . . ?
C24 C23 H23 119.4 . . ?
C23 C24 C25 120.4(3) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
C25A C25 C24 118.6(3) . . ?
C25A C25 H25 120.7 . . ?
C24 C25 H25 120.7 . . ?
C25 C25A C21B 121.0(3) . . ?
C25 C25A C17 128.8(2) . . ?
C21B C25A C17 110.2(3) . . ?
O4 C26 C26A 112.6(2) . . ?
O4 C26 C34A 113.7(2) . . ?
C26A C26 C34A 101.9(2) . . ?
O4 C26 C11 106.2(2) . . ?
C26A C26 C11 112.6(2) . . ?
C34A C26 C11 109.9(2) . . ?
C27 C26A C30A 121.5(3) . . ?
C27 C26A C26 128.6(3) . . ?
C30A C26A C26 109.8(3) . . ?
C26A C27 C28 118.2(3) . . ?
C26A C27 H27 120.9 . . ?
C28 C27 H27 120.9 . . ?
C29 C28 C27 120.6(3) . . ?
C29 C28 H28 119.7 . . ?
C27 C28 H28 119.7 . . ?
C30 C29 C28 121.3(3) . . ?
C30 C29 H29 119.4 . . ?
C28 C29 H29 119.4 . . ?
C29 C30 C30A 118.7(3) . . ?
C29 C30 H30 120.7 . . ?
C30A C30 H30 120.7 . . ?
C30 C30A C26A 119.6(3) . . ?
C30 C30A C30B 131.1(3) . . ?
C26A C30A C30B 109.3(3) . . ?
C31 C30B C34A 120.3(3) . . ?
C31 C30B C30A 130.6(3) . . ?
C34A C30B C30A 109.1(3) . . ?
C32 C31 C30B 119.1(3) . . ?
C32 C31 H31 120.5 . . ?
C30B C31 H31 120.5 . . ?
C31 C32 C33 121.3(3) . . ?
C31 C32 H32 119.4 . . ?
C33 C32 H32 119.4 . . ?
C34 C33 C32 120.5(3) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
C34A C34 C33 118.5(3) . . ?
C34A C34 H34 120.8 . . ?
C33 C34 H34 120.8 . . ?
C34 C34A C30B 120.4(3) . . ?
C34 C34A C26 130.1(3) . . ?
C30B C34A C26 109.4(3) . . ?
H5A O5 H5B 108.9 . . ?

