# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers.
# This journal is © the Partner Organisations 2017

####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 996790'
_audit_update_record             
;
2017-03-20 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H38 O9'
_chemical_formula_weight         554.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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, y+1/2, -z'

_cell_length_a                   7.90440(10)
_cell_length_b                   11.5678(2)
_cell_length_c                   15.8146(2)
_cell_angle_alpha                90
_cell_angle_beta                 98.2670(10)
_cell_angle_gamma                90
_cell_volume                     1431.01(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    290(2)
_cell_measurement_reflns_used    7481
_cell_measurement_theta_min      3.8181
_cell_measurement_theta_max      69.4405

_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_F_000             592
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.230
_exptl_absorpt_coefficient_mu    0.775
_shelx_estimated_absorpt_T_min   0.768
_shelx_estimated_absorpt_T_max   0.842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93003
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      290(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_measurement_device_type  'Gemini S Ultra, Agilent Technologies'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 15.9149
_diffrn_reflns_number            11215
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         4.754
_diffrn_reflns_theta_max         69.568
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             5242
_reflns_number_gt                5042
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.871
_reflns_Friedel_fraction_max     0.961
_reflns_Friedel_fraction_full    0.980

_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       'CrysAlisPro (Agilent Technologies)'
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Ortep-3 (L. J. Farrugia, 2001)'
_computing_publication_material  SHELXL-2013

_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)+(0.0552P)²+0.1072P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2282 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.05(6)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         5242
_refine_ls_number_parameters     363
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0337
_refine_ls_wR_factor_ref         0.0896
_refine_ls_wR_factor_gt          0.0879
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_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
O8 O 0.3936(2) 0.61461(12) 0.76489(10) 0.0411(3) Uani 1 1 d . . . . .
O6 O 0.10948(18) 0.53131(14) 0.82343(10) 0.0413(3) Uani 1 1 d . . . . .
O3 O -0.1172(2) 0.01809(18) 0.64612(12) 0.0574(5) Uani 1 1 d . . . . .
O7 O -0.1144(2) 0.4736(2) 0.73018(16) 0.0725(6) Uani 1 1 d . . . . .
O4 O 0.4404(3) 0.09438(14) 0.83765(12) 0.0521(4) Uani 1 1 d . . . . .
H4 H 0.3437 0.0977 0.8109 0.078 Uiso 1 1 calc R U . . .
O2 O 0.0958(3) 0.07301(19) 0.74565(12) 0.0623(5) Uani 1 1 d . . . . .
O1 O 0.6012(3) 0.1443(2) 0.50864(14) 0.0681(6) Uani 1 1 d . . . . .
C14 C 0.4515(3) 0.30754(17) 0.83080(13) 0.0346(4) Uani 1 1 d . . . . .
C13 C 0.3287(2) 0.38983(18) 0.86622(13) 0.0339(4) Uani 1 1 d . . . . .
C12 C 0.2197(2) 0.44798(17) 0.79035(13) 0.0337(4) Uani 1 1 d . . . . .
H12 H 0.1472 0.3887 0.7592 0.040 Uiso 1 1 calc R U . . .
C30 C 0.6135(3) 0.2497(2) 0.70852(14) 0.0402(5) Uani 1 1 d . . . . .
H30A H 0.5844 0.1693 0.7163 0.048 Uiso 1 1 calc R U . . .
H30B H 0.7347 0.2602 0.7277 0.048 Uiso 1 1 calc R U . . .
C17 C 0.2210(3) 0.3022(2) 0.91101(14) 0.0398(5) Uani 1 1 d . . . . .
H17 H 0.1504 0.2598 0.8652 0.048 Uiso 1 1 calc R U . . .
O9 O 0.1756(3) 0.72163(18) 0.69873(17) 0.0780(6) Uani 1 1 d . . . . .
C10 C 0.2500(3) 0.33522(19) 0.58543(13) 0.0367(4) Uani 1 1 d . . . . .
C1 C 0.4286(3) 0.38251(18) 0.60976(14) 0.0369(4) Uani 1 1 d . . . . .
H1 H 0.4505 0.4423 0.5688 0.044 Uiso 1 1 calc R U . . .
C9 C 0.4607(3) 0.43297(17) 0.70187(14) 0.0351(4) Uani 1 1 d . . . . .
H9 H 0.5631 0.4815 0.7054 0.042 Uiso 1 1 calc R U . . .
C8 C 0.5089(2) 0.32820(17) 0.75726(14) 0.0346(4) Uani 1 1 d . . . . .
C4 C 0.3285(3) 0.13328(19) 0.55634(14) 0.0414(5) Uani 1 1 d . . . . .
C25 C -0.0548(3) 0.5351(2) 0.78692(17) 0.0473(5) Uani 1 1 d . . . . .
C11 C 0.3176(3) 0.50920(17) 0.72706(14) 0.0352(4) Uani 1 1 d . . . . .
H11 H 0.2381 0.5288 0.6756 0.042 Uiso 1 1 calc R U . . .
C6 C 0.0403(3) 0.1785(2) 0.61322(16) 0.0456(5) Uani 1 1 d . . . . .
H6A H -0.0219 0.2467 0.6268 0.055 Uiso 1 1 calc R U . . .
H6B H -0.0082 0.1535 0.5563 0.055 Uiso 1 1 calc R U . . .
C3 C 0.5079(3) 0.1847(2) 0.55518(14) 0.0434(5) Uani 1 1 d . . . . .
C15 C 0.4763(3) 0.19855(19) 0.88569(14) 0.0409(5) Uani 1 1 d . . . . .
H15 H 0.5945 0.1960 0.9146 0.049 Uiso 1 1 calc R U . . .
C27 C 0.3063(4) 0.7141(2) 0.74719(18) 0.0516(6) Uani 1 1 d . . . . .
C18 C 0.4248(3) 0.4773(2) 0.92886(15) 0.0434(5) Uani 1 1 d . . . . .
H18A H 0.3440 0.5278 0.9500 0.065 Uiso 1 1 calc R U . . .
H18B H 0.5011 0.5221 0.8999 0.065 Uiso 1 1 calc R U . . .
H18C H 0.4891 0.4367 0.9758 0.065 Uiso 1 1 calc R U . . .
C2 C 0.5667(3) 0.2862(2) 0.61255(15) 0.0397(5) Uani 1 1 d . . . . .
H2 H 0.6687 0.3195 0.5934 0.048 Uiso 1 1 calc R U . . .
C16 C 0.3560(3) 0.2162(2) 0.95254(15) 0.0477(5) Uani 1 1 d . . . . .
H16A H 0.4175 0.2476 1.0050 0.057 Uiso 1 1 calc R U . . .
H16B H 0.3033 0.1437 0.9653 0.057 Uiso 1 1 calc R U . . .
C5 C 0.2279(3) 0.21136(19) 0.61253(13) 0.0358(4) Uani 1 1 d . . . . .
H5 H 0.2854 0.2045 0.6715 0.043 Uiso 1 1 calc R U . . .
C7 C 0.0146(3) 0.0849(2) 0.67550(14) 0.0432(5) Uani 1 1 d . . . . .
C19 C 0.1300(3) 0.3982(2) 0.54007(17) 0.0533(6) Uani 1 1 d . . . . .
H19A H 0.1551 0.4723 0.5228 0.064 Uiso 1 1 calc R U . . .
H19B H 0.0204 0.3683 0.5254 0.064 Uiso 1 1 calc R U . . .
C22 C 0.1328(4) 0.4114(3) 1.04570(19) 0.0643(7) Uani 1 1 d . . . . .
H22 H 0.2393 0.4328 1.0743 0.077 Uiso 1 1 calc R U . . .
O5 O -0.1470(3) 0.3913(3) 1.01457(18) 0.1017(10) Uani 1 1 d . . . . .
C29 C 0.2406(4) 0.1259(3) 0.46337(16) 0.0580(7) Uani 1 1 d . . . . .
H29A H 0.1280 0.0941 0.4620 0.087 Uiso 1 1 calc R U . . .
H29B H 0.3063 0.0770 0.4313 0.087 Uiso 1 1 calc R U . . .
H29C H 0.2325 0.2018 0.4387 0.087 Uiso 1 1 calc R U . . .
C20 C 0.1005(3) 0.3489(2) 0.96752(16) 0.0504(6) Uani 1 1 d . . . . .
C28 C 0.3514(4) 0.0105(2) 0.59328(18) 0.0573(7) Uani 1 1 d . . . . .
H28A H 0.4056 0.0144 0.6516 0.086 Uiso 1 1 calc R U . . .
