# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_1.THF
_database_code_depnum_ccdc_archive 'CCDC 1432493'
_audit_update_record             
;
2015-10-21 deposited with the CCDC.
2018-12-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H48 O12, C4 H8 O '
_chemical_formula_sum            'C48 H56 O13'
_chemical_formula_weight         840.93

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   12.990(3)
_cell_length_b                   17.916(4)
_cell_length_c                   20.699(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.068(3)
_cell_angle_gamma                90.00
_cell_volume                     4629.1(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9947
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      23.83

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1792
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9760
_exptl_absorpt_correction_T_max  0.9896
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26370
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_sigmaI/netI    0.0633
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.99
_diffrn_reflns_theta_max         24.00
_reflns_number_total             7085
_reflns_number_gt                5382
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
The value of sine(theta_max)/wavelength is less than 0.575
            Calculated sin(theta_max)/wavelength =    0.5723
Resolution (too) Low [sin(theta)/Lambda < 0.6]..      24.00 Degree

 The data were cut around 0.86 angstroms as they were very weak at high
 resolution. The crystals used were very weakly diffracting. Several were
  tested and the best one used to acquire data (over 48 hours), however the 
  data set is still low resolution. 

 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7085
_refine_ls_number_parameters     691
_refine_ls_number_restraints     1224
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.0950
_refine_ls_wR_factor_ref         0.3381
_refine_ls_wR_factor_gt          0.3234
_refine_ls_goodness_of_fit_ref   1.374
_refine_ls_restrained_S_all      1.297
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0136(3) 0.9371(2) 0.83928(18) 0.0356(9) Uani 1 1 d U A 4
C2 C 0.0141(3) 0.8604(2) 0.83019(18) 0.0340(9) Uani 1 1 d U A 4
H2 H -0.0117 0.8295 0.8582 0.041 Uiso 1 1 calc R A 4
C3 C 0.0527(3) 0.8286(2) 0.77986(17) 0.0318(8) Uani 1 1 d U A 4
C4 C 0.0880(3) 0.8772(2) 0.73690(17) 0.0322(8) Uani 1 1 d U A 4
C5 C 0.0937(3) 0.9537(2) 0.74736(17) 0.0325(8) Uani 1 1 d U A 4
C6 C 0.0567(3) 0.9838(2) 0.79849(18) 0.0351(9) Uani 1 1 d U A 4
H6 H 0.0603 1.0350 0.8059 0.042 Uiso 1 1 calc R A 4
C7 C -0.0351(3) 0.9712(2) 0.88876(19) 0.0375(9) Uani 1 1 d U A 4
C8 C 0.0313(3) 0.8276(2) 0.62703(17) 0.0361(9) Uani 1 1 d U A 4
H8A H 0.0030 0.8723 0.6020 0.043 Uiso 1 1 calc R A 4
H8B H -0.0256 0.8047 0.6422 0.043 Uiso 1 1 calc R A 4
C9 C 0.0696(4) 0.7739(3) 0.5823(2) 0.0489(11) Uani 1 1 d U A 4
H9A H 0.1020 0.7307 0.6084 0.059 Uiso 1 1 calc R A 4
H9B H 0.1237 0.7980 0.5654 0.059 Uiso 1 1 calc R A 4
C10 C -0.0227(5) 0.7486(3) 0.5236(2) 0.0655(14) Uani 1 1 d U A 4
H10A H -0.0771 0.7259 0.5404 0.098 Uiso 1 1 calc R A 4
H10B H 0.0031 0.7130 0.4971 0.098 Uiso 1 1 calc R A 4
H10C H -0.0522 0.7909 0.4963 0.098 Uiso 1 1 calc R A 4
C11 C 0.0550(3) 0.7445(2) 0.77202(18) 0.0351(9) Uani 1 1 d U A 4
H11A H -0.0177 0.7256 0.7600 0.042 Uiso 1 1 calc R A 4
H11B H 0.0860 0.7325 0.7357 0.042 Uiso 1 1 calc R A 4
C12 C 0.1191(3) 0.7068(2) 0.83553(17) 0.0343(9) Uani 1 1 d U A 4
C13 C 0.0686(3) 0.6626(2) 0.87350(18) 0.0345(9) Uani 1 1 d U A 4
H13 H -0.0052 0.6556 0.8591 0.041 Uiso 1 1 calc R A 4
C14 C 0.1279(3) 0.6291(2) 0.93246(18) 0.0338(9) Uani 1 1 d U A 4
C15 C 0.2379(3) 0.6443(2) 0.95797(18) 0.0349(9) Uani 1 1 d U A 4
H15 H 0.2762 0.6239 0.9989 0.042 Uiso 1 1 calc R A 4
C16 C 0.2899(3) 0.6898(2) 0.92235(19) 0.0356(9) Uani 1 1 d U A 4
C17 C 0.2303(3) 0.7151(2) 0.85864(18) 0.0349(9) Uani 1 1 d U A 4
C18 C 0.0722(3) 0.5766(2) 0.96656(19) 0.0383(9) Uani 1 1 d U A 4
C19 C 0.3437(18) 0.7158(15) 0.7891(12) 0.079(5) Uani 0.571(14) 1 d PU A 1
H19A H 0.3956 0.6886 0.8238 0.095 Uiso 0.571(14) 1 calc PR A 1
H19B H 0.3834 0.7514 0.7700 0.095 Uiso 0.571(14) 1 calc PR A 1
C20 C 0.2902(8) 0.6595(8) 0.7330(5) 0.067(3) Uani 0.571(14) 1 d PU A 1
H20A H 0.2450 0.6264 0.7503 0.081 Uiso 0.571(14) 1 calc PR A 1
H20B H 0.2440 0.6871 0.6958 0.081 Uiso 0.571(14) 1 calc PR A 1
C21 C 0.3666(11) 0.6109(10) 0.7052(5) 0.096(5) Uani 0.571(14) 1 d PU A 1
H21A H 0.4352 0.6349 0.7141 0.145 Uiso 0.571(14) 1 calc PR A 1
H21B H 0.3372 0.6048 0.6575 0.145 Uiso 0.571(14) 1 calc PR A 1
H21C H 0.3748 0.5629 0.7266 0.145 Uiso 0.571(14) 1 calc PR A 1
C19' C 0.362(2) 0.7107(19) 0.7934(14) 0.062(5) Uani 0.429(14) 1 d PU A 2
H19C H 0.4323 0.7333 0.8064 0.075 Uiso 0.429(14) 1 calc PR A 2
H19D H 0.3664 0.6592 0.8083 0.075 Uiso 0.429(14) 1 calc PR A 2
C20' C 0.3081(12) 0.7177(13) 0.7170(7) 0.083(5) Uani 0.429(14) 1 d PU A 2
H20C H 0.2946 0.7693 0.7032 0.099 Uiso 0.429(14) 1 calc PR A 2
H20D H 0.2418 0.6896 0.7031 0.099 Uiso 0.429(14) 1 calc PR A 2
C21' C 0.3973(16) 0.6826(14) 0.6901(8) 0.105(6) Uani 0.429(14) 1 d PU A 2
H21D H 0.4283 0.6408 0.7178 0.158 Uiso 0.429(14) 1 calc PR A 2
H21E H 0.4518 0.7192 0.6912 0.158 Uiso 0.429(14) 1 calc PR A 2
H21F H 0.3671 0.6660 0.6447 0.158 Uiso 0.429(14) 1 calc PR A 2
C22 C 0.4005(3) 0.7199(2) 0.9538(2) 0.0412(9) Uani 1 1 d U . .
H22A H 0.4476 0.7064 0.9266 0.049 Uiso 1 1 calc R A 4
H22B H 0.4292 0.6986 0.9983 0.049 Uiso 1 1 calc R A 4
C23 C 0.3945(3) 0.8039(2) 0.95884(18) 0.0360(9) Uani 1 1 d U A .
C24 C 0.3198(3) 0.8350(2) 0.98760(17) 0.0337(9) Uani 1 1 d U . .
H24 H 0.2823 0.8040 1.0092 0.040 Uiso 1 1 calc R A .
C25 C 0.2997(3) 0.9115(2) 0.98494(17) 0.0341(9) Uani 1 1 d U A .
C26 C 0.3578(3) 0.9575(2) 0.95249(17) 0.0353(9) Uani 1 1 d U . .
H26 H 0.3440 1.0085 0.9496 0.042 Uiso 1 1 calc R A .
C27 C 0.4360(3) 0.9284(2) 0.92446(17) 0.0353(9) Uani 1 1 d U A .
C28 C 0.4537(3) 0.8523(2) 0.92868(17) 0.0356(9) Uani 1 1 d U . .
C29 C 0.635(2) 0.8333(14) 0.9391(13) 0.052(4) Uani 0.541(16) 1 d PU A 1
H29A H 0.6461 0.8142 0.9844 0.062 Uiso 0.541(16) 1 calc PR A 1
H29B H 0.6541 0.8858 0.9412 0.062 Uiso 0.541(16) 1 calc PR A 1
C30 C 0.703(2) 0.7845(12) 0.8967(13) 0.085(5) Uani 0.541(16) 1 d PU A 1
H30A H 0.6938 0.8111 0.8546 0.102 Uiso 0.541(16) 1 calc PR A 1
H30B H 0.7777 0.7904 0.9214 0.102 Uiso 0.541(16) 1 calc PR A 1
C31 C 0.6915(12) 0.7117(10) 0.8798(9) 0.123(6) Uani 0.541(16) 1 d PU A 1
H31A H 0.7501 0.6839 0.9079 0.185 Uiso 0.541(16) 1 calc PR A 1
H31B H 0.6909 0.7059 0.8336 0.185 Uiso 0.541(16) 1 calc PR A 1
H31C H 0.6252 0.6935 0.8858 0.185 Uiso 0.541(16) 1 calc PR A 1
C29' C 0.638(3) 0.8140(16) 0.9384(18) 0.053(5) Uani 0.459(16) 1 d PU A 2
H29C H 0.6562 0.8554 0.9697 0.064 Uiso 0.459(16) 1 calc PR A 2
H29D H 0.6464 0.7682 0.9643 0.064 Uiso 0.459(16) 1 calc PR A 2
C30' C 0.7088(19) 0.8131(9) 0.8976(11) 0.052(4) Uani 0.459(16) 1 d PU A 2
H30C H 0.7123 0.7612 0.8850 0.063 Uiso 0.459(16) 1 calc PR A 2
H30D H 0.7785 0.8246 0.9279 0.063 Uiso 0.459(16) 1 calc PR A 2
C31' C 0.7045(11) 0.8556(10) 0.8359(7) 0.091(5) Uani 0.459(16) 1 d PU A 2
H31D H 0.6326 0.8551 0.8069 0.137 Uiso 0.459(16) 1 calc PR A 2
H31E H 0.7517 0.8331 0.8131 0.137 Uiso 0.459(16) 1 calc PR A 2
H31F H 0.7263 0.9062 0.8474 0.137 Uiso 0.459(16) 1 calc PR A 2
C32 C 0.2198(3) 0.9427(2) 1.01468(18) 0.0357(9) Uani 1 1 d U . .