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
C8A C1 C2 O2 -177.8(2) . . . . ?
C9 C1 C2 O2 7.9(4) . . . . ?
C8A C1 C2 C3 4.2(4) . . . . ?
C9 C1 C2 C3 -170.0(2) . . . . ?
C1 C2 C3 C4 -4.5(4) . . . . ?
O2 C2 C3 C4 177.4(2) . . . . ?
C1 C2 C3 C17 167.8(2) . . . . ?
O2 C2 C3 C17 -10.3(3) . . . . ?
C2 C3 C4 C4A 1.3(4) . . . . ?
C17 C3 C4 C4A -170.8(2) . . . . ?
C3 C4 C4A C8A 2.0(4) . . . . ?
C3 C4 C4A C5 178.8(3) . . . . ?
C8A C4A C5 C6 0.0(4) . . . . ?
C4 C4A C5 C6 -176.8(3) . . . . ?
C4A C5 C6 C7 -0.9(4) . . . . ?
C5 C6 C7 C8 1.6(5) . . . . ?
C6 C7 C8 C8A -1.5(4) . . . . ?
C4 C4A C8A C8 176.9(3) . . . . ?
C5 C4A C8A C8 0.1(4) . . . . ?
C4 C4A C8A C1 -2.3(4) . . . . ?
C5 C4A C8A C1 -179.1(2) . . . . ?
C7 C8 C8A C4A 0.7(4) . . . . ?
C7 C8 C8A C1 179.9(3) . . . . ?
C2 C1 C8A C4A -0.7(4) . . . . ?
C9 C1 C8A C4A 173.3(2) . . . . ?
C2 C1 C8A C8 -179.9(3) . . . . ?
C9 C1 C8A C8 -5.9(4) . . . . ?
C2 C1 C9 C10 65.2(3) . . . . ?
C8A C1 C9 C10 -108.8(3) . . . . ?
C2 C1 C9 C16A -113.3(3) . . . . ?
C8A C1 C9 C16A 72.7(3) . . . . ?
C16A C9 C10 O3 -179.2(2) . . . . ?
C1 C9 C10 O3 2.2(3) . . . . ?
C16A C9 C10 C11 1.5(4) . . . . ?
C1 C9 C10 C11 -177.1(2) . . . . ?
O3 C10 C11 C12 180.0(2) . . . . ?
C9 C10 C11 C12 -0.8(4) . . . . ?
O3 C10 C11 C26 -3.1(4) . . . . ?
C9 C10 C11 C26 176.2(2) . . . . ?
C10 C11 C12 C12A -0.7(4) . . . . ?
C26 C11 C12 C12A -177.6(2) . . . . ?
C11 C12 C12A C16A 1.3(4) . . . . ?
C11 C12 C12A C13 -177.4(3) . . . . ?
C12 C12A C13 C14 178.5(3) . . . . ?
C16A C12A C13 C14 -0.2(4) . . . . ?
C12A C13 C14 C15 2.5(4) . . . . ?
C13 C14 C15 C16 -2.8(5) . . . . ?
C14 C15 C16 C16A 0.8(4) . . . . ?
C15 C16 C16A C12A 1.4(4) . . . . ?
C15 C16 C16A C9 -178.5(3) . . . . ?
C12 C12A C16A C16 179.5(2) . . . . ?
C13 C12A C16A C16 -1.7(4) . . . . ?
C12 C12A C16A C9 -0.6(4) . . . . ?
C13 C12A C16A C9 178.2(2) . . . . ?
C10 C9 C16A C16 179.1(2) . . . . ?
C1 C9 C16A C16 -2.4(4) . . . . ?
C10 C9 C16A C12A -0.8(4) . . . . ?
C1 C9 C16A C12A 177.7(2) . . . . ?
C4 C3 C17 O1 -137.6(3) . . . . ?
C2 C3 C17 O1 50.4(3) . . . . ?
C4 C3 C17 C25A -16.4(4) . . . . ?
C2 C3 C17 C25A 171.6(2) . . . . ?
C4 C3 C17 C17A 97.9(3) . . . . ?
C2 C3 C17 C17A -74.1(3) . . . . ?
O1 C17 C17A C18 -73.9(4) . . . . ?
C3 C17 C17A C18 50.8(4) . . . . ?
C25A C17 C17A C18 173.8(3) . . . . ?
O1 C17 C17A C21A 110.0(3) . . . . ?
C3 C17 C17A C21A -125.4(3) . . . . ?
C25A C17 C17A C21A -2.3(3) . . . . ?
C21A C17A C18 C19 -1.5(5) . . . . ?
C17 C17A C18 C19 -177.3(3) . . . . ?
C17A C18 C19 C20 -0.8(5) . . . . ?
C18 C19 C20 C21 1.9(6) . . . . ?
C19 C20 C21 C21A -0.6(5) . . . . ?
C18 C17A C21A C21 2.8(4) . . . . ?
C17 C17A C21A C21 179.4(3) . . . . ?
C18 C17A C21A C21B -175.5(3) . . . . ?
C17 C17A C21A C21B 1.1(3) . . . . ?
C20 C21 C21A C17A -1.7(5) . . . . ?