H28B H 0.4212 -0.0338 0.5604 0.086 Uiso 1 1 calc R U . . .
H28C H 0.2416 -0.0258 0.5910 0.086 Uiso 1 1 calc R U . . .
C26 C -0.1482(4) 0.6271(3) 0.8281(3) 0.0761(9) Uani 1 1 d . . . . .
H26A H -0.1051 0.7016 0.8151 0.114 Uiso 1 1 calc R U . . .
H26B H -0.1312 0.6159 0.8889 0.114 Uiso 1 1 calc R U . . .
H26C H -0.2680 0.6228 0.8068 0.114 Uiso 1 1 calc R U . . .
C21 C -0.0698(4) 0.3407(4) 0.9527(2) 0.0811(11) Uani 1 1 d . . . . .
H21 H -0.1292 0.3042 0.9050 0.097 Uiso 1 1 calc R U . . .
C31 C 0.3943(5) 0.8115(2) 0.7983(3) 0.0764(9) Uani 1 1 d . . . . .
H31A H 0.4965 0.7832 0.8322 0.115 Uiso 1 1 calc R U . . .
H31B H 0.3194 0.8428 0.8352 0.115 Uiso 1 1 calc R U . . .
H31C H 0.4233 0.8707 0.7604 0.115 Uiso 1 1 calc R U . . .
C24 C -0.1596(5) -0.0740(3) 0.7009(2) 0.0749(9) Uani 1 1 d . . . . .
H24A H -0.2571 -0.1155 0.6730 0.112 Uiso 1 1 calc R U . . .
H24B H -0.1857 -0.0420 0.7535 0.112 Uiso 1 1 calc R U . . .
H24C H -0.0642 -0.1258 0.7127 0.112 Uiso 1 1 calc R U . . .
C23 C -0.0179(5) 0.4337(4) 1.0702(2) 0.0826(11) Uani 1 1 d . . . . .
H23 H -0.0320 0.4737 1.1197 0.099 Uiso 1 1 calc 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
O8 C27 1.350(3) . ?
O8 C11 1.450(2) . ?
O6 C25 1.344(3) . ?
O6 C12 1.447(2) . ?
O3 C7 1.326(3) . ?
O3 C24 1.442(4) . ?
O7 C25 1.188(3) . ?
O4 C15 1.431(3) . ?
O4 H4 0.8200 . ?
O2 C7 1.207(3) . ?
O1 C3 1.209(3) . ?
C14 C8 1.329(3) . ?
C14 C13 1.523(3) . ?
C14 C15 1.527(3) . ?
C13 C12 1.529(3) . ?
C13 C18 1.538(3) . ?
C13 C17 1.558(3) . ?
C12 C11 1.525(3) . ?
C12 H12 0.9800 . ?
C30 C8 1.512(3) . ?
C30 C2 1.567(3) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C17 C20 1.497(3) . ?
C17 C16 1.536(3) . ?
C17 H17 0.9800 . ?
O9 C27 1.198(3) . ?
C10 C19 1.323(3) . ?
C10 C1 1.511(3) . ?
C10 C5 1.513(3) . ?
C1 C9 1.556(3) . ?
C1 C2 1.557(3) . ?
C1 H1 0.9800 . ?
C9 C8 1.512(3) . ?
C9 C11 1.531(3) . ?
C9 H9 0.9800 . ?
C4 C29 1.536(3) . ?
C4 C28 1.536(3) . ?
C4 C3 1.541(3) . ?
C4 C5 1.562(3) . ?
C25 C26 1.496(4) . ?
C11 H11 0.9800 . ?
C6 C7 1.497(3) . ?
C6 C5 1.533(3) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C3 C2 1.515(3) . ?
C15 C16 1.534(3) . ?
C15 H15 0.9800 . ?
C27 C31 1.498(4) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C2 H2 0.9800 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C5 H5 0.9800 . ?
C19 H19A 0.9300 . ?
C19 H19B 0.9300 . ?
C22 C23 1.329(5) . ?
C22 C20 1.424(4) . ?
C22 H22 0.9300 . ?
O5 C23 1.340(5) . ?
O5 C21 1.358(4) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C20 C21 1.336(4) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C21 H21 0.9300 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C23 H23 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
C27 O8 C11 117.51(18) . . ?
C25 O6 C12 117.47(17) . . ?
C7 O3 C24 117.3(2) . . ?
C15 O4 H4 109.5 . . ?
C8 C14 C13 121.67(19) . . ?
C8 C14 C15 127.86(19) . . ?
C13 C14 C15 110.09(18) . . ?
C14 C13 C12 107.68(16) . . ?
C14 C13 C18 111.49(17) . . ?
C12 C13 C18 112.73(18) . . ?
C14 C13 C17 100.34(17) . . ?
C12 C13 C17 111.09(17) . . ?
C18 C13 C17 112.75(17) . . ?
O6 C12 C11 108.47(16) . . ?
O6 C12 C13 108.07(16) . . ?
C11 C12 C13 115.93(16) . . ?
O6 C12 H12 108.0 . . ?
C11 C12 H12 108.0 . . ?
C13 C12 H12 108.0 . . ?
C8 C30 C2 105.19(17) . . ?
C8 C30 H30A 110.7 . . ?
C2 C30 H30A 110.7 . . ?
C8 C30 H30B 110.7 . . ?
C2 C30 H30B 110.7 . . ?
H30A C30 H30B 108.8 . . ?
C20 C17 C16 116.2(2) . . ?
C20 C17 C13 118.2(2) . . ?
C16 C17 C13 102.96(18) . . ?
C20 C17 H17 106.2 . . ?
C16 C17 H17 106.2 . . ?
C13 C17 H17 106.2 . . ?
C19 C10 C1 120.6(2) . . ?
C19 C10 C5 124.9(2) . . ?
C1 C10 C5 114.34(18) . . ?
C10 C1 C9 113.26(16) . . ?
C10 C1 C2 111.96(18) . . ?
C9 C1 C2 102.87(16) . . ?
C10 C1 H1 109.5 . . ?
C9 C1 H1 109.5 . . ?
C2 C1 H1 109.5 . . ?
C8 C9 C11 116.42(17) . . ?
C8 C9 C1 103.61(16) . . ?
C11 C9 C1 115.62(17) . . ?
C8 C9 H9 106.9 . . ?
C11 C9 H9 106.9 . . ?
C1 C9 H9 106.9 . . ?
C14 C8 C9 124.19(18) . . ?
C14 C8 C30 128.2(2) . . ?
C9 C8 C30 107.26(18) . . ?
C29 C4 C28 109.0(2) . . ?
C29 C4 C3 107.50(19) . . ?
C28 C4 C3 107.6(2) . . ?
C29 C4 C5 112.32(19) . . ?
C28 C4 C5 111.10(18) . . ?
C3 C4 C5 109.14(17) . . ?
O7 C25 O6 123.9(2) . . ?
O7 C25 C26 126.0(2) . . ?
O6 C25 C26 110.0(2) . . ?
O8 C11 C12 109.82(16) . . ?
O8 C11 C9 108.29(16) . . ?
C12 C11 C9 111.53(16) . . ?
O8 C11 H11 109.1 . . ?
C12 C11 H11 109.1 . . ?
C9 C11 H11 109.1 . . ?
C7 C6 C5 114.03(19) . . ?
C7 C6 H6A 108.7 . . ?
C5 C6 H6A 108.7 . . ?
C7 C6 H6B 108.7 . . ?
C5 C6 H6B 108.7 . . ?
H6A C6 H6B 107.6 . . ?
O1 C3 C2 120.2(2) . . ?
O1 C3 C4 120.1(2) . . ?
C2 C3 C4 119.73(18) . . ?
O4 C15 C14 113.20(17) . . ?
O4 C15 C16 112.49(19) . . ?
C14 C15 C16 103.92(18) . . ?
O4 C15 H15 109.0 . . ?
C14 C15 H15 109.0 . . ?
C16 C15 H15 109.0 . . ?
O9 C27 O8 124.3(3) . . ?
O9 C27 C31 125.5(3) . . ?
O8 C27 C31 110.2(2) . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C13 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C3 C2 C1 112.58(18) . . ?
C3 C2 C30 112.39(19) . . ?
C1 C2 C30 106.67(17) . . ?
C3 C2 H2 108.4 . . ?
C1 C2 H2 108.4 . . ?
C30 C2 H2 108.4 . . ?
C15 C16 C17 104.65(18) . . ?
C15 C16 H16A 110.8 . . ?
C17 C16 H16A 110.8 . . ?
C15 C16 H16B 110.8 . . ?
C17 C16 H16B 110.8 . . ?