C33 C 0.4924(3) 0.9797(2) 0.8859(2) 0.0419(10) Uani 1 1 d U . .
H33A H 0.5471 1.0087 0.9173 0.050 Uiso 1 1 calc R A .
H33B H 0.5267 0.9502 0.8585 0.050 Uiso 1 1 calc R . .
C34 C 0.4093(3) 1.0319(2) 0.84128(18) 0.0388(9) Uani 1 1 d U A .
C35 C 0.4013(3) 1.1046(2) 0.8599(2) 0.0422(10) Uani 1 1 d U . .
H35 H 0.4543 1.1246 0.8955 0.051 Uiso 1 1 calc R A .
C36 C 0.3142(4) 1.1495(2) 0.8261(2) 0.0438(10) Uani 1 1 d U A .
C37 C 0.2344(3) 1.1172(2) 0.7740(2) 0.0418(10) Uani 1 1 d U . .
H37 H 0.1755 1.1458 0.7519 0.050 Uiso 1 1 calc R A .
C38 C 0.2403(3) 1.0448(2) 0.75464(18) 0.0345(9) Uani 1 1 d U A .
C39 C 0.3321(3) 1.0030(2) 0.78697(18) 0.0343(9) Uani 1 1 d U . .
C40 C 0.4207(11) 0.9075(12) 0.7396(7) 0.059(3) Uani 0.542(11) 1 d PDU A 1
H40A H 0.4342 0.8544 0.7461 0.070 Uiso 0.542(11) 1 calc PR A 1
H40B H 0.4864 0.9345 0.7601 0.070 Uiso 0.542(11) 1 calc PR A 1
C41 C 0.3757(9) 0.9278(7) 0.6586(5) 0.074(3) Uani 0.542(11) 1 d PU A 1
H41A H 0.4158 0.8963 0.6361 0.089 Uiso 0.542(11) 1 calc PR A 1
H41B H 0.3024 0.9099 0.6446 0.089 Uiso 0.542(11) 1 calc PR A 1
C42 C 0.3737(11) 1.0022(8) 0.6285(6) 0.093(4) Uani 0.542(11) 1 d PU A 1
H42A H 0.3213 1.0326 0.6407 0.140 Uiso 0.542(11) 1 calc PR A 1
H42B H 0.3556 0.9976 0.5804 0.140 Uiso 0.542(11) 1 calc PR A 1
H42C H 0.4431 1.0249 0.6445 0.140 Uiso 0.542(11) 1 calc PR A 1
C40' C 0.4070(19) 0.9238(15) 0.7252(11) 0.083(6) Uani 0.458(11) 1 d PDU A 2
H40C H 0.4798 0.9155 0.7525 0.100 Uiso 0.458(11) 1 calc PR A 2
H40D H 0.4055 0.9692 0.6995 0.100 Uiso 0.458(11) 1 calc PR A 2
C41' C 0.3694(13) 0.8574(10) 0.6774(7) 0.091(5) Uani 0.458(11) 1 d PU A 2
H41C H 0.3433 0.8189 0.7019 0.109 Uiso 0.458(11) 1 calc PR A 2
H41D H 0.3090 0.8739 0.6411 0.109 Uiso 0.458(11) 1 calc PR A 2
C42' C 0.4478(15) 0.8236(10) 0.6478(8) 0.104(6) Uani 0.458(11) 1 d PU A 2
H42D H 0.4959 0.8613 0.6406 0.156 Uiso 0.458(11) 1 calc PR A 2
H42E H 0.4115 0.8009 0.6057 0.156 Uiso 0.458(11) 1 calc PR A 2
H42F H 0.4877 0.7863 0.6778 0.156 Uiso 0.458(11) 1 calc PR A 2
C43 C 0.3082(4) 1.2274(3) 0.8490(3) 0.0596(12) Uani 1 1 d U . .
C44 C 0.1463(3) 1.0052(2) 0.70700(18) 0.0351(9) Uani 1 1 d U . .
H44A H 0.1709 0.9763 0.6745 0.042 Uiso 1 1 calc R A 4
H44B H 0.0947 1.0416 0.6827 0.042 Uiso 1 1 calc R A 4
O1 O -0.0450(3) 1.04158(17) 0.88884(17) 0.0574(9) Uani 1 1 d U . .
O2 O -0.0690(3) 0.92894(17) 0.92704(15) 0.0527(8) Uani 1 1 d U . .
H2A H -0.0905 0.9543 0.9536 0.079 Uiso 1 1 calc R A 4
O3 O -0.0253(2) 0.56637(16) 0.94597(14) 0.0455(7) Uani 1 1 d U . .
O4 O 0.1345(2) 0.54058(16) 1.01764(14) 0.0466(8) Uani 1 1 d U . .
H4 H 0.0983 0.5121 1.0334 0.070 Uiso 1 1 calc R A 4
O5 O 0.1706(3) 0.89952(17) 1.04442(15) 0.0486(8) Uani 1 1 d U A .
H5 H 0.1137 0.9187 1.0452 0.073 Uiso 1 1 calc R . .
O6 O 0.1998(3) 1.01257(17) 1.00849(16) 0.0529(8) Uani 1 1 d U A .
O7 O 0.3757(4) 1.2546(2) 0.8951(2) 0.0958(14) Uani 1 1 d U A .
O8 O 0.2243(3) 1.2639(2) 0.8144(2) 0.0726(11) Uani 1 1 d U A .
H8 H 0.2254 1.3063 0.8294 0.109 Uiso 1 1 calc R . .
O9 O 0.1191(2) 0.84673(15) 0.68393(11) 0.0351(7) Uani 1 1 d U . .
O10 O 0.2801(2) 0.75565(17) 0.81979(13) 0.0465(8) Uani 1 1 d U . .
O11 O 0.5265(2) 0.82118(17) 0.89859(13) 0.0441(7) Uani 1 1 d U A .
O13 O 0.7900(6) 0.8986(4) 0.6360(4) 0.099(2) Uani 0.675(8) 1 d PDU B 1
C45 C 0.7849(12) 0.9623(9) 0.6768(9) 0.112(4) Uani 0.675(8) 1 d PDU B 1
H45A H 0.8331 1.0015 0.6710 0.135 Uiso 0.675(8) 1 calc PR B 1
H45B H 0.8009 0.9492 0.7240 0.135 Uiso 0.675(8) 1 calc PR B 1
C46 C 0.6739(11) 0.9834(9) 0.6495(7) 0.136(4) Uani 0.675(8) 1 d PDU B 1
H46A H 0.6314 0.9629 0.6771 0.163 Uiso 0.675(8) 1 calc PR B 1
H46B H 0.6673 1.0373 0.6493 0.163 Uiso 0.675(8) 1 calc PR B 1
C47 C 0.6355(10) 0.9552(8) 0.5820(6) 0.121(4) Uani 0.675(8) 1 d PDU B 1
H47A H 0.6163 0.9963 0.5504 0.146 Uiso 0.675(8) 1 calc PR B 1
H47B H 0.5724 0.9246 0.5778 0.146 Uiso 0.675(8) 1 calc PR B 1
C48 C 0.7220(11) 0.9101(7) 0.5672(6) 0.116(4) Uani 0.675(8) 1 d PDU B 1
H48A H 0.6953 0.8633 0.5453 0.140 Uiso 0.675(8) 1 calc PR B 1
H48B H 0.7592 0.9374 0.5399 0.140 Uiso 0.675(8) 1 calc PR B 1
C48' C 0.787(2) 1.0330(15) 0.7097(15) 0.135(7) Uani 0.325(8) 1 d PDU B 2
H48C H 0.8548 1.0469 0.7410 0.162 Uiso 0.325(8) 1 calc PR B 2
H48D H 0.7562 1.0769 0.6842 0.162 Uiso 0.325(8) 1 calc PR B 2
C45' C 0.806(3) 0.963(2) 0.6563(19) 0.122(7) Uani 0.325(8) 1 d PDU B 2
H45C H 0.7750 0.9756 0.6093 0.147 Uiso 0.325(8) 1 calc PR B 2
H45D H 0.8811 0.9500 0.6642 0.147 Uiso 0.325(8) 1 calc PR B 2
C46' C 0.713(2) 1.0026(15) 0.7467(16) 0.143(8) Uani 0.325(8) 1 d PDU B 2
H46C H 0.7322 1.0205 0.7927 0.172 Uiso 0.325(8) 1 calc PR B 2
H46D H 0.6395 1.0172 0.7249 0.172 Uiso 0.325(8) 1 calc PR B 2
O13' O 0.746(2) 0.9076(13) 0.6803(12) 0.154(6) Uani 0.325(8) 1 d PDU B 2
C47' C 0.724(3) 0.9224(16) 0.7449(14) 0.142(8) Uani 0.325(8) 1 d PDU B 2
H47C H 0.6593 0.8975 0.7474 0.171 Uiso 0.325(8) 1 calc PR B 2
H47D H 0.7834 0.9054 0.7819 0.171 Uiso 0.325(8) 1 calc PR B 2
O12 O 0.3364(2) 0.93075(16) 0.76749(13) 0.0445(7) Uani 1 1 d DU A .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.388(6) . ?
C1 C6 1.410(5) . ?