C20 C21 C21A C21B 176.1(3) . . . . ?
C17A C21A C21B C25A 0.8(3) . . . . ?
C21 C21A C21B C25A -177.2(3) . . . . ?
C17A C21A C21B C22 -179.7(3) . . . . ?
C21 C21A C21B C22 2.2(6) . . . . ?
C25A C21B C22 C23 -1.9(5) . . . . ?
C21A C21B C22 C23 178.7(3) . . . . ?
C21B C22 C23 C24 1.5(5) . . . . ?
C22 C23 C24 C25 0.2(5) . . . . ?
C23 C24 C25 C25A -1.6(5) . . . . ?
C24 C25 C25A C21B 1.2(4) . . . . ?
C24 C25 C25A C17 -175.9(3) . . . . ?
C22 C21B C25A C25 0.5(5) . . . . ?
C21A C21B C25A C25 -180.0(3) . . . . ?
C22 C21B C25A C17 178.1(3) . . . . ?
C21A C21B C25A C17 -2.4(3) . . . . ?
O1 C17 C25A C25 64.0(4) . . . . ?
C3 C17 C25A C25 -60.1(4) . . . . ?
C17A C17 C25A C25 -179.8(3) . . . . ?
O1 C17 C25A C21B -113.4(2) . . . . ?
C3 C17 C25A C21B 122.6(3) . . . . ?
C17A C17 C25A C21B 2.8(3) . . . . ?
C12 C11 C26 O4 -142.5(3) . . . . ?
C10 C11 C26 O4 40.6(3) . . . . ?
C12 C11 C26 C26A -18.8(4) . . . . ?
C10 C11 C26 C26A 164.3(2) . . . . ?
C12 C11 C26 C34A 94.1(3) . . . . ?
C10 C11 C26 C34A -82.8(3) . . . . ?
O4 C26 C26A C27 54.1(4) . . . . ?
C34A C26 C26A C27 176.2(3) . . . . ?
C11 C26 C26A C27 -66.1(4) . . . . ?
O4 C26 C26A C30A -128.6(2) . . . . ?
C34A C26 C26A C30A -6.5(3) . . . . ?
C11 C26 C26A C30A 111.3(3) . . . . ?
C30A C26A C27 C28 -1.8(5) . . . . ?
C26 C26A C27 C28 175.2(3) . . . . ?
C26A C27 C28 C29 -1.1(5) . . . . ?
C27 C28 C29 C30 2.0(5) . . . . ?
C28 C29 C30 C30A 0.0(5) . . . . ?
C29 C30 C30A C26A -2.9(5) . . . . ?
C29 C30 C30A C30B 178.5(3) . . . . ?
C27 C26A C30A C30 3.8(4) . . . . ?
C26 C26A C30A C30 -173.7(3) . . . . ?
C27 C26A C30A C30B -177.3(3) . . . . ?
C26 C26A C30A C30B 5.2(3) . . . . ?
C30 C30A C30B C31 -2.8(6) . . . . ?
C26A C30A C30B C31 178.4(3) . . . . ?
C30 C30A C30B C34A 177.2(3) . . . . ?
C26A C30A C30B C34A -1.5(3) . . . . ?
C34A C30B C31 C32 0.4(5) . . . . ?
C30A C30B C31 C32 -179.6(3) . . . . ?
C30B C31 C32 C33 -0.3(5) . . . . ?
C31 C32 C33 C34 0.0(5) . . . . ?
C32 C33 C34 C34A 0.2(5) . . . . ?
C33 C34 C34A C30B -0.1(4) . . . . ?
C33 C34 C34A C26 -176.9(3) . . . . ?
C31 C30B C34A C34 -0.2(4) . . . . ?
C30A C30B C34A C34 179.8(3) . . . . ?
C31 C30B C34A C26 177.3(3) . . . . ?
C30A C30B C34A C26 -2.8(3) . . . . ?
O4 C26 C34A C34 -55.9(4) . . . . ?
C26A C26 C34A C34 -177.4(3) . . . . ?
C11 C26 C34A C34 63.0(4) . . . . ?
O4 C26 C34A C30B 127.0(3) . . . . ?
C26A C26 C34A C30B 5.5(3) . . . . ?
C11 C26 C34A C30B -114.1(3) . . . . ?

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
_geom_hbond_publ_flag

O1 H1O O2 . 0.90 1.84 2.641(2) 147 yes
O2 H2O O5 . 0.90 1.88 2.732(2) 157 yes
O3 H3O O4 . 0.90 1.78 2.572(2) 145 yes
O4 H4O O1 1_455 0.90 1.85 2.722(2) 163 yes

_refine_diff_density_max         0.404
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.062

_shelxl_version_number           2014/6