H16A C16 H16B 108.9 . . ?
C10 C5 C6 112.84(18) . . ?
C10 C5 C4 107.32(16) . . ?
C6 C5 C4 115.63(19) . . ?
C10 C5 H5 106.9 . . ?
C6 C5 H5 106.9 . . ?
C4 C5 H5 106.9 . . ?
O2 C7 O3 122.9(2) . . ?
O2 C7 C6 125.6(2) . . ?
O3 C7 C6 111.4(2) . . ?
C10 C19 H19A 120.0 . . ?
C10 C19 H19B 120.0 . . ?
H19A C19 H19B 120.0 . . ?
C23 C22 C20 107.2(3) . . ?
C23 C22 H22 126.4 . . ?
C20 C22 H22 126.4 . . ?
C23 O5 C21 104.6(3) . . ?
C4 C29 H29A 109.5 . . ?
C4 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C4 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C21 C20 C22 103.8(3) . . ?
C21 C20 C17 125.5(3) . . ?
C22 C20 C17 130.7(3) . . ?
C4 C28 H28A 109.5 . . ?
C4 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C4 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
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 . . ?
C20 C21 O5 112.8(3) . . ?
C20 C21 H21 123.6 . . ?
O5 C21 H21 123.6 . . ?
C27 C31 H31A 109.5 . . ?
C27 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C27 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O3 C24 H24A 109.5 . . ?
O3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
O3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C23 O5 111.6(3) . . ?
C22 C23 H23 124.2 . . ?
O5 C23 H23 124.2 . . ?

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
O4 H4 O2 0.82 2.10 2.908(3) 169.3 .

_refine_diff_density_max         0.143
_refine_diff_density_min         -0.177
_refine_diff_density_rms         0.036

_shelxl_version_number           2013-4



####################################################################### 
# 
# 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_shelxl_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1532038'
_audit_update_record             
;
2017-05-19 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H38 O9'
_chemical_formula_weight         554.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 '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                   14.68150(10)
_cell_length_b                   17.2043(2)
_cell_length_c                   23.1115(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5837.62(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    21524
_cell_measurement_theta_min      3.9330
_cell_measurement_theta_max      71.2150

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_F_000             2368
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    0.760
_shelx_estimated_absorpt_T_min   0.863
_shelx_estimated_absorpt_T_max   0.901
_exptl_absorpt_correction_T_min  0.67687
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      291(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.2169
_diffrn_reflns_number            42142
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.567
_diffrn_reflns_theta_max         71.336
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             11193
_reflns_number_gt                10110
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.811
_reflns_Friedel_fraction_max     0.983
_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       'CrysAlisPro (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 (L. J. Farrugia, 2001)'
_computing_publication_material  SHELXL-97

_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)+(0.1220P)²+1.3538P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 4197 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.02(5)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         11193
_refine_ls_number_parameters     735
_refine_ls_number_restraints     59
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0635
_refine_ls_wR_factor_ref         0.1891
_refine_ls_wR_factor_gt          0.1821
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.119
_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
O6 O 0.29865(19) 0.51076(15) 0.45619(12) 0.0553(6) Uani 1 1 d . . . . .
O8 O 0.11849(19) 0.47993(17) 0.44620(12) 0.0591(6) Uani 1 1 d . . . . .
O15 O 0.7728(3) 0.73694(16) 0.63302(12) 0.0678(8) Uani 1 1 d . . . . .
O1 O 0.3662(2) 0.14495(18) 0.56879(13) 0.0675(8) Uani 1 1 d . . . . .
O4 O 0.2568(2) 0.20875(17) 0.33437(13) 0.0660(7) Uani 1 1 d . . . . .
O3 O 0.1917(2) 0.4504(2) 0.63793(15) 0.0787(9) Uani 1 1 d . . . . .
O12 O 0.9030(3) 0.4107(2) 0.59974(19) 0.0876(11) Uani 1 1 d . . . . .
C8 C 0.1439(2) 0.3170(2) 0.41323(16) 0.0483(7) Uani 1 1 d . . . . .
C10 C 0.1738(2) 0.2809(2) 0.51044(15) 0.0455(7) Uani 1 1 d . . . . .
C1 C 0.2553(2) 0.25499(19) 0.47012(14) 0.0425(6) Uani 1 1 d . . . . .
H1 H 0.2409 0.2014 0.4590 0.051 Uiso 1 1 calc R U . . .
C49 C 0.9080(3) 0.5972(2) 0.67250(18) 0.0574(9) Uani 1 1 d . . . . .
H49 H 0.8748 0.5889 0.7088 0.069 Uiso 1 1 calc R U . . .
C12 C 0.2726(2) 0.4299(2) 0.46190(15) 0.0466(7) Uani 1 1 d . . . . .
H12 H 0.3095 0.4071 0.4929 0.056 Uiso 1 1 calc R U . . .
O2 O 0.1270(3) 0.3791(3) 0.70608(15) 0.0938(12) Uani 1 1 d . . . . .
C13 C 0.2927(2) 0.38505(19) 0.40633(15) 0.0437(7) Uani 1 1 d . . . . .
C15 C 0.2906(3) 0.2596(2) 0.36300(16) 0.0492(7) Uani 1 1 d . . . . .
C3 C 0.3301(2) 0.2064(2) 0.55864(16) 0.0494(8) Uani 1 1 d . . . . .
C9 C 0.1281(2) 0.3468(2) 0.47395(15) 0.0478(7) Uani 1 1 d . . . . .
H9 H 0.0627 0.3494 0.4823 0.057 Uiso 1 1 calc R U . . .
O14 O 0.6918(4) 0.6750(3) 0.53902(17) 0.1167(18) Uani 1 1 d . U . . .
C14 C 0.2456(2) 0.30363(19) 0.41203(14) 0.0434(7) Uani 1 1 d . . . . .
C47 C 0.7515(3) 0.6546(2) 0.63518(17) 0.0575(9) Uani 1 1 d . . . . .
H47 H 0.7313 0.6425 0.6746 0.069 Uiso 1 1 calc R U . . .
C17 C 0.3948(2) 0.3610(2) 0.39598(16) 0.0494(8) Uani 1 1 d . . . . .
H17 H 0.4188 0.3420 0.4329 0.059 Uiso 1 1 calc R U . . .
C2 C 0.3468(2) 0.2492(2) 0.50265(16) 0.0477(7) Uani 1 1 d . . . . .
H2A H 0.3910 0.2214 0.4793 0.057 Uiso 1 1 calc R U . . .
H2B H 0.3704 0.3008 0.5105 0.057 Uiso 1 1 calc R U . . .
C5 C 0.2066(2) 0.3070(2) 0.57115(15) 0.0480(7) Uani 1 1 d . . . . .
H5 H 0.2439 0.3534 0.5647 0.058 Uiso 1 1 calc R U . . .
C7 C 0.1470(3) 0.3880(3) 0.65700(18) 0.0622(10) Uani 1 1 d . . . . .
O5 O 0.5454(4) 0.4977(3) 0.3173(2) 0.1220(17) Uani 1 1 d . . . . .
C11 C 0.1720(2) 0.4271(2) 0.48121(16) 0.0490(7) Uani 1 1 d . . . . .
H11 H 0.1678 0.4428 0.5219 0.059 Uiso 1 1 calc R U . . .
C4 C 0.2701(2) 0.2476(2) 0.60273(15) 0.0527(8) Uani 1 1 d . . . . .
C18 C 0.2568(3) 0.4275(2) 0.35258(16) 0.0528(8) Uani 1 1 d . . . . .
H18A H 0.1943 0.4419 0.3586 0.079 Uiso 1 1 calc R U . . .
H18B H 0.2611 0.3938 0.3196 0.079 Uiso 1 1 calc R U . . .
H18C H 0.2925 0.4734 0.3459 0.079 Uiso 1 1 calc R U . . .
C51 C 0.8891(3) 0.4740(3) 0.6210(2) 0.0670(11) Uani 1 1 d . . . . .
C48 C 0.8349(3) 0.6051(2) 0.62260(16) 0.0576(9) Uani 1 1 d . . . . .
O7 O 0.3717(5) 0.5047(3) 0.5402(2) 0.140(2) Uani 1 1 d . . . . .
C6 C 0.1248(3) 0.3342(3) 0.60841(17) 0.0581(9) Uani 1 1 d . . . . .
H6A H 0.0813 0.3598 0.5832 0.070 Uiso 1 1 calc R U . . .
H6B H 0.0951 0.2886 0.6243 0.070 Uiso 1 1 calc R U . . .