C1 C7 1.476(5) . ?
C2 C3 1.397(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.409(5) . ?
C3 C11 1.516(5) . ?
C4 O9 1.382(4) . ?
C4 C5 1.386(5) . ?
C5 C6 1.387(5) . ?
C5 C44 1.527(5) . ?
C6 H6 0.9300 . ?
C7 O2 1.261(5) . ?
C7 O1 1.267(5) . ?
C8 O9 1.436(5) . ?
C8 C9 1.511(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.520(7) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.507(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C17 1.399(6) . ?
C12 C13 1.400(5) . ?
C13 C14 1.386(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.406(6) . ?
C14 C18 1.481(5) . ?
C15 C16 1.392(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.406(5) . ?
C16 C22 1.504(6) . ?
C17 O10 1.371(4) . ?
C18 O3 1.233(5) . ?
C18 O4 1.310(5) . ?
C19 O10 1.37(2) . ?
C19 C20 1.55(3) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.545(13) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C19' C20' 1.55(3) . ?
C19' O10 1.55(3) . ?
C19' H19C 0.9700 . ?
C19' H19D 0.9700 . ?
C20' C21' 1.55(2) . ?
C20' H20C 0.9700 . ?
C20' H20D 0.9700 . ?
C21' H21D 0.9600 . ?
C21' H21E 0.9600 . ?
C21' H21F 0.9600 . ?
C22 C23 1.512(6) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.388(5) . ?
C23 C28 1.414(6) . ?
C24 C25 1.393(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.407(5) . ?
C25 C32 1.458(5) . ?
C26 C27 1.403(6) . ?
C26 H26 0.9300 . ?
C27 C28 1.380(6) . ?
C27 C33 1.531(5) . ?
C28 O11 1.386(5) . ?
C29 O11 1.44(3) . ?
C29 C30 1.66(4) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C31 1.35(2) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C29' C30' 1.41(4) . ?
C29' O11 1.46(4) . ?
C29' H29C 0.9700 . ?
C29' H29D 0.9700 . ?
C30' C31' 1.47(3) . ?
C30' H30C 0.9700 . ?
C30' H30D 0.9700 . ?
C31' H31D 0.9600 . ?
C31' H31E 0.9600 . ?
C31' H31F 0.9600 . ?
C32 O5 1.266(5) . ?
C32 O6 1.278(5) . ?
C33 C34 1.531(6) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.370(6) . ?
C34 C39 1.383(6) . ?
C35 C36 1.406(6) . ?
C35 H35 0.9300 . ?
C36 C37 1.398(6) . ?
C36 C43 1.483(7) . ?
C37 C38 1.366(6) . ?
C37 H37 0.9300 . ?
C38 C39 1.409(6) . ?
C38 C44 1.516(6) . ?
C39 O12 1.362(5) . ?
C40 O12 1.434(13) . ?
C40 C41 1.655(18) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 C42 1.469(18) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C40' O12 1.437(15) . ?
C40' C41' 1.54(3) . ?
C40' H40C 0.9700 . ?
C40' H40D 0.9700 . ?
C41' C42' 1.46(2) . ?
C41' H41C 0.9700 . ?
C41' H41D 0.9700 . ?
C42' H42D 0.9600 . ?
C42' H42E 0.9600 . ?
C42' H42F 0.9600 . ?
C43 O7 1.206(7) . ?
C43 O8 1.303(7) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
O2 H2A 0.8200 . ?
O4 H4 0.8200 . ?
O5 H5 0.8200 . ?
O8 H8 0.8200 . ?
O13 C45 1.430(13) . ?
O13 C48 1.468(12) . ?
C45 C46 1.446(15) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 C47 1.438(13) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C47 C48 1.483(13) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C48' C46' 1.491(18) . ?
C48' C45' 1.73(5) . ?
C48' H48C 0.9700 . ?
C48' H48D 0.9700 . ?
C45' O13' 1.440(18) . ?
C45' H45C 0.9700 . ?
C45' H45D 0.9700 . ?
C46' C47' 1.446(18) . ?
C46' H46C 0.9700 . ?
C46' H46D 0.9700 . ?
O13' C47' 1.464(18) . ?
C47' H47C 0.9700 . ?
C47' H47D 0.9700 . ?

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
C2 C1 C6 119.2(3) . . ?
C2 C1 C7 121.6(3) . . ?
C6 C1 C7 119.2(3) . . ?
C1 C2 C3 121.4(3) . . ?
C1 C2 H2 119.3 . . ?
C3 C2 H2 119.3 . . ?
C2 C3 C4 117.7(3) . . ?
C2 C3 C11 120.5(3) . . ?
C4 C3 C11 121.9(3) . . ?
O9 C4 C5 120.0(3) . . ?
O9 C4 C3 118.2(3) . . ?
C5 C4 C3 121.7(3) . . ?
C4 C5 C6 119.2(3) . . ?
C4 C5 C44 121.6(3) . . ?
C6 C5 C44 119.0(3) . . ?
C5 C6 C1 120.4(4) . . ?
C5 C6 H6 119.8 . . ?
C1 C6 H6 119.8 . . ?
O2 C7 O1 122.9(3) . . ?
O2 C7 C1 118.6(3) . . ?
O1 C7 C1 118.4(3) . . ?
O9 C8 C9 109.5(3) . . ?
O9 C8 H8A 109.8 . . ?
C9 C8 H8A 109.8 . . ?
O9 C8 H8B 109.8 . . ?
C9 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?
C8 C9 C10 111.0(4) . . ?
C8 C9 H9A 109.4 . . ?
C10 C9 H9A 109.4 . . ?
C8 C9 H9B 109.4 . . ?
C10 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
C12 C11 C3 112.0(3) . . ?
C12 C11 H11A 109.2 . . ?
C3 C11 H11A 109.2 . . ?
C12 C11 H11B 109.2 . . ?
C3 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
C17 C12 C13 117.9(3) . . ?
C17 C12 C11 121.2(3) . . ?
C13 C12 C11 120.8(3) . . ?
C14 C13 C12 120.4(4) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C13 C14 C15 120.4(3) . . ?
C13 C14 C18 117.9(4) . . ?
C15 C14 C18 121.6(3) . . ?
C16 C15 C14 120.4(3) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C15 C16 C17 117.6(4) . . ?
C15 C16 C22 121.7(3) . . ?
C17 C16 C22 120.2(3) . . ?
O10 C17 C12 117.8(3) . . ?
O10 C17 C16 119.6(3) . . ?
C12 C17 C16 122.3(3) . . ?
O3 C18 O4 123.6(3) . . ?
O3 C18 C14 121.4(3) . . ?
O4 C18 C14 115.0(4) . . ?
O10 C19 C20 118.9(16) . . ?
O10 C19 H19A 107.6 . . ?
C20 C19 H19A 107.6 . . ?
O10 C19 H19B 107.6 . . ?
C20 C19 H19B 107.6 . . ?
H19A C19 H19B 107.0 . . ?
C21 C20 C19 116.4(11) . . ?
C21 C20 H20A 108.2 . . ?
C19 C20 H20A 108.2 . . ?
C21 C20 H20B 108.2 . . ?
C19 C20 H20B 108.2 . . ?
H20A C20 H20B 107.3 . . ?
C20' C19' O10 99.2(15) . . ?
C20' C19' H19C 111.9 . . ?
O10 C19' H19C 111.9 . . ?
C20' C19' H19D 111.9 . . ?
O10 C19' H19D 111.9 . . ?
H19C C19' H19D 109.6 . . ?
C19' C20' C21' 99.5(16) . . ?
C19' C20' H20C 111.9 . . ?
C21' C20' H20C 111.9 . . ?
C19' C20' H20D 111.9 . . ?
C21' C20' H20D 111.9 . . ?
H20C C20' H20D 109.6 . . ?
C20' C21' H21D 109.5 . . ?
C20' C21' H21E 109.5 . . ?
H21D C21' H21E 109.5 . . ?
C20' C21' H21F 109.5 . . ?
H21D C21' H21F 109.5 . . ?
H21E C21' H21F 109.5 . . ?
C16 C22 C23 109.0(3) . . ?
C16 C22 H22A 109.9 . . ?
C23 C22 H22A 109.9 . . ?
C16 C22 H22B 109.9 . . ?
C23 C22 H22B 109.9 . . ?
H22A C22 H22B 108.3 . . ?
C24 C23 C28 118.2(4) . . ?
C24 C23 C22 119.0(3) . . ?
C28 C23 C22 122.4(3) . . ?
C23 C24 C25 121.6(3) . . ?
C23 C24 H24 119.2 . . ?
C25 C24 H24 119.2 . . ?
C24 C25 C26 118.5(3) . . ?
C24 C25 C32 120.5(3) . . ?
C26 C25 C32 121.0(4) . . ?
C27 C26 C25 121.6(4) . . ?
C27 C26 H26 119.2 . . ?
C25 C26 H26 119.2 . . ?
C28 C27 C26 117.9(3) . . ?
C28 C27 C33 122.1(3) . . ?
C26 C27 C33 119.8(4) . . ?
C27 C28 O11 119.4(3) . . ?
C27 C28 C23 122.2(3) . . ?
O11 C28 C23 118.3(4) . . ?
O11 C29 C30 101.0(17) . . ?
O11 C29 H29A 111.6 . . ?
C30 C29 H29A 111.6 . . ?
O11 C29 H29B 111.6 . . ?
C30 C29 H29B 111.6 . . ?
H29A C29 H29B 109.4 . . ?
C31 C30 C29 128(2) . . ?
C31 C30 H30A 105.4 . . ?
C29 C30 H30A 105.4 . . ?
C31 C30 H30B 105.4 . . ?
C29 C30 H30B 105.4 . . ?
H30A C30 H30B 106.0 . . ?
C30' C29' O11 112(3) . . ?
C30' C29' H29C 109.2 . . ?
O11 C29' H29C 109.2 . . ?
C30' C29' H29D 109.2 . . ?
O11 C29' H29D 109.2 . . ?
H29C C29' H29D 107.9 . . ?
C29' C30' C31' 130(2) . . ?
C29' C30' H30C 104.9 . . ?
C31' C30' H30C 104.9 . . ?