C20 C 0.4587(3) 0.4231(3) 0.3747(2) 0.0609(9) Uani 1 1 d . . . . .
O10 O 0.6667(4) 0.4199(3) 0.7942(3) 0.1295(19) Uani 1 1 d . . . . .
O13 O 1.0927(4) 0.7414(4) 0.6817(3) 0.1311(19) Uani 1 1 d . U . . .
C38 C 0.7416(3) 0.5027(3) 0.72741(18) 0.0626(9) Uani 1 1 d . . . . .
H38A H 0.7966 0.4787 0.7423 0.075 Uiso 1 1 calc R U . . .
H38B H 0.7456 0.5583 0.7337 0.075 Uiso 1 1 calc R U . . .
C19 C 0.1069(3) 0.2133(2) 0.51492(18) 0.0566(9) Uani 1 1 d . . . . .
H19A H 0.0763 0.2066 0.4786 0.085 Uiso 1 1 calc R U . . .
H19B H 0.0629 0.2241 0.5446 0.085 Uiso 1 1 calc R U . . .
H19C H 0.1394 0.1666 0.5245 0.085 Uiso 1 1 calc R U . . .
C37 C 0.7316(3) 0.4853(2) 0.66219(18) 0.0598(9) Uani 1 1 d . . . . .
H37 H 0.7374 0.4288 0.6589 0.072 Uiso 1 1 calc R U . . .
C44 C 0.8012(3) 0.5194(2) 0.61615(18) 0.0598(9) Uani 1 1 d . . . . .
C53 C 0.9711(3) 0.6646(3) 0.6817(2) 0.0678(11) Uani 1 1 d . . . . .
C16 C 0.3861(3) 0.2908(2) 0.3555(2) 0.0607(9) Uani 1 1 d . . . . .
H16A H 0.3962 0.3064 0.3157 0.073 Uiso 1 1 calc R U . . .
H16B H 0.4306 0.2514 0.3656 0.073 Uiso 1 1 calc R U . . .
O16 O 0.6975(6) 0.7541(3) 0.7154(2) 0.142(3) Uani 1 1 d . . . . .
C36 C 0.6337(3) 0.5043(3) 0.6384(2) 0.0686(11) Uani 1 1 d . . . . .
O9 O 0.1033(6) 0.5599(4) 0.5206(2) 0.166(3) Uani 1 1 d . . . . .
C28 C 0.3376(3) 0.2925(3) 0.64190(18) 0.0670(11) Uani 1 1 d . . . . .
H28A H 0.3795 0.2566 0.6593 0.100 Uiso 1 1 calc R U . . .
H28B H 0.3044 0.3192 0.6717 0.100 Uiso 1 1 calc R U . . .
H28C H 0.3707 0.3296 0.6190 0.100 Uiso 1 1 calc R U . . .
C54 C 0.9539(4) 0.7314(3) 0.7160(2) 0.0815(13) Uani 1 1 d . . . . .
H54 H 0.9002 0.7419 0.7358 0.098 Uiso 1 1 calc R U . . .
C33 C 0.6590(4) 0.4701(3) 0.7582(3) 0.0848(15) Uani 1 1 d . . . . .
C45 C 0.7417(4) 0.5143(3) 0.56322(19) 0.0705(11) Uani 1 1 d . . . . .
C57 C 0.7367(5) 0.7803(3) 0.6760(2) 0.0871(17) Uani 1 1 d . . . . .
C30 C 0.0821(3) 0.3027(3) 0.37308(19) 0.0611(10) Uani 1 1 d . . . . .
H30A H 0.0207 0.3110 0.3809 0.073 Uiso 1 1 calc R U . . .
H30B H 0.1000 0.2843 0.3370 0.073 Uiso 1 1 calc R U . . .
C55 C 1.0272(6) 0.7763(4) 0.7151(3) 0.1008(18) Uani 1 1 d . U . . .
H55 H 1.0332 0.8238 0.7340 0.121 Uiso 1 1 calc R U . . .
C29 C 0.2211(3) 0.1871(3) 0.6410(2) 0.0776(13) Uani 1 1 d . . . . .
H29A H 0.1722 0.1639 0.6196 0.116 Uiso 1 1 calc R U . . .
H29B H 0.1970 0.2123 0.6748 0.116 Uiso 1 1 calc R U . . .
H29C H 0.2635 0.1476 0.6525 0.116 Uiso 1 1 calc R U . . .
C35 C 0.5735(3) 0.5467(3) 0.6835(3) 0.0844(17) Uani 1 1 d . . . . .
H35 H 0.6041 0.5964 0.6908 0.101 Uiso 1 1 calc R U . . .
C25 C 0.3451(4) 0.5421(3) 0.4999(3) 0.0851(15) Uani 1 1 d . . . . .
C52 C 0.8843(5) 0.6319(3) 0.5673(2) 0.0822(14) Uani 1 1 d . . . . .
H52A H 0.9086 0.6831 0.5731 0.123 Uiso 1 1 calc R U . . .
H52B H 0.8420 0.6328 0.5356 0.123 Uiso 1 1 calc R U . . .
H52C H 0.9331 0.5966 0.5587 0.123 Uiso 1 1 calc R U . . .
C46 C 0.6713(4) 0.6390(3) 0.5942(2) 0.0818(15) Uani 1 1 d . . . . .
H46 H 0.6160 0.6623 0.6103 0.098 Uiso 1 1 calc R U . . .
C34 C 0.5677(4) 0.5058(4) 0.7436(3) 0.096(2) Uani 1 1 d . . . . .
C27 C 0.0823(5) 0.5402(4) 0.4717(2) 0.107(2) Uani 1 1 d . . . . .
C50 C 0.9556(3) 0.5206(3) 0.6572(3) 0.0756(12) Uani 1 1 d . . . . .
H50A H 1.0109 0.5306 0.6356 0.091 Uiso 1 1 calc R U . . .
H50B H 0.9713 0.4923 0.6922 0.091 Uiso 1 1 calc R U . . .
C64 C 0.7601(6) 0.4839(3) 0.5122(2) 0.0938(17) Uani 1 1 d . . . . .
H64A H 0.7160 0.4839 0.4833 0.113 Uiso 1 1 calc R U . . .
H64B H 0.8172 0.4625 0.5050 0.113 Uiso 1 1 calc R U . . .
C43 C 0.6546(4) 0.5513(3) 0.5832(2) 0.0802(15) Uani 1 1 d . . . . .
H43 H 0.6064 0.5439 0.5544 0.096 Uiso 1 1 calc R U . . .
C22 C 0.5121(4) 0.4734(4) 0.4094(3) 0.0825(14) Uani 1 1 d . . . . .
H22 H 0.5123 0.4754 0.4496 0.099 Uiso 1 1 calc R U . . .
C23 C 0.5620(5) 0.5172(4) 0.3739(4) 0.104(2) Uani 1 1 d . . . . .
H23 H 0.6024 0.5556 0.3858 0.125 Uiso 1 1 calc R U . . .
C24 C 0.2224(5) 0.5048(4) 0.6806(4) 0.108(2) Uani 1 1 d . . . . .
H24A H 0.2585 0.5443 0.6623 0.162 Uiso 1 1 calc R U . . .
H24B H 0.2585 0.4782 0.7090 0.162 Uiso 1 1 calc R U . . .
H24C H 0.1708 0.5283 0.6991 0.162 Uiso 1 1 calc R U . . .
C58 C 0.7599(7) 0.8642(3) 0.6675(3) 0.112(3) Uani 1 1 d . . . . .
H58A H 0.8248 0.8708 0.6694 0.168 Uiso 1 1 calc R U . . .
H58B H 0.7315 0.8947 0.6972 0.168 Uiso 1 1 calc R U . . .
H58C H 0.7384 0.8810 0.6303 0.168 Uiso 1 1 calc R U . . .
C21 C 0.4824(5) 0.4401(5) 0.3203(3) 0.099(2) Uani 1 1 d . . . . .
H21 H 0.4584 0.4152 0.2880 0.118 Uiso 1 1 calc R U . . .
C56 C 1.0569(5) 0.6737(4) 0.6629(3) 0.104(2) Uani 1 1 d . . . . .
H56 H 1.0877 0.6380 0.6399 0.125 Uiso 1 1 calc R U . . .
C61 C 0.5886(4) 0.4272(3) 0.6194(3) 0.0875(16) Uani 1 1 d . . . . .
H61A H 0.6205 0.4065 0.5866 0.131 Uiso 1 1 calc R U . . .
H61B H 0.5262 0.4366 0.6091 0.131 Uiso 1 1 calc R U . . .
H61C H 0.5910 0.3905 0.6507 0.131 Uiso 1 1 calc R U . . .
C39 C 0.5539(5) 0.5701(6) 0.7910(3) 0.126(3) Uani 1 1 d . . . . .
H39A H 0.5593 0.5471 0.8287 0.189 Uiso 1 1 calc R U . . .
H39B H 0.4945 0.5927 0.7869 0.189 Uiso 1 1 calc R U . . .
H39C H 0.5994 0.6097 0.7865 0.189 Uiso 1 1 calc R U . . .
C26 C 0.3643(7) 0.6266(4) 0.4883(4) 0.124(3) Uani 1 1 d . . . . .
H26A H 0.3866 0.6325 0.4495 0.186 Uiso 1 1 calc R U . . .
H26B H 0.4093 0.6451 0.5152 0.186 Uiso 1 1 calc R U . . .
H26C H 0.3092 0.6561 0.4929 0.186 Uiso 1 1 calc R U . . .
C41 C 0.4802(4) 0.5683(5) 0.6572(4) 0.122(3) Uani 1 1 d . . . . .
H41A H 0.4849 0.5671 0.6153 0.147 Uiso 1 1 calc R U . . .
H41B H 0.4357 0.5295 0.6686 0.147 Uiso 1 1 calc R U . . .
C59 C 0.6212(10) 0.7058(7) 0.5084(5) 0.178(5) Uani 1 1 d D U . . .
C31 C 0.0224(7) 0.5840(6) 0.4311(3) 0.146(4) Uani 1 1 d . . . . .
H31A H 0.0592 0.6167 0.4068 0.219 Uiso 1 1 calc R U . . .
H31B H -0.0193 0.6156 0.4527 0.219 Uiso 1 1 calc R U . . .
H31C H -0.0110 0.5480 0.4075 0.219 Uiso 1 1 calc R U . . .
C40 C 0.4921(6) 0.4450(7) 0.7515(5) 0.159(5) Uani 1 1 d . . . . .
H40A H 0.4923 0.4100 0.7191 0.239 Uiso 1 1 calc R U . . .
H40B H 0.4342 0.4707 0.7538 0.239 Uiso 1 1 calc R U . . .
H40C H 0.5027 0.4163 0.7865 0.239 Uiso 1 1 calc R U . . .
C60 C 0.6512(13) 0.7370(7) 0.4552(5) 0.218(7) Uani 1 1 d . U . . .
H60A H 0.6575 0.7924 0.4587 0.262 Uiso 1 1 calc R U . . .
H60B H 0.6075 0.7253 0.4256 0.262 Uiso 1 1 calc R U . . .
H60C H 0.7089 0.7146 0.4452 0.262 Uiso 1 1 calc R U . . .
C42 C 0.4465(5) 0.6472(6) 0.6754(5) 0.162(4) Uani 1 1 d D U . . .
O19 O 0.5522(9) 0.7188(10) 0.5352(7) 0.301(8) Uani 1 1 d D U . . .
O18 O 0.3606(5) 0.6519(5) 0.6894(5) 0.233(4) Uani 1 1 d D U . . .
O17 O 0.4904(7) 0.7040(5) 0.6808(6) 0.218(4) Uani 1 1 d D U . . .
C63 C 0.3337(12) 0.7348(6) 0.6960(9) 0.259(9) Uani 1 1 d D U . . .
H63A H 0.2970 0.7502 0.6636 0.311 Uiso 1 1 calc R U . . .
H63B H 0.3873 0.7666 0.6977 0.311 Uiso 1 1 calc R U . . .
H63C H 0.2993 0.7410 0.7311 0.311 Uiso 1 1 calc 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
O6 C25 1.334(6) . ?
O6 C12 1.448(4) . ?
O8 C27 1.307(6) . ?
O8 C11 1.449(4) . ?
O15 C57 1.351(6) . ?
O15 C47 1.452(5) . ?
O1 C3 1.206(5) . ?
O4 C15 1.204(5) . ?
O3 C7 1.334(6) . ?
O3 C24 1.432(7) . ?
O12 C51 1.212(6) . ?
C8 C30 1.320(5) . ?
C8 C9 1.512(5) . ?
C8 C14 1.512(5) . ?
C10 C19 1.526(5) . ?
C10 C5 1.550(5) . ?
C10 C9 1.563(5) . ?
C10 C1 1.582(4) . ?
C1 C2 1.542(4) . ?
C1 C14 1.588(4) . ?
C1 H1 0.9800 . ?
C49 C53 1.500(7) . ?
C49 C50 1.533(6) . ?
C49 C48 1.581(6) . ?
C49 H49 0.9800 . ?
C12 C13 1.527(5) . ?
C12 C11 1.544(5) . ?
C12 H12 0.9800 . ?
O2 C7 1.182(5) . ?
C13 C18 1.534(5) . ?
C13 C14 1.567(5) . ?
C13 C17 1.574(5) . ?
C15 C16 1.512(6) . ?
C15 C14 1.514(5) . ?
C3 C2 1.509(5) . ?
C3 C4 1.521(5) . ?
C9 C11 1.534(5) . ?
C9 H9 0.9800 . ?
O14 C59 1.362(13) . ?
O14 C46 1.450(8) . ?
C47 C48 1.520(6) . ?
C47 C46 1.535(7) . ?
C47 H47 0.9800 . ?
C17 C20 1.504(5) . ?
C17 C16 1.533(6) . ?
C17 H17 0.9800 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C5 C6 1.551(5) . ?
C5 C4 1.565(5) . ?
C5 H5 0.9800 . ?
C7 C6 1.491(6) . ?
O5 C21 1.357(7) . ?
O5 C23 1.371(10) . ?
C11 H11 0.9800 . ?
C4 C29 1.544(6) . ?
C4 C28 1.549(6) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C51 C44 1.513(6) . ?
C51 C50 1.515(8) . ?
C48 C52 1.541(6) . ?
C48 C44 1.563(6) . ?
O7 C25 1.196(8) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C20 C21 1.337(7) . ?
C20 C22 1.418(7) . ?
O10 C33 1.204(8) . ?
O13 C56 1.350(9) . ?
O13 C55 1.371(10) . ?
C38 C33 1.514(7) . ?
C38 C37 1.543(6) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C37 C36 1.573(6) . ?
C37 C44 1.587(6) . ?
C37 H37 0.9800 . ?
C44 C45 1.505(6) . ?
C53 C56 1.341(8) . ?
C53 C54 1.419(8) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
O16 C57 1.168(7) . ?
C36 C43 1.541(8) . ?
C36 C61 1.547(6) . ?
C36 C35 1.550(7) . ?
O9 C27 1.219(9) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C54 C55 1.325(9) . ?
C54 H54 0.9300 . ?
C33 C34 1.514(10) . ?
C45 C64 1.318(7) . ?
C45 C43 1.501(8) . ?
C57 C58 1.496(8) . ?
C30 H30A 0.9300 . ?
C30 H30B 0.9300 . ?
C55 H55 0.9300 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C35 C41 1.545(8) . ?
C35 C34 1.559(10) . ?
C35 H35 0.9800 . ?
C25 C26 1.504(9) . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C46 C43 1.550(7) . ?
C46 H46 0.9800 . ?
C34 C40 1.535(9) . ?
C34 C39 1.570(8) . ?
C27 C31 1.491(8) . ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
C64 H64A 0.9300 . ?
C64 H64B 0.9300 . ?
C43 H43 0.9800 . ?
C22 C23 1.334(8) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
C21 H21 0.9300 . ?
C56 H56 0.9300 . ?
C61 H61A 0.9600 . ?
C61 H61B 0.9600 . ?
C61 H61C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C41 C42 1.504(11) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C59 O19 1.207(7) . ?
C59 C60 1.413(17) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C60 H60A 0.9600 . ?
C60 H60B 0.9600 . ?
C60 H60C 0.9600 . ?
C42 O17 1.179(6) . ?
C42 O18 1.304(6) . ?
O18 C63 1.487(6) . ?
C63 H63A 0.9600 . ?
C63 H63B 0.9600 . ?
C63 H63C 0.9600 . ?

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
C25 O6 C12 117.0(4) . . ?
C27 O8 C11 117.8(4) . . ?
C57 O15 C47 115.4(4) . . ?
C7 O3 C24 117.0(5) . . ?
C30 C8 C9 127.6(4) . . ?
C30 C8 C14 129.6(4) . . ?
C9 C8 C14 102.7(3) . . ?
C19 C10 C5 111.1(3) . . ?
C19 C10 C9 108.2(3) . . ?
C5 C10 C9 114.3(3) . . ?