C29' C30' H30D 104.9 . . ?
C31' C30' H30D 104.9 . . ?
H30C C30' H30D 105.8 . . ?
C30' C31' H31D 109.5 . . ?
C30' C31' H31E 109.5 . . ?
H31D C31' H31E 109.5 . . ?
C30' C31' H31F 109.5 . . ?
H31D C31' H31F 109.5 . . ?
H31E C31' H31F 109.5 . . ?
O5 C32 O6 122.1(3) . . ?
O5 C32 C25 119.0(4) . . ?
O6 C32 C25 118.8(3) . . ?
C34 C33 C27 108.8(3) . . ?
C34 C33 H33A 109.9 . . ?
C27 C33 H33A 109.9 . . ?
C34 C33 H33B 109.9 . . ?
C27 C33 H33B 109.9 . . ?
H33A C33 H33B 108.3 . . ?
C35 C34 C39 119.3(4) . . ?
C35 C34 C33 120.5(4) . . ?
C39 C34 C33 119.6(4) . . ?
C34 C35 C36 121.2(4) . . ?
C34 C35 H35 119.4 . . ?
C36 C35 H35 119.4 . . ?
C37 C36 C35 118.0(4) . . ?
C37 C36 C43 122.9(4) . . ?
C35 C36 C43 119.1(4) . . ?
C38 C37 C36 122.0(4) . . ?
C38 C37 H37 119.0 . . ?
C36 C37 H37 119.0 . . ?
C37 C38 C39 118.2(4) . . ?
C37 C38 C44 122.3(4) . . ?
C39 C38 C44 118.9(3) . . ?
O12 C39 C34 121.1(4) . . ?
O12 C39 C38 117.6(3) . . ?
C34 C39 C38 121.0(4) . . ?
O12 C40 C41 104.4(10) . . ?
O12 C40 H40A 110.9 . . ?
C41 C40 H40A 110.9 . . ?
O12 C40 H40B 110.9 . . ?
C41 C40 H40B 110.9 . . ?
H40A C40 H40B 108.9 . . ?
C42 C41 C40 126.1(12) . . ?
C42 C41 H41A 105.8 . . ?
C40 C41 H41A 105.8 . . ?
C42 C41 H41B 105.8 . . ?
C40 C41 H41B 105.8 . . ?
H41A C41 H41B 106.2 . . ?
O12 C40' C41' 108.4(18) . . ?
O12 C40' H40C 110.0 . . ?
C41' C40' H40C 110.0 . . ?
O12 C40' H40D 110.0 . . ?
C41' C40' H40D 110.0 . . ?
H40C C40' H40D 108.4 . . ?
C42' C41' C40' 117.2(15) . . ?
C42' C41' H41C 108.0 . . ?
C40' C41' H41C 108.0 . . ?
C42' C41' H41D 108.0 . . ?
C40' C41' H41D 108.0 . . ?
H41C C41' H41D 107.2 . . ?
C41' C42' H42D 109.5 . . ?
C41' C42' H42E 109.5 . . ?
H42D C42' H42E 109.5 . . ?
C41' C42' H42F 109.5 . . ?
H42D C42' H42F 109.5 . . ?
H42E C42' H42F 109.5 . . ?
O7 C43 O8 123.1(5) . . ?
O7 C43 C36 122.9(5) . . ?
O8 C43 C36 114.0(4) . . ?
C38 C44 C5 109.2(3) . . ?
C38 C44 H44A 109.8 . . ?
C5 C44 H44A 109.8 . . ?
C38 C44 H44B 109.8 . . ?
C5 C44 H44B 109.8 . . ?
H44A C44 H44B 108.3 . . ?
C32 O5 H5 109.5 . . ?
C43 O8 H8 109.5 . . ?
C4 O9 C8 113.9(3) . . ?
C17 O10 C19 116.0(12) . . ?
C17 O10 C19' 114.3(13) . . ?
C19 O10 C19' 6.8(19) . . ?
C28 O11 C29 110.9(10) . . ?
C28 O11 C29' 118.4(11) . . ?
C29 O11 C29' 13.8(18) . . ?
C45 O13 C48 110.3(10) . . ?
O13 C45 C46 100.4(11) . . ?
O13 C45 H45A 111.7 . . ?
C46 C45 H45A 111.7 . . ?
O13 C45 H45B 111.7 . . ?
C46 C45 H45B 111.7 . . ?
H45A C45 H45B 109.5 . . ?
C47 C46 C45 109.2(12) . . ?
C47 C46 H46A 109.8 . . ?
C45 C46 H46A 109.8 . . ?
C47 C46 H46B 109.8 . . ?
C45 C46 H46B 109.8 . . ?
H46A C46 H46B 108.3 . . ?
C46 C47 C48 108.2(11) . . ?
C46 C47 H47A 110.1 . . ?
C48 C47 H47A 110.1 . . ?
C46 C47 H47B 110.1 . . ?
C48 C47 H47B 110.1 . . ?
H47A C47 H47B 108.4 . . ?
O13 C48 C47 99.3(9) . . ?
O13 C48 H48A 111.9 . . ?
C47 C48 H48A 111.9 . . ?
O13 C48 H48B 111.9 . . ?
C47 C48 H48B 111.9 . . ?
H48A C48 H48B 109.6 . . ?
C46' C48' C45' 107(2) . . ?
C46' C48' H48C 110.3 . . ?
C45' C48' H48C 110.3 . . ?
C46' C48' H48D 110.3 . . ?
C45' C48' H48D 110.3 . . ?
H48C C48' H48D 108.6 . . ?
O13' C45' C48' 95(2) . . ?
O13' C45' H45C 112.7 . . ?
C48' C45' H45C 112.7 . . ?
O13' C45' H45D 112.7 . . ?
C48' C45' H45D 112.7 . . ?
H45C C45' H45D 110.2 . . ?
C47' C46' C48' 105(3) . . ?
C47' C46' H46C 110.7 . . ?
C48' C46' H46C 110.7 . . ?
C47' C46' H46D 110.7 . . ?
C48' C46' H46D 110.7 . . ?
H46C C46' H46D 108.8 . . ?
C45' O13' C47' 117(3) . . ?
C46' C47' O13' 105(2) . . ?
C46' C47' H47C 110.8 . . ?
O13' C47' H47C 110.8 . . ?
C46' C47' H47D 110.8 . . ?
O13' C47' H47D 110.9 . . ?
H47C C47' H47D 108.9 . . ?
C39 O12 C40 119.6(9) . . ?
C39 O12 C40' 110.4(12) . . ?
C40 O12 C40' 16.8(14) . . ?

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
C6 C1 C2 C3 -2.5(6) . . . . ?
C7 C1 C2 C3 175.0(4) . . . . ?
C1 C2 C3 C4 -2.1(5) . . . . ?
C1 C2 C3 C11 178.5(3) . . . . ?
C2 C3 C4 O9 -175.4(3) . . . . ?
C11 C3 C4 O9 4.0(5) . . . . ?
C2 C3 C4 C5 5.8(5) . . . . ?
C11 C3 C4 C5 -174.8(3) . . . . ?
O9 C4 C5 C6 176.5(3) . . . . ?
C3 C4 C5 C6 -4.7(5) . . . . ?
O9 C4 C5 C44 -7.5(5) . . . . ?
C3 C4 C5 C44 171.3(3) . . . . ?
C4 C5 C6 C1 -0.1(5) . . . . ?
C44 C5 C6 C1 -176.2(3) . . . . ?
C2 C1 C6 C5 3.6(6) . . . . ?
C7 C1 C6 C5 -173.9(3) . . . . ?
C2 C1 C7 O2 5.7(6) . . . . ?
C6 C1 C7 O2 -176.8(4) . . . . ?
C2 C1 C7 O1 -171.3(4) . . . . ?
C6 C1 C7 O1 6.2(6) . . . . ?
O9 C8 C9 C10 176.6(4) . . . . ?
C2 C3 C11 C12 -57.3(5) . . . . ?
C4 C3 C11 C12 123.4(4) . . . . ?
C3 C11 C12 C17 -68.7(4) . . . . ?
C3 C11 C12 C13 110.9(4) . . . . ?
C17 C12 C13 C14 0.7(5) . . . . ?
C11 C12 C13 C14 -178.9(3) . . . . ?
C12 C13 C14 C15 5.6(5) . . . . ?
C12 C13 C14 C18 -173.5(3) . . . . ?
C13 C14 C15 C16 -3.7(5) . . . . ?
C18 C14 C15 C16 175.4(3) . . . . ?
C14 C15 C16 C17 -4.3(5) . . . . ?
C14 C15 C16 C22 167.4(3) . . . . ?
C13 C12 C17 O10 177.1(3) . . . . ?
C11 C12 C17 O10 -3.3(5) . . . . ?
C13 C12 C17 C16 -9.2(5) . . . . ?
C11 C12 C17 C16 170.4(3) . . . . ?
C15 C16 C17 O10 -175.5(3) . . . . ?
C22 C16 C17 O10 12.6(5) . . . . ?
C15 C16 C17 C12 10.9(6) . . . . ?
C22 C16 C17 C12 -160.9(4) . . . . ?
C13 C14 C18 O3 -4.7(5) . . . . ?
C15 C14 C18 O3 176.2(4) . . . . ?
C13 C14 C18 O4 172.8(3) . . . . ?
C15 C14 C18 O4 -6.3(5) . . . . ?
O10 C19 C20 C21 -174.3(15) . . . . ?
O10 C19' C20' C21' 172.4(18) . . . . ?
C15 C16 C22 C23 -114.5(4) . . . . ?
C17 C16 C22 C23 57.0(4) . . . . ?
C16 C22 C23 C24 50.6(4) . . . . ?
C16 C22 C23 C28 -122.2(4) . . . . ?
C28 C23 C24 C25 2.5(5) . . . . ?
C22 C23 C24 C25 -170.6(3) . . . . ?
C23 C24 C25 C26 -0.4(5) . . . . ?
C23 C24 C25 C32 179.1(3) . . . . ?
C24 C25 C26 C27 -1.4(5) . . . . ?
C32 C25 C26 C27 179.1(3) . . . . ?
C25 C26 C27 C28 0.9(5) . . . . ?
C25 C26 C27 C33 176.3(3) . . . . ?
C26 C27 C28 O11 176.8(3) . . . . ?
C33 C27 C28 O11 1.5(5) . . . . ?
C26 C27 C28 C23 1.2(5) . . . . ?
C33 C27 C28 C23 -174.0(3) . . . . ?
C24 C23 C28 C27 -2.9(5) . . . . ?
C22 C23 C28 C27 169.9(3) . . . . ?
C24 C23 C28 O11 -178.6(3) . . . . ?
C22 C23 C28 O11 -5.7(5) . . . . ?
O11 C29 C30 C31 -56(3) . . . . ?
O11 C29' C30' C31' 38(3) . . . . ?
C24 C25 C32 O5 1.7(5) . . . . ?
C26 C25 C32 O5 -178.8(3) . . . . ?
C24 C25 C32 O6 -176.7(3) . . . . ?
C26 C25 C32 O6 2.8(5) . . . . ?
C28 C27 C33 C34 133.0(4) . . . . ?
C26 C27 C33 C34 -42.1(5) . . . . ?
C27 C33 C34 C35 102.5(4) . . . . ?
C27 C33 C34 C39 -68.3(4) . . . . ?
C39 C34 C35 C36 2.0(6) . . . . ?
C33 C34 C35 C36 -168.7(4) . . . . ?
C34 C35 C36 C37 1.7(6) . . . . ?
C34 C35 C36 C43 178.8(4) . . . . ?
C35 C36 C37 C38 -1.5(6) . . . . ?
C43 C36 C37 C38 -178.5(4) . . . . ?
C36 C37 C38 C39 -2.3(6) . . . . ?
C36 C37 C38 C44 169.1(3) . . . . ?
C35 C34 C39 O12 -179.1(3) . . . . ?
C33 C34 C39 O12 -8.2(5) . . . . ?
C35 C34 C39 C38 -6.1(5) . . . . ?
C33 C34 C39 C38 164.8(3) . . . . ?
C37 C38 C39 O12 179.4(3) . . . . ?
C44 C38 C39 O12 7.7(5) . . . . ?
C37 C38 C39 C34 6.2(5) . . . . ?
C44 C38 C39 C34 -165.6(3) . . . . ?
O12 C40 C41 C42 77.9(15) . . . . ?
O12 C40' C41' C42' -158.5(14) . . . . ?
C37 C36 C43 O7 178.0(5) . . . . ?
C35 C36 C43 O7 1.0(7) . . . . ?
C37 C36 C43 O8 -2.8(6) . . . . ?
C35 C36 C43 O8 -179.8(4) . . . . ?
C37 C38 C44 C5 -102.1(4) . . . . ?
C39 C38 C44 C5 69.3(4) . . . . ?
C4 C5 C44 C38 -119.0(4) . . . . ?
C6 C5 C44 C38 57.0(4) . . . . ?
C5 C4 O9 C8 -101.5(4) . . . . ?
C3 C4 O9 C8 79.6(4) . . . . ?
C9 C8 O9 C4 -162.2(3) . . . . ?
C12 C17 O10 C19 -110.6(12) . . . . ?
C16 C17 O10 C19 75.6(12) . . . . ?
C12 C17 O10 C19' -117.8(12) . . . . ?
C16 C17 O10 C19' 68.3(12) . . . . ?
C20 C19 O10 C17 67(2) . . . . ?
C20 C19 O10 C19' 145(22) . . . . ?
C20' C19' O10 C17 118.2(16) . . . . ?
C20' C19' O10 C19 12(19) . . . . ?
C27 C28 O11 C29 78.1(12) . . . . ?
C23 C28 O11 C29 -106.2(12) . . . . ?
C27 C28 O11 C29' 90.8(16) . . . . ?
C23 C28 O11 C29' -93.5(15) . . . . ?
C30 C29 O11 C28 174.6(13) . . . . ?
C30 C29 O11 C29' 49(9) . . . . ?
C30' C29' O11 C28 -154.4(14) . . . . ?
C30' C29' O11 C29 -95(11) . . . . ?
C48 O13 C45 C46 36.1(15) . . . . ?
O13 C45 C46 C47 -23.6(18) . . . . ?
C45 C46 C47 C48 4.1(18) . . . . ?
C45 O13 C48 C47 -33.4(13) . . . . ?
C46 C47 C48 O13 16.7(14) . . . . ?
C46' C48' C45' O13' -5(3) . . . . ?
C45' C48' C46' C47' 24(3) . . . . ?
C48' C45' O13' C47' -17(4) . . . . ?
C48' C46' C47' O13' -33(3) . . . . ?
C45' O13' C47' C46' 33(4) . . . . ?
C34 C39 O12 C40 -67.8(8) . . . . ?
C38 C39 O12 C40 119.0(8) . . . . ?
C34 C39 O12 C40' -83.3(11) . . . . ?
C38 C39 O12 C40' 103.5(11) . . . . ?
C41 C40 O12 C39 -85.7(11) . . . . ?
C41 C40 O12 C40' -25(5) . . . . ?
C41' C40' O12 C39 -151.8(12) . . . . ?
C41' C40' O12 C40 82(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        24.00
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.086
####################################################################### 
# 
# 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_4.MeOH
_database_code_depnum_ccdc_archive 'CCDC 1432497'
_audit_update_record             
;
2015-10-21 deposited with the CCDC.
2018-12-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H36 O11'
_chemical_formula_weight         752.74

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1   '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.236(2)
_cell_length_b                   13.402(3)
_cell_length_c                   15.695(4)
_cell_angle_alpha                64.813(6)
_cell_angle_beta                 74.226(6)
_cell_angle_gamma                83.780(6)
_cell_volume                     1874.9(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2908
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      24.25
_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             788
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9737
_exptl_absorpt_correction_T_max  0.9830
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13045
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0974
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.22
_diffrn_reflns_theta_max         25.68
_reflns_number_total             7019
_reflns_number_gt                3432
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0881P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7019
_refine_ls_number_parameters     508
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1611
_refine_ls_R_factor_gt           0.0702
_refine_ls_wR_factor_ref         0.1963
_refine_ls_wR_factor_gt          0.1562
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3376(4) 0.3208(3) -0.1603(2) 0.0475(9) Uani 1 1 d . . .
C2 C 0.2380(4) 0.2399(3) -0.1167(2) 0.0482(9) Uani 1 1 d . . .
H2 H 0.1603 0.2509 -0.1417 0.058 Uiso 1 1 calc R . .
C3 C 0.2493(3) 0.1436(3) -0.0379(2) 0.0423(8) Uani 1 1 d . . .
C4 C 0.3643(4) 0.1288(3) -0.0029(2) 0.0443(9) Uani 1 1 d . . .
C5 C 0.4687(3) 0.2083(3) -0.0464(2) 0.0435(8) Uani 1 1 d . . .
C6 C 0.4526(4) 0.3038(3) -0.1246(2) 0.0481(9) Uani 1 1 d . . .
H6 H 0.5213 0.3592 -0.1548 0.058 Uiso 1 1 calc R . .
C7 C 0.3220(4) 0.4255(3) -0.2419(3) 0.0558(10) Uani 1 1 d . . .
C8 C 0.5914(4) 0.1939(3) -0.0056(3) 0.0514(9) Uani 1 1 d . . .
H8A H 0.6208 0.1161 0.0154 0.062 Uiso 1 1 calc R . .
H8B H 0.6671 0.2405 -0.0572 0.062 Uiso 1 1 calc R . .
C9 C 0.5605(3) 0.2247(3) 0.0790(2) 0.0460(9) Uani 1 1 d . . .
C10 C 0.5623(4) 0.3344(3) 0.0633(3) 0.0529(10) Uani 1 1 d . . .
H10 H 0.5849 0.3895 -0.0015 0.064 Uiso 1 1 calc R . .
C11 C 0.5318(4) 0.3652(3) 0.1399(3) 0.0598(11) Uani 1 1 d . . .
H11 H 0.5361 0.4407 0.1279 0.072 Uiso 1 1 calc R . .
C12 C 0.4952(4) 0.2857(3) 0.2342(3) 0.0565(10) Uani 1 1 d . . .
H12 H 0.4726 0.3074 0.2867 0.068 Uiso 1 1 calc R . .
C13 C 0.4907(4) 0.1755(3) 0.2535(2) 0.0469(9) Uani 1 1 d . . .
C14 C 0.5266(3) 0.1460(3) 0.1752(3) 0.0465(9) Uani 1 1 d . . .
C15 C 0.4523(4) 0.0903(3) 0.3579(2) 0.0579(10) Uani 1 1 d . . .
H15A H 0.5350 0.0476 0.3718 0.070 Uiso 1 1 calc R . .
H15B H 0.4280 0.1308 0.4001 0.070 Uiso 1 1 calc R . .
C16 C 0.3393(4) 0.0080(3) 0.3906(2) 0.0507(9) Uani 1 1 d . . .
C17 C 0.2157(4) 0.0315(3) 0.3629(2) 0.0464(9) Uani 1 1 d . . .
C18 C 0.3527(4) -0.0983(3) 0.4583(2) 0.0526(10) Uani 1 1 d . . .
H18 H 0.4340 -0.1181 0.4795 0.063 Uiso 1 1 calc R . .
C19 C 0.2494(4) -0.1768(3) 0.4958(2) 0.0489(9) Uani 1 1 d . . .
C20 C 0.1309(4) -0.1496(3) 0.4653(2) 0.0481(9) Uani 1 1 d . . .
H20 H 0.0621 -0.2042 0.4900 0.058 Uiso 1 1 calc R . .
C21 C 0.1104(3) -0.0450(3) 0.3996(2) 0.0439(8) Uani 1 1 d . . .
C22 C 0.2705(5) -0.2896(3) 0.5649(3) 0.0582(10) Uani 1 1 d . . .
C23 C 0.1766(4) 0.2248(3) 0.3070(3) 0.0526(9) Uani 1 1 d . . .
C24 C 0.1598(4) 0.3224(3) 0.2194(3) 0.0544(10) Uani 1 1 d . . .
C25 C 0.1855(4) 0.3199(3) 0.1304(3) 0.0619(11) Uani 1 1 d . . .