C19 C10 C1 108.2(3) . . ?
C5 C10 C1 112.3(3) . . ?
C9 C10 C1 102.2(3) . . ?
C2 C1 C10 113.0(3) . . ?
C2 C1 C14 121.6(3) . . ?
C10 C1 C14 106.3(3) . . ?
C2 C1 H1 104.8 . . ?
C10 C1 H1 104.8 . . ?
C14 C1 H1 104.8 . . ?
C53 C49 C50 114.6(4) . . ?
C53 C49 C48 117.1(4) . . ?
C50 C49 C48 102.4(4) . . ?
C53 C49 H49 107.4 . . ?
C50 C49 H49 107.4 . . ?
C48 C49 H49 107.4 . . ?
O6 C12 C13 111.0(3) . . ?
O6 C12 C11 108.0(3) . . ?
C13 C12 C11 114.3(3) . . ?
O6 C12 H12 107.8 . . ?
C13 C12 H12 107.8 . . ?
C11 C12 H12 107.8 . . ?
C12 C13 C18 112.0(3) . . ?
C12 C13 C14 107.2(3) . . ?
C18 C13 C14 110.0(3) . . ?
C12 C13 C17 116.4(3) . . ?
C18 C13 C17 109.2(3) . . ?
C14 C13 C17 101.4(3) . . ?
O4 C15 C16 125.2(4) . . ?
O4 C15 C14 126.6(3) . . ?
C16 C15 C14 108.2(3) . . ?
O1 C3 C2 121.6(4) . . ?
O1 C3 C4 122.2(3) . . ?
C2 C3 C4 116.2(3) . . ?
C8 C9 C11 110.0(3) . . ?
C8 C9 C10 100.9(3) . . ?
C11 C9 C10 114.4(3) . . ?
C8 C9 H9 110.4 . . ?
C11 C9 H9 110.4 . . ?
C10 C9 H9 110.4 . . ?
C59 O14 C46 117.7(8) . . ?
C8 C14 C15 121.3(3) . . ?
C8 C14 C13 107.5(3) . . ?
C15 C14 C13 101.1(3) . . ?
C8 C14 C1 98.8(3) . . ?
C15 C14 C1 109.3(3) . . ?
C13 C14 C1 120.2(3) . . ?
O15 C47 C48 111.6(4) . . ?
O15 C47 C46 108.3(3) . . ?
C48 C47 C46 113.7(3) . . ?
O15 C47 H47 107.7 . . ?
C48 C47 H47 107.7 . . ?
C46 C47 H47 107.7 . . ?
C20 C17 C16 114.3(3) . . ?
C20 C17 C13 117.2(3) . . ?
C16 C17 C13 102.7(3) . . ?
C20 C17 H17 107.3 . . ?
C16 C17 H17 107.3 . . ?
C13 C17 H17 107.3 . . ?
C3 C2 C1 107.9(3) . . ?
C3 C2 H2A 110.1 . . ?
C1 C2 H2A 110.1 . . ?
C3 C2 H2B 110.1 . . ?
C1 C2 H2B 110.1 . . ?
H2A C2 H2B 108.4 . . ?
C10 C5 C6 110.4(3) . . ?
C10 C5 C4 114.7(3) . . ?
C6 C5 C4 113.6(3) . . ?
C10 C5 H5 105.8 . . ?
C6 C5 H5 105.8 . . ?
C4 C5 H5 105.8 . . ?
O2 C7 O3 123.0(5) . . ?
O2 C7 C6 126.0(5) . . ?
O3 C7 C6 111.0(3) . . ?
C21 O5 C23 104.6(5) . . ?
O8 C11 C9 106.0(3) . . ?
O8 C11 C12 109.7(3) . . ?
C9 C11 C12 113.5(3) . . ?
O8 C11 H11 109.2 . . ?
C9 C11 H11 109.2 . . ?
C12 C11 H11 109.2 . . ?
C3 C4 C29 109.9(4) . . ?
C3 C4 C28 104.7(3) . . ?
C29 C4 C28 107.4(4) . . ?
C3 C4 C5 109.7(3) . . ?
C29 C4 C5 115.4(3) . . ?
C28 C4 C5 109.1(3) . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C13 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O12 C51 C44 125.3(5) . . ?
O12 C51 C50 126.2(5) . . ?
C44 C51 C50 108.5(4) . . ?
C47 C48 C52 111.7(4) . . ?
C47 C48 C44 106.9(4) . . ?
C52 C48 C44 110.7(4) . . ?
C47 C48 C49 117.1(3) . . ?
C52 C48 C49 108.2(4) . . ?
C44 C48 C49 101.8(3) . . ?
C7 C6 C5 115.9(3) . . ?
C7 C6 H6A 108.3 . . ?
C5 C6 H6A 108.3 . . ?
C7 C6 H6B 108.3 . . ?
C5 C6 H6B 108.3 . . ?
H6A C6 H6B 107.4 . . ?
C21 C20 C22 104.8(4) . . ?
C21 C20 C17 128.7(5) . . ?
C22 C20 C17 126.3(4) . . ?
C56 O13 C55 106.6(5) . . ?
C33 C38 C37 108.2(4) . . ?
C33 C38 H38A 110.1 . . ?
C37 C38 H38A 110.1 . . ?
C33 C38 H38B 110.1 . . ?
C37 C38 H38B 110.1 . . ?
H38A C38 H38B 108.4 . . ?
C10 C19 H19A 109.5 . . ?
C10 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C10 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C38 C37 C36 112.9(4) . . ?
C38 C37 C44 121.5(4) . . ?
C36 C37 C44 106.1(4) . . ?
C38 C37 H37 105.0 . . ?
C36 C37 H37 105.0 . . ?
C44 C37 H37 105.0 . . ?
C45 C44 C51 121.7(4) . . ?
C45 C44 C48 108.4(4) . . ?
C51 C44 C48 102.1(4) . . ?
C45 C44 C37 98.6(4) . . ?
C51 C44 C37 108.0(3) . . ?
C48 C44 C37 119.2(3) . . ?
C56 C53 C54 104.7(5) . . ?
C56 C53 C49 128.7(5) . . ?
C54 C53 C49 126.5(4) . . ?
C15 C16 C17 106.7(3) . . ?
C15 C16 H16A 110.4 . . ?
C17 C16 H16A 110.4 . . ?
C15 C16 H16B 110.4 . . ?
C17 C16 H16B 110.4 . . ?
H16A C16 H16B 108.6 . . ?
C43 C36 C61 107.5(4) . . ?
C43 C36 C35 115.1(4) . . ?
C61 C36 C35 110.6(4) . . ?
C43 C36 C37 102.5(4) . . ?
C61 C36 C37 108.2(4) . . ?
C35 C36 C37 112.5(4) . . ?
C4 C28 H28A 109.5 . . ?
C4 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C4 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C55 C54 C53 108.6(6) . . ?
C55 C54 H54 125.7 . . ?
C53 C54 H54 125.7 . . ?
O10 C33 C34 121.9(6) . . ?
O10 C33 C38 121.0(6) . . ?
C34 C33 C38 117.0(5) . . ?
C64 C45 C43 128.2(5) . . ?
C64 C45 C44 129.2(5) . . ?
C43 C45 C44 102.7(3) . . ?
O16 C57 O15 123.7(4) . . ?
O16 C57 C58 126.0(5) . . ?
O15 C57 C58 110.2(5) . . ?
C8 C30 H30A 120.0 . . ?
C8 C30 H30B 120.0 . . ?
H30A C30 H30B 120.0 . . ?
C54 C55 O13 108.8(6) . . ?
C54 C55 H55 125.6 . . ?
O13 C55 H55 125.6 . . ?
C4 C29 H29A 109.5 . . ?
C4 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C4 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C41 C35 C36 110.7(5) . . ?
C41 C35 C34 114.3(6) . . ?
C36 C35 C34 114.7(5) . . ?
C41 C35 H35 105.4 . . ?
C36 C35 H35 105.4 . . ?
C34 C35 H35 105.4 . . ?
O7 C25 O6 122.6(5) . . ?
O7 C25 C26 126.7(5) . . ?
O6 C25 C26 110.6(5) . . ?
C48 C52 H52A 109.5 . . ?
C48 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C48 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O14 C46 C47 108.0(5) . . ?
O14 C46 C43 107.8(4) . . ?
C47 C46 C43 113.1(4) . . ?
O14 C46 H46 109.3 . . ?
C47 C46 H46 109.3 . . ?
C43 C46 H46 109.3 . . ?
C33 C34 C40 109.7(7) . . ?
C33 C34 C35 109.5(4) . . ?