H25 H 0.2146 0.2533 0.1235 0.074 Uiso 1 1 calc R . .
C26 C 0.1693(5) 0.4134(4) 0.0504(3) 0.0818(14) Uani 1 1 d . . .
H26 H 0.1876 0.4111 -0.0114 0.098 Uiso 1 1 calc R . .
C27 C 0.1276(5) 0.5083(4) 0.0598(4) 0.0933(16) Uani 1 1 d . . .
H27 H 0.1152 0.5720 0.0046 0.112 Uiso 1 1 calc R . .
C28 C 0.1032(6) 0.5134(4) 0.1471(4) 0.1116(19) Uani 1 1 d . . .
H28 H 0.0736 0.5801 0.1534 0.134 Uiso 1 1 calc R . .
C29 C 0.1219(5) 0.4194(4) 0.2277(4) 0.0985(17) Uani 1 1 d . . .
H29 H 0.1080 0.4229 0.2887 0.118 Uiso 1 1 calc R . .
C30 C -0.0257(4) -0.0168(3) 0.3754(2) 0.0518(9) Uani 1 1 d . . .
H30A H -0.0773 0.0241 0.4134 0.062 Uiso 1 1 calc R . .
H30B H -0.0751 -0.0870 0.3996 0.062 Uiso 1 1 calc R . .
C31 C -0.0318(3) 0.0496(3) 0.2702(2) 0.0447(8) Uani 1 1 d . . .
C32 C -0.1184(4) 0.1385(3) 0.2469(3) 0.0539(10) Uani 1 1 d . . .
H32 H -0.1712 0.1596 0.2965 0.065 Uiso 1 1 calc R . .
C33 C -0.1289(4) 0.1966(3) 0.1529(3) 0.0566(10) Uani 1 1 d . . .
H33 H -0.1912 0.2557 0.1383 0.068 Uiso 1 1 calc R . .
C34 C -0.0501(4) 0.1696(3) 0.0804(3) 0.0556(10) Uani 1 1 d . . .
H34 H -0.0575 0.2118 0.0156 0.067 Uiso 1 1 calc R . .
C35 C 0.0413(3) 0.0818(3) 0.0985(2) 0.0450(9) Uani 1 1 d . . .
C36 C 0.0428(3) 0.0219(2) 0.1951(2) 0.0414(8) Uani 1 1 d . . .
C37 C 0.0707(5) -0.1681(3) 0.2434(3) 0.0657(11) Uani 1 1 d . . .
C38 C 0.1522(5) -0.2639(3) 0.2925(3) 0.0724(13) Uani 1 1 d . . .
C39 C 0.0944(7) -0.3671(4) 0.3361(4) 0.123(2) Uani 1 1 d . . .
H39 H 0.0071 -0.3763 0.3301 0.148 Uiso 1 1 calc R . .
C40 C 0.1614(11) -0.4570(5) 0.3882(5) 0.164(4) Uani 1 1 d . . .
H40 H 0.1207 -0.5280 0.4167 0.197 Uiso 1 1 calc R . .
C41 C 0.2812(11) -0.4462(7) 0.3993(5) 0.153(4) Uani 1 1 d . . .
H41 H 0.3244 -0.5087 0.4384 0.184 Uiso 1 1 calc R . .
C42 C 0.3447(7) -0.3431(6) 0.3537(4) 0.121(2) Uani 1 1 d . . .
H42 H 0.4331 -0.3355 0.3589 0.145 Uiso 1 1 calc R . .
C43 C 0.2777(6) -0.2519(4) 0.3006(3) 0.0888(15) Uani 1 1 d . . .
H43 H 0.3194 -0.1810 0.2700 0.107 Uiso 1 1 calc R . .
C44 C 0.1348(4) 0.0601(3) 0.0156(2) 0.0501(9) Uani 1 1 d . . .
H44A H 0.0826 0.0634 -0.0301 0.060 Uiso 1 1 calc R . .
H44B H 0.1729 -0.0149 0.0414 0.060 Uiso 1 1 calc R . .
C45 C 0.6726(8) 0.7886(7) 0.3697(8) 0.246(5) Uani 1 1 d . . .
H45A H 0.7412 0.7403 0.3501 0.369 Uiso 1 1 calc R . .
H45B H 0.5818 0.7603 0.3823 0.369 Uiso 1 1 calc R . .
H45C H 0.6841 0.7906 0.4289 0.369 Uiso 1 1 calc R . .
O1 O 0.4109(3) 0.5007(2) -0.2736(2) 0.0788(9) Uani 1 1 d . . .
O2 O 0.2217(3) 0.4392(2) -0.2772(2) 0.0846(10) Uani 1 1 d . . .
H2A H 0.2062 0.5164 -0.3252 0.101 Uiso 1 1 d R . .
O3 O 0.3694(3) 0.03235(18) 0.07557(16) 0.0565(7) Uani 1 1 d . . .
H3 H 0.4224 0.0397 0.1051 0.085 Uiso 1 1 calc R . .
O4 O 0.3825(3) -0.3117(2) 0.5869(2) 0.0888(10) Uani 1 1 d . . .
H4A H 0.4013 -0.3873 0.6390 0.107 Uiso 1 1 d R . .
O5 O 0.1774(3) -0.3609(2) 0.5984(2) 0.0774(9) Uani 1 1 d . . .
O6 O 0.1712(3) 0.2226(2) 0.3851(2) 0.0758(8) Uani 1 1 d . . .
O7 O 0.1997(3) 0.13415(18) 0.28865(16) 0.0529(7) Uani 1 1 d . . .
O8 O 0.1267(2) -0.07162(18) 0.22227(15) 0.0488(6) Uani 1 1 d . . .
O9 O -0.0344(4) -0.1757(2) 0.2269(3) 0.1096(13) Uani 1 1 d . . .
O10 O 0.5234(3) 0.03650(18) 0.18962(18) 0.0606(7) Uani 1 1 d . . .
H10A H 0.5708 -0.0014 0.2282 0.091 Uiso 1 1 calc R . .
O11 O 0.6883(4) 0.8968(3) 0.2941(3) 0.1302(14) Uani 1 1 d . . .
H11A H 0.7787 0.9053 0.2530 0.195 Uiso 1 1 d R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.383(4) . ?
C1 C6 1.394(4) . ?
C1 C7 1.472(5) . ?
C2 C3 1.377(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.391(4) . ?
C3 C44 1.509(4) . ?
C4 O3 1.362(4) . ?
C4 C5 1.406(4) . ?
C5 C6 1.377(4) . ?
C5 C8 1.518(4) . ?
C6 H6 0.9500 . ?
C7 O2 1.256(4) . ?
C7 O1 1.272(4) . ?
C8 C9 1.497(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.385(5) . ?
C9 C14 1.397(5) . ?
C10 C11 1.380(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.381(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.379(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.392(5) . ?
C13 C15 1.516(5) . ?
C14 O10 1.389(4) . ?
C15 C16 1.513(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C18 1.388(4) . ?
C16 C17 1.408(5) . ?
C17 C21 1.395(4) . ?
C17 O7 1.403(4) . ?
C18 C19 1.394(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.381(5) . ?
C19 C22 1.473(5) . ?
C20 C21 1.377(4) . ?
C20 H20 0.9500 . ?
C21 C30 1.511(5) . ?
C22 O4 1.255(4) . ?
C22 O5 1.263(4) . ?
C23 O6 1.199(4) . ?
C23 O7 1.347(4) . ?
C23 C24 1.476(5) . ?
C24 C29 1.365(5) . ?
C24 C25 1.365(5) . ?
C25 C26 1.380(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.352(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.354(7) . ?
C27 H27 0.9500 . ?
C28 C29 1.395(6) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C30 C31 1.521(4) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.384(5) . ?
C31 C36 1.391(4) . ?
C32 C33 1.373(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.365(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.401(5) . ?
C34 H34 0.9500 . ?
C35 C36 1.385(4) . ?
C35 C44 1.509(5) . ?
C36 O8 1.414(4) . ?
C37 O9 1.196(5) . ?
C37 O8 1.342(4) . ?
C37 C38 1.488(6) . ?
C38 C43 1.357(6) . ?
C38 C39 1.372(6) . ?
C39 C40 1.370(8) . ?
C39 H39 0.9500 . ?
C40 C41 1.315(10) . ?
C40 H40 0.9500 . ?
C41 C42 1.395(10) . ?
C41 H41 0.9500 . ?
C42 C43 1.387(6) . ?
C42 H42 0.9500 . ?
C43 H43 0.9500 . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 O11 1.421(9) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
O2 H2A 1.0140 . ?
O3 H3 0.8400 . ?
O4 H4A 1.0345 . ?
O10 H10A 0.8400 . ?
O11 H11A 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
C2 C1 C6 119.3(3) . . ?
C2 C1 C7 120.9(3) . . ?
C6 C1 C7 119.7(3) . . ?
C3 C2 C1 121.3(3) . . ?
C3 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
C2 C3 C4 118.4(3) . . ?
C2 C3 C44 121.3(3) . . ?
C4 C3 C44 120.1(3) . . ?
O3 C4 C3 115.8(3) . . ?
O3 C4 C5 122.3(3) . . ?
C3 C4 C5 121.9(3) . . ?
C6 C5 C4 117.7(3) . . ?
C6 C5 C8 120.5(3) . . ?
C4 C5 C8 121.7(3) . . ?
C5 C6 C1 121.4(3) . . ?
C5 C6 H6 119.3 . . ?
C1 C6 H6 119.3 . . ?
O2 C7 O1 121.8(3) . . ?
O2 C7 C1 120.0(3) . . ?
O1 C7 C1 118.2(3) . . ?
C9 C8 C5 111.6(3) . . ?
C9 C8 H8A 109.3 . . ?
C5 C8 H8A 109.3 . . ?
C9 C8 H8B 109.3 . . ?
C5 C8 H8B 109.3 . . ?
H8A C8 H8B 108.0 . . ?
C10 C9 C14 117.7(3) . . ?
C10 C9 C8 120.1(3) . . ?
C14 C9 C8 122.2(3) . . ?
C11 C10 C9 121.3(3) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C10 C11 C12 119.6(3) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
C13 C12 C11 121.2(4) . . ?
C13 C12 H12 119.4 . . ?
C11 C12 H12 119.4 . . ?
C12 C13 C14 118.1(3) . . ?
C12 C13 C15 119.8(3) . . ?
C14 C13 C15 122.0(3) . . ?
O10 C14 C13 121.0(3) . . ?
O10 C14 C9 116.9(3) . . ?
C13 C14 C9 122.0(3) . . ?
C16 C15 C13 120.3(3) . . ?
C16 C15 H15A 107.2 . . ?
C13 C15 H15A 107.2 . . ?
C16 C15 H15B 107.2 . . ?
C13 C15 H15B 107.2 . . ?
H15A C15 H15B 106.9 . . ?
C18 C16 C17 116.1(3) . . ?
C18 C16 C15 118.3(3) . . ?
C17 C16 C15 125.5(3) . . ?
C21 C17 O7 116.9(3) . . ?
C21 C17 C16 123.7(3) . . ?
O7 C17 C16 119.2(3) . . ?
C16 C18 C19 121.5(3) . . ?
C16 C18 H18 119.2 . . ?
C19 C18 H18 119.2 . . ?
C20 C19 C18 120.0(3) . . ?
C20 C19 C22 120.5(3) . . ?
C18 C19 C22 119.4(3) . . ?
C21 C20 C19 121.3(3) . . ?
C21 C20 H20 119.4 . . ?
C19 C20 H20 119.4 . . ?
C20 C21 C17 117.4(3) . . ?
C20 C21 C30 119.1(3) . . ?
C17 C21 C30 123.3(3) . . ?
O4 C22 O5 122.3(3) . . ?
O4 C22 C19 118.2(4) . . ?
O5 C22 C19 119.4(4) . . ?
O6 C23 O7 122.6(3) . . ?
O6 C23 C24 126.7(4) . . ?
O7 C23 C24 110.7(3) . . ?
C29 C24 C25 119.2(4) . . ?
C29 C24 C23 118.5(4) . . ?
C25 C24 C23 122.3(3) . . ?
C24 C25 C26 120.3(4) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C27 C26 C25 120.1(4) . . ?
C27 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C26 C27 C28 120.7(4) . . ?
C26 C27 H27 119.7 . . ?
C28 C27 H27 119.7 . . ?
C27 C28 C29 119.2(5) . . ?
C27 C28 H28 120.4 . . ?
C29 C28 H28 120.4 . . ?
C24 C29 C28 120.4(5) . . ?
C24 C29 H29 119.8 . . ?
C28 C29 H29 119.8 . . ?
C21 C30 C31 119.6(3) . . ?
C21 C30 H30A 107.4 . . ?
C31 C30 H30A 107.4 . . ?
C21 C30 H30B 107.4 . . ?
C31 C30 H30B 107.4 . . ?
H30A C30 H30B 106.9 . . ?
C32 C31 C36 117.4(3) . . ?
C32 C31 C30 120.1(3) . . ?
C36 C31 C30 122.5(3) . . ?
C33 C32 C31 120.7(4) . . ?
C33 C32 H32 119.7 . . ?
C31 C32 H32 119.7 . . ?
C34 C33 C32 120.2(3) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C33 C34 C35 122.1(3) . . ?
C33 C34 H34 118.9 . . ?
C35 C34 H34 118.9 . . ?
C36 C35 C34 115.6(3) . . ?
C36 C35 C44 123.7(3) . . ?
C34 C35 C44 120.6(3) . . ?
C35 C36 C31 123.8(3) . . ?
C35 C36 O8 120.4(3) . . ?
C31 C36 O8 115.8(3) . . ?
O9 C37 O8 123.7(4) . . ?
O9 C37 C38 124.2(4) . . ?
O8 C37 C38 112.0(4) . . ?
C43 C38 C39 119.2(5) . . ?
C43 C38 C37 122.3(4) . . ?
C39 C38 C37 118.4(5) . . ?
C40 C39 C38 120.6(7) . . ?
C40 C39 H39 119.7 . . ?
C38 C39 H39 119.7 . . ?
C41 C40 C39 120.9(8) . . ?
C41 C40 H40 119.5 . . ?
C39 C40 H40 119.5 . . ?
C40 C41 C42 119.9(7) . . ?
C40 C41 H41 120.0 . . ?
C42 C41 H41 120.0 . . ?
C43 C42 C41 119.3(7) . . ?
C43 C42 H42 120.3 . . ?
C41 C42 H42 120.3 . . ?
C38 C43 C42 119.9(6) . . ?
C38 C43 H43 120.1 . . ?
C42 C43 H43 120.1 . . ?
C35 C44 C3 111.1(3) . . ?
C35 C44 H44A 109.4 . . ?
C3 C44 H44A 109.4 . . ?
C35 C44 H44B 109.4 . . ?
C3 C44 H44B 109.4 . . ?
H44A C44 H44B 108.0 . . ?
O11 C45 H45A 109.5 . . ?
O11 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
O11 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C7 O2 H2A 117.3 . . ?
C4 O3 H3 109.5 . . ?
C22 O4 H4A 122.2 . . ?
C23 O7 C17 120.0(3) . . ?
C37 O8 C36 115.8(3) . . ?
C14 O10 H10A 109.5 . . ?
C45 O11 H11A 109.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 1.0(5) . . . . ?
C7 C1 C2 C3 -177.4(3) . . . . ?
C1 C2 C3 C4 -0.3(5) . . . . ?
C1 C2 C3 C44 174.0(3) . . . . ?
C2 C3 C4 O3 179.6(3) . . . . ?
C44 C3 C4 O3 5.1(4) . . . . ?
C2 C3 C4 C5 -0.9(5) . . . . ?
C44 C3 C4 C5 -175.3(3) . . . . ?
O3 C4 C5 C6 -179.1(3) . . . . ?
C3 C4 C5 C6 1.4(5) . . . . ?
O3 C4 C5 C8 -2.9(5) . . . . ?
C3 C4 C5 C8 177.6(3) . . . . ?
C4 C5 C6 C1 -0.7(5) . . . . ?
C8 C5 C6 C1 -177.0(3) . . . . ?
C2 C1 C6 C5 -0.5(5) . . . . ?
C7 C1 C6 C5 178.0(3) . . . . ?
C2 C1 C7 O2 -4.9(5) . . . . ?
C6 C1 C7 O2 176.7(3) . . . . ?
C2 C1 C7 O1 174.0(3) . . . . ?
C6 C1 C7 O1 -4.4(5) . . . . ?
C6 C5 C8 C9 95.6(4) . . . . ?
C4 C5 C8 C9 -80.5(4) . . . . ?
C5 C8 C9 C10 -80.9(4) . . . . ?
C5 C8 C9 C14 97.8(4) . . . . ?
C14 C9 C10 C11 0.1(5) . . . . ?
C8 C9 C10 C11 178.8(3) . . . . ?
C9 C10 C11 C12 -1.8(6) . . . . ?
C10 C11 C12 C13 1.2(6) . . . . ?
C11 C12 C13 C14 1.1(5) . . . . ?
C11 C12 C13 C15 179.0(3) . . . . ?
C12 C13 C14 O10 -179.5(3) . . . . ?
C15 C13 C14 O10 2.6(5) . . . . ?
C12 C13 C14 C9 -2.9(5) . . . . ?
C15 C13 C14 C9 179.3(3) . . . . ?
C10 C9 C14 O10 179.1(3) . . . . ?
C8 C9 C14 O10 0.4(5) . . . . ?
C10 C9 C14 C13 2.3(5) . . . . ?
C8 C9 C14 C13 -176.4(3) . . . . ?
C12 C13 C15 C16 126.8(4) . . . . ?
C14 C13 C15 C16 -55.3(5) . . . . ?
C13 C15 C16 C18 143.8(4) . . . . ?
C13 C15 C16 C17 -40.4(5) . . . . ?
C18 C16 C17 C21 0.1(5) . . . . ?
C15 C16 C17 C21 -175.7(3) . . . . ?
C18 C16 C17 O7 -174.4(3) . . . . ?
C15 C16 C17 O7 9.7(5) . . . . ?
C17 C16 C18 C19 0.2(5) . . . . ?
C15 C16 C18 C19 176.4(3) . . . . ?
C16 C18 C19 C20 0.5(5) . . . . ?
C16 C18 C19 C22 177.9(3) . . . . ?
C18 C19 C20 C21 -1.6(5) . . . . ?
C22 C19 C20 C21 -179.0(3) . . . . ?
C19 C20 C21 C17 1.9(5) . . . . ?
C19 C20 C21 C30 -174.6(3) . . . . ?
O7 C17 C21 C20 173.5(3) . . . . ?
C16 C17 C21 C20 -1.1(5) . . . . ?
O7 C17 C21 C30 -10.2(5) . . . . ?
C16 C17 C21 C30 175.2(3) . . . . ?
C20 C19 C22 O4 176.6(4) . . . . ?
C18 C19 C22 O4 -0.9(5) . . . . ?
C20 C19 C22 O5 -2.1(5) . . . . ?
C18 C19 C22 O5 -179.5(4) . . . . ?
O6 C23 C24 C29 -6.6(6) . . . . ?
O7 C23 C24 C29 173.3(4) . . . . ?
O6 C23 C24 C25 171.1(4) . . . . ?
O7 C23 C24 C25 -9.0(5) . . . . ?
C29 C24 C25 C26 -1.9(6) . . . . ?
C23 C24 C25 C26 -179.5(4) . . . . ?
C24 C25 C26 C27 -0.2(7) . . . . ?
C25 C26 C27 C28 1.0(8) . . . . ?
C26 C27 C28 C29 0.1(9) . . . . ?
C25 C24 C29 C28 3.0(7) . . . . ?
C23 C24 C29 C28 -179.2(5) . . . . ?
C27 C28 C29 C24 -2.2(9) . . . . ?
C20 C21 C30 C31 -137.1(3) . . . . ?
C17 C21 C30 C31 46.7(5) . . . . ?
C21 C30 C31 C32 -132.9(3) . . . . ?
C21 C30 C31 C36 50.1(5) . . . . ?