C40 C34 C35 116.9(7) . . ?
C33 C34 C39 104.1(5) . . ?
C40 C34 C39 107.7(6) . . ?
C35 C34 C39 108.1(6) . . ?
O9 C27 O8 122.4(5) . . ?
O9 C27 C31 126.4(6) . . ?
O8 C27 C31 110.9(6) . . ?
C51 C50 C49 106.8(4) . . ?
C51 C50 H50A 110.4 . . ?
C49 C50 H50A 110.4 . . ?
C51 C50 H50B 110.4 . . ?
C49 C50 H50B 110.4 . . ?
H50A C50 H50B 108.6 . . ?
C45 C64 H64A 120.0 . . ?
C45 C64 H64B 120.0 . . ?
H64A C64 H64B 120.0 . . ?
C45 C43 C36 101.7(4) . . ?
C45 C43 C46 109.2(5) . . ?
C36 C43 C46 114.0(4) . . ?
C45 C43 H43 110.6 . . ?
C36 C43 H43 110.6 . . ?
C46 C43 H43 110.6 . . ?
C23 C22 C20 107.4(5) . . ?
C23 C22 H22 126.3 . . ?
C20 C22 H22 126.3 . . ?
C22 C23 O5 110.6(5) . . ?
C22 C23 H23 124.7 . . ?
O5 C23 H23 124.7 . . ?
O3 C24 H24A 109.5 . . ?
O3 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
O3 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C20 C21 O5 112.6(6) . . ?
C20 C21 H21 123.7 . . ?
O5 C21 H21 123.7 . . ?
C53 C56 O13 111.2(6) . . ?
C53 C56 H56 124.4 . . ?
O13 C56 H56 124.4 . . ?
C36 C61 H61A 109.5 . . ?
C36 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C36 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C34 C39 H39A 109.5 . . ?
C34 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C34 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
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 . . ?
C42 C41 C35 113.5(5) . . ?
C42 C41 H41A 108.9 . . ?
C35 C41 H41A 108.9 . . ?
C42 C41 H41B 108.9 . . ?
C35 C41 H41B 108.9 . . ?
H41A C41 H41B 107.7 . . ?
O19 C59 O14 116.4(11) . . ?
O19 C59 C60 129.6(13) . . ?
O14 C59 C60 111.2(13) . . ?
C27 C31 H31A 109.5 . . ?
C27 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C27 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C34 C40 H40A 109.5 . . ?
C34 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C34 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
O17 C42 O18 116.8(8) . . ?
O17 C42 C41 126.7(7) . . ?
O18 C42 C41 116.4(8) . . ?
C42 O18 C63 110.0(9) . . ?
O18 C63 H63A 109.5 . . ?
O18 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
O18 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 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
C19 C10 C1 C2 -114.0(3) . . . . ?
C5 C10 C1 C2 8.9(4) . . . . ?
C9 C10 C1 C2 131.9(3) . . . . ?
C19 C10 C1 C14 110.1(3) . . . . ?
C5 C10 C1 C14 -126.9(3) . . . . ?
C9 C10 C1 C14 -4.0(3) . . . . ?
C25 O6 C12 C13 -134.3(4) . . . . ?
C25 O6 C12 C11 99.7(4) . . . . ?
O6 C12 C13 C18 -48.5(4) . . . . ?
C11 C12 C13 C18 74.0(4) . . . . ?
O6 C12 C13 C14 -169.2(2) . . . . ?
C11 C12 C13 C14 -46.8(4) . . . . ?
O6 C12 C13 C17 78.1(4) . . . . ?
C11 C12 C13 C17 -159.4(3) . . . . ?
C30 C8 C9 C11 -115.8(4) . . . . ?
C14 C8 C9 C11 67.4(3) . . . . ?
C30 C8 C9 C10 123.0(4) . . . . ?
C14 C8 C9 C10 -53.8(3) . . . . ?
C19 C10 C9 C8 -80.4(3) . . . . ?
C5 C10 C9 C8 155.3(3) . . . . ?
C1 C10 C9 C8 33.7(3) . . . . ?
C19 C10 C9 C11 161.6(3) . . . . ?
C5 C10 C9 C11 37.2(4) . . . . ?
C1 C10 C9 C11 -84.4(3) . . . . ?
C30 C8 C14 C15 -8.2(6) . . . . ?
C9 C8 C14 C15 168.5(3) . . . . ?
C30 C8 C14 C13 107.2(5) . . . . ?
C9 C8 C14 C13 -76.1(3) . . . . ?
C30 C8 C14 C1 -127.2(4) . . . . ?
C9 C8 C14 C1 49.5(3) . . . . ?
O4 C15 C14 C8 -29.6(5) . . . . ?
C16 C15 C14 C8 150.0(3) . . . . ?
O4 C15 C14 C13 -148.2(4) . . . . ?
C16 C15 C14 C13 31.4(4) . . . . ?
O4 C15 C14 C1 84.1(4) . . . . ?
C16 C15 C14 C1 -96.3(3) . . . . ?
C12 C13 C14 C8 65.9(3) . . . . ?
C18 C13 C14 C8 -56.1(4) . . . . ?
C17 C13 C14 C8 -171.6(3) . . . . ?
C12 C13 C14 C15 -166.0(3) . . . . ?
C18 C13 C14 C15 72.0(3) . . . . ?
C17 C13 C14 C15 -43.5(3) . . . . ?
C12 C13 C14 C1 -45.8(4) . . . . ?
C18 C13 C14 C1 -167.8(3) . . . . ?
C17 C13 C14 C1 76.7(3) . . . . ?
C2 C1 C14 C8 -158.1(3) . . . . ?
C10 C1 C14 C8 -27.0(3) . . . . ?
C2 C1 C14 C15 74.2(4) . . . . ?
C10 C1 C14 C15 -154.7(3) . . . . ?
C2 C1 C14 C13 -41.9(4) . . . . ?
C10 C1 C14 C13 89.3(3) . . . . ?
C57 O15 C47 C48 -136.4(4) . . . . ?
C57 O15 C47 C46 97.7(5) . . . . ?
C12 C13 C17 C20 -77.9(4) . . . . ?
C18 C13 C17 C20 50.0(4) . . . . ?
C14 C13 C17 C20 166.1(3) . . . . ?
C12 C13 C17 C16 155.9(3) . . . . ?
C18 C13 C17 C16 -76.2(3) . . . . ?
C14 C13 C17 C16 39.9(3) . . . . ?
O1 C3 C2 C1 117.4(4) . . . . ?
C4 C3 C2 C1 -66.3(4) . . . . ?
C10 C1 C2 C3 45.8(4) . . . . ?
C14 C1 C2 C3 174.1(3) . . . . ?
C19 C10 C5 C6 -60.4(4) . . . . ?
C9 C10 C5 C6 62.4(4) . . . . ?
C1 C10 C5 C6 178.3(3) . . . . ?
C19 C10 C5 C4 69.5(4) . . . . ?
C9 C10 C5 C4 -167.7(3) . . . . ?
C1 C10 C5 C4 -51.8(4) . . . . ?
C24 O3 C7 O2 5.3(7) . . . . ?
C24 O3 C7 C6 -176.2(4) . . . . ?
C27 O8 C11 C9 123.1(5) . . . . ?
C27 O8 C11 C12 -113.9(5) . . . . ?
C8 C9 C11 O8 69.4(3) . . . . ?
C10 C9 C11 O8 -177.8(3) . . . . ?
C8 C9 C11 C12 -51.1(4) . . . . ?
C10 C9 C11 C12 61.7(4) . . . . ?
O6 C12 C11 O8 46.6(4) . . . . ?
C13 C12 C11 O8 -77.4(4) . . . . ?
O6 C12 C11 C9 165.1(3) . . . . ?
C13 C12 C11 C9 41.0(4) . . . . ?
O1 C3 C4 C29 -31.6(5) . . . . ?
C2 C3 C4 C29 152.2(3) . . . . ?
O1 C3 C4 C28 83.5(5) . . . . ?
C2 C3 C4 C28 -92.7(4) . . . . ?
O1 C3 C4 C5 -159.6(3) . . . . ?
C2 C3 C4 C5 24.2(4) . . . . ?
C10 C5 C4 C3 34.9(4) . . . . ?
C6 C5 C4 C3 163.2(3) . . . . ?
C10 C5 C4 C29 -89.9(4) . . . . ?
C6 C5 C4 C29 38.4(5) . . . . ?
C10 C5 C4 C28 149.0(3) . . . . ?
C6 C5 C4 C28 -82.6(4) . . . . ?
O15 C47 C48 C52 -49.8(5) . . . . ?
C46 C47 C48 C52 73.1(5) . . . . ?
O15 C47 C48 C44 -171.0(3) . . . . ?
C46 C47 C48 C44 -48.1(5) . . . . ?
O15 C47 C48 C49 75.7(4) . . . . ?
C46 C47 C48 C49 -161.4(4) . . . . ?
C53 C49 C48 C47 -77.6(5) . . . . ?
C50 C49 C48 C47 156.1(4) . . . . ?
C53 C49 C48 C52 49.6(5) . . . . ?
C50 C49 C48 C52 -76.7(4) . . . . ?
C53 C49 C48 C44 166.2(4) . . . . ?
C50 C49 C48 C44 40.0(4) . . . . ?
O2 C7 C6 C5 -126.3(5) . . . . ?
O3 C7 C6 C5 55.3(5) . . . . ?
C10 C5 C6 C7 -157.2(4) . . . . ?
C4 C5 C6 C7 72.3(5) . . . . ?
C16 C17 C20 C21 26.4(7) . . . . ?
C13 C17 C20 C21 -93.9(7) . . . . ?
C16 C17 C20 C22 -149.0(5) . . . . ?
C13 C17 C20 C22 90.7(6) . . . . ?
C33 C38 C37 C36 45.7(5) . . . . ?
C33 C38 C37 C44 173.3(4) . . . . ?
O12 C51 C44 C45 -32.2(7) . . . . ?
C50 C51 C44 C45 148.3(5) . . . . ?
O12 C51 C44 C48 -153.1(5) . . . . ?
C50 C51 C44 C48 27.4(5) . . . . ?
O12 C51 C44 C37 80.5(6) . . . . ?
C50 C51 C44 C37 -99.0(4) . . . . ?
C47 C48 C44 C45 65.8(4) . . . . ?
C52 C48 C44 C45 -56.0(5) . . . . ?
C49 C48 C44 C45 -170.8(3) . . . . ?
C47 C48 C44 C51 -164.5(3) . . . . ?
C52 C48 C44 C51 73.6(5) . . . . ?
C49 C48 C44 C51 -41.2(4) . . . . ?
C47 C48 C44 C37 -45.8(5) . . . . ?
C52 C48 C44 C37 -167.6(4) . . . . ?
C49 C48 C44 C37 77.6(4) . . . . ?
C38 C37 C44 C45 -158.0(4) . . . . ?
C36 C37 C44 C45 -27.4(4) . . . . ?
C38 C37 C44 C51 74.6(5) . . . . ?
C36 C37 C44 C51 -154.8(4) . . . . ?
C38 C37 C44 C48 -41.1(6) . . . . ?
C36 C37 C44 C48 89.5(4) . . . . ?
C50 C49 C53 C56 21.2(8) . . . . ?
C48 C49 C53 C56 -98.8(7) . . . . ?
C50 C49 C53 C54 -154.3(5) . . . . ?
C48 C49 C53 C54 85.7(6) . . . . ?
O4 C15 C16 C17 173.1(4) . . . . ?
C14 C15 C16 C17 -6.5(4) . . . . ?
C20 C17 C16 C15 -149.2(3) . . . . ?
C13 C17 C16 C15 -21.1(4) . . . . ?
C38 C37 C36 C43 132.2(4) . . . . ?
C44 C37 C36 C43 -3.2(4) . . . . ?
C38 C37 C36 C61 -114.5(5) . . . . ?
C44 C37 C36 C61 110.2(4) . . . . ?
C38 C37 C36 C35 8.0(6) . . . . ?
C44 C37 C36 C35 -127.3(4) . . . . ?
C56 C53 C54 C55 1.2(7) . . . . ?
C49 C53 C54 C55 177.6(5) . . . . ?
C37 C38 C33 O10 118.1(6) . . . . ?
C37 C38 C33 C34 -64.4(5) . . . . ?
C51 C44 C45 C64 -12.4(8) . . . . ?
C48 C44 C45 C64 105.3(6) . . . . ?
C37 C44 C45 C64 -129.8(6) . . . . ?
C51 C44 C45 C43 166.6(4) . . . . ?
C48 C44 C45 C43 -75.7(5) . . . . ?
C37 C44 C45 C43 49.1(4) . . . . ?
C47 O15 C57 O16 6.3(10) . . . . ?
C47 O15 C57 C58 -177.4(5) . . . . ?
C53 C54 C55 O13 -0.4(8) . . . . ?
C56 O13 C55 C54 -0.5(8) . . . . ?
C43 C36 C35 C41 59.9(7) . . . . ?
C61 C36 C35 C41 -62.1(7) . . . . ?
C37 C36 C35 C41 176.7(6) . . . . ?
C43 C36 C35 C34 -169.0(4) . . . . ?
C61 C36 C35 C34 69.0(5) . . . . ?
C37 C36 C35 C34 -52.1(6) . . . . ?
C12 O6 C25 O7 6.4(9) . . . . ?
C12 O6 C25 C26 -178.2(6) . . . . ?
C59 O14 C46 C47 -145.3(8) . . . . ?
C59 O14 C46 C43 92.1(8) . . . . ?
O15 C47 C46 O14 49.2(5) . . . . ?
C48 C47 C46 O14 -75.4(5) . . . . ?
O15 C47 C46 C43 168.4(5) . . . . ?
C48 C47 C46 C43 43.8(6) . . . . ?
O10 C33 C34 C40 -31.5(8) . . . . ?
C38 C33 C34 C40 151.0(6) . . . . ?
O10 C33 C34 C35 -161.1(5) . . . . ?
C38 C33 C34 C35 21.4(6) . . . . ?
O10 C33 C34 C39 83.5(7) . . . . ?
C38 C33 C34 C39 -94.0(6) . . . . ?
C41 C35 C34 C33 166.2(5) . . . . ?
C36 C35 C34 C33 36.8(6) . . . . ?
C41 C35 C34 C40 40.7(8) . . . . ?
C36 C35 C34 C40 -88.7(7) . . . . ?
C41 C35 C34 C39 -80.9(6) . . . . ?
C36 C35 C34 C39 149.7(5) . . . . ?
C11 O8 C27 O9 11.8(11) . . . . ?
C11 O8 C27 C31 -174.5(6) . . . . ?
O12 C51 C50 C49 178.3(5) . . . . ?
C44 C51 C50 C49 -2.3(5) . . . . ?
C53 C49 C50 C51 -151.5(4) . . . . ?
C48 C49 C50 C51 -23.6(5) . . . . ?
C64 C45 C43 C36 125.6(6) . . . . ?
C44 C45 C43 C36 -53.3(4) . . . . ?
C64 C45 C43 C46 -113.6(6) . . . . ?
C44 C45 C43 C46 67.4(5) . . . . ?
C61 C36 C43 C45 -80.9(5) . . . . ?
C35 C36 C43 C45 155.5(4) . . . . ?
C37 C36 C43 C45 33.0(4) . . . . ?
C61 C36 C43 C46 161.7(4) . . . . ?
C35 C36 C43 C46 38.1(6) . . . . ?
C37 C36 C43 C46 -84.4(5) . . . . ?
O14 C46 C43 C45 65.9(5) . . . . ?
C47 C46 C43 C45 -53.4(6) . . . . ?
O14 C46 C43 C36 178.9(5) . . . . ?
C47 C46 C43 C36 59.5(6) . . . . ?
C21 C20 C22 C23 1.1(7) . . . . ?
C17 C20 C22 C23 177.4(5) . . . . ?
C20 C22 C23 O5 -0.9(8) . . . . ?
C21 O5 C23 C22 0.4(9) . . . . ?
C22 C20 C21 O5 -0.9(8) . . . . ?
C17 C20 C21 O5 -177.0(5) . . . . ?
C23 O5 C21 C20 0.4(9) . . . . ?
C54 C53 C56 O13 -1.5(8) . . . . ?
C49 C53 C56 O13 -177.8(5) . . . . ?
C55 O13 C56 C53 1.3(9) . . . . ?
C36 C35 C41 C42 -140.3(8) . . . . ?
C34 C35 C41 C42 88.3(9) . . . . ?
C46 O14 C59 O19 18.5(19) . . . . ?
C46 O14 C59 C60 -178.5(9) . . . . ?
C35 C41 C42 O17 39.7(18) . . . . ?
C35 C41 C42 O18 -136.7(10) . . . . ?
O17 C42 O18 C63 13.4(19) . . . . ?
C41 C42 O18 C63 -169.8(12) . . . . ?

_refine_diff_density_max         0.654
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.049

_shelxl_version_number           2013-4