C36 C31 C32 C33 -0.2(5) . . . . ?
C30 C31 C32 C33 -177.4(3) . . . . ?
C31 C32 C33 C34 -2.4(6) . . . . ?
C32 C33 C34 C35 1.3(6) . . . . ?
C33 C34 C35 C36 2.2(5) . . . . ?
C33 C34 C35 C44 -175.0(3) . . . . ?
C34 C35 C36 C31 -5.0(5) . . . . ?
C44 C35 C36 C31 172.2(3) . . . . ?
C34 C35 C36 O8 177.1(3) . . . . ?
C44 C35 C36 O8 -5.8(5) . . . . ?
C32 C31 C36 C35 4.1(5) . . . . ?
C30 C31 C36 C35 -178.8(3) . . . . ?
C32 C31 C36 O8 -177.9(3) . . . . ?
C30 C31 C36 O8 -0.8(4) . . . . ?
O9 C37 C38 C43 172.8(5) . . . . ?
O8 C37 C38 C43 -9.1(6) . . . . ?
O9 C37 C38 C39 -11.3(7) . . . . ?
O8 C37 C38 C39 166.8(4) . . . . ?
C43 C38 C39 C40 0.7(8) . . . . ?
C37 C38 C39 C40 -175.3(5) . . . . ?
C38 C39 C40 C41 1.4(12) . . . . ?
C39 C40 C41 C42 -3.2(13) . . . . ?
C40 C41 C42 C43 3.0(11) . . . . ?
C39 C38 C43 C42 -0.9(7) . . . . ?
C37 C38 C43 C42 174.9(4) . . . . ?
C41 C42 C43 C38 -0.9(8) . . . . ?
C36 C35 C44 C3 -102.4(4) . . . . ?
C34 C35 C44 C3 74.6(4) . . . . ?
C2 C3 C44 C35 -91.0(4) . . . . ?
C4 C3 C44 C35 83.3(4) . . . . ?
O6 C23 O7 C17 1.3(5) . . . . ?
C24 C23 O7 C17 -178.6(3) . . . . ?
C21 C17 O7 C23 108.7(4) . . . . ?
C16 C17 O7 C23 -76.4(4) . . . . ?
O9 C37 O8 C36 11.2(6) . . . . ?
C38 C37 O8 C36 -166.9(3) . . . . ?
C35 C36 O8 C37 -89.5(4) . . . . ?
C31 C36 O8 C37 92.4(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.044
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1432496'
_audit_update_record             
;
2015-10-21 deposited with the CCDC.
2018-12-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H32 O10'
_chemical_formula_weight         720.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'

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

_cell_length_a                   27.040(6)
_cell_length_b                   17.777(4)
_cell_length_c                   8.1345(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3910.2(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    203(2)
_cell_measurement_reflns_used    5056
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      26.29

_exptl_crystal_description       rhombus
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1504
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.632
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      203(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27221
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0412
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         1.89
_diffrn_reflns_theta_max         27.46
_reflns_number_total             4614
_reflns_number_gt                3249
_reflns_threshold_expression     >2sigma(I)

_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-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0987P)²+1.9659P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4614
_refine_ls_number_parameters     257
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0906
_refine_ls_R_factor_gt           0.0649
_refine_ls_wR_factor_ref         0.1964
_refine_ls_wR_factor_gt          0.1833
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      5.461
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.0807(3) 0.1873(5) 0.9483(14) 0.054(3) Uani 1 1 d D . .
H1 H 0.0568 0.1943 1.0105 0.065 Uiso 0.50 1 calc PRD . .
O2 O 0.2874(4) 0.2500 0.6185(14) 0.030(3) Uani 1 2 d SD . .
H2 H 0.3000 0.2081 0.5985 0.06(11) Uiso 0.50 1 d PRD . .
O3 O 0.2926(5) 0.2500 0.0417(16) 0.042(3) Uani 1 2 d SD . .
H3A H 0.2818 0.1986 0.0247 0.050 Uiso 0.50 1 d PR . .
O4 O 0.4949(4) 0.1870(6) 0.4004(16) 0.062(3) Uani 1 1 d . . .
H4 H 0.5213 0.1942 0.4503 0.093 Uiso 0.50 1 calc PR . .
O5 O 0.3302(3) 0.1086(4) 0.4800(9) 0.0256(18) Uani 1 1 d . . .
O6 O 0.3541(3) -0.0077(5) 0.4061(11) 0.039(2) Uani 1 1 d . . .
C1 C 0.1012(6) 0.2500 0.916(2) 0.032(4) Uani 1 2 d S . .
C2 C 0.1496(6) 0.2500 0.8368(19) 0.026(3) Uani 1 2 d S . .
C3 C 0.1729(4) 0.1822(6) 0.7966(13) 0.025(2) Uani 1 1 d . . .
H3 H 0.1570 0.1365 0.8207 0.030 Uiso 1 1 calc RD . .
C4 C 0.2188(4) 0.1809(6) 0.7221(12) 0.023(2) Uani 1 1 d . . .
C5 C 0.2417(5) 0.2500 0.6872(17) 0.021(3) Uani 1 2 d S . .
C6 C 0.2429(4) 0.1073(6) 0.6718(14) 0.028(2) Uani 1 1 d . . .
H6A H 0.2770 0.1061 0.7120 0.033 Uiso 1 1 calc R . .
H6B H 0.2249 0.0654 0.7224 0.033 Uiso 1 1 calc R . .
C7 C 0.2427(4) 0.0980(6) 0.4863(14) 0.025(2) Uani 1 1 d . . .
C8 C 0.1982(5) 0.0908(7) 0.4035(16) 0.035(3) Uani 1 1 d . . .
H8 H 0.1686 0.0881 0.4637 0.042 Uiso 1 1 calc R . .
C9 C 0.1966(5) 0.0876(7) 0.2338(16) 0.036(3) Uani 1 1 d . . .
H9 H 0.1661 0.0825 0.1794 0.043 Uiso 1 1 calc R . .
C10 C 0.2402(4) 0.0919(7) 0.1436(15) 0.032(3) Uani 1 1 d . . .
H10 H 0.2388 0.0900 0.0282 0.038 Uiso 1 1 calc R . .
C11 C 0.2857(4) 0.0990(6) 0.2209(13) 0.026(2) Uani 1 1 d . . .
C12 C 0.3328(4) 0.1076(6) 0.1223(14) 0.029(3) Uani 1 1 d . . .
H12A H 0.3549 0.0656 0.1477 0.035 Uiso 1 1 calc R . .
H12B H 0.3247 0.1051 0.0049 0.035 Uiso 1 1 calc R . .
C13 C 0.3594(4) 0.1809(6) 0.1568(13) 0.027(2) Uani 1 1 d . . .
C14 C 0.3370(6) 0.2500 0.1198(18) 0.026(3) Uani 1 2 d S . .
C15 C 0.4052(4) 0.1824(7) 0.2339(15) 0.031(3) Uani 1 1 d . . .
H15 H 0.4211 0.1368 0.2591 0.037 Uiso 1 1 calc R . .
C16 C 0.4281(6) 0.2500 0.274(2) 0.032(4) Uani 1 2 d S . .
C17 C 0.4754(6) 0.2500 0.364(2) 0.037(4) Uani 1 2 d S . .
C18 C 0.2856(4) 0.1002(6) 0.3929(13) 0.024(2) Uani 1 1 d . . .
C19 C 0.3608(4) 0.0478(6) 0.4862(14) 0.029(2) Uani 1 1 d . . .
C20 C 0.4019(4) 0.0585(7) 0.6032(15) 0.034(3) Uani 1 1 d . . .
C21 C 0.4065(6) 0.1228(9) 0.7003(18) 0.050(4) Uani 1 1 d . . .
H21 H 0.3835 0.1620 0.6904 0.060 Uiso 1 1 calc R . .
C22 C 0.4450(7) 0.1288(12) 0.811(2) 0.069(5) Uani 1 1 d . . .
H22 H 0.4479 0.1715 0.8785 0.083 Uiso 1 1 calc R . .
C23 C 0.4793(7) 0.0708(13) 0.821(2) 0.075(6) Uani 1 1 d . . .
H23 H 0.5059 0.0750 0.8950 0.090 Uiso 1 1 calc R . .
C24 C 0.4751(6) 0.0077(12) 0.726(2) 0.070(5) Uani 1 1 d . . .
H24 H 0.4988 -0.0309 0.7338 0.084 Uiso 1 1 calc R . .
C25 C 0.4362(5) 0.0008(9) 0.6176(19) 0.049(4) Uani 1 1 d . . .
H25 H 0.4329 -0.0429 0.5536 0.058 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.272(12) . ?
O1 H1 0.8300 . ?
O2 C5 1.357(18) . ?
O2 H2 0.8353 . ?
O3 C14 1.360(19) . ?
O3 H3A 0.9700 . ?
O4 C17 1.272(13) . ?
O4 H4 0.8300 . ?
O5 C19 1.361(13) . ?
O5 C18 1.407(13) . ?
O6 C19 1.197(14) . ?
C1 O1 1.272(12) 7_565 ?
C1 C2 1.46(2) . ?
C2 C3 1.400(13) . ?
C2 C3 1.400(13) 7_565 ?
C3 C4 1.382(15) . ?
C3 H3 0.9400 . ?
C4 C5 1.403(12) . ?
C4 C6 1.516(14) . ?
C5 C4 1.403(12) 7_565 ?
C6 C7 1.518(15) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 C8 1.385(17) . ?
C7 C18 1.388(15) . ?
C8 C9 1.383(19) . ?
C8 H8 0.9400 . ?
C9 C10 1.390(18) . ?
C9 H9 0.9400 . ?
C10 C11 1.387(16) . ?
C10 H10 0.9400 . ?
C11 C18 1.399(15) . ?
C11 C12 1.512(16) . ?
C12 C13 1.515(16) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C13 C15 1.389(16) . ?
C13 C14 1.402(13) . ?
C14 C13 1.402(13) 7_565 ?
C15 C16 1.392(14) . ?
C15 H15 0.9400 . ?
C16 C15 1.392(14) 7_565 ?
C16 C17 1.47(2) . ?
C17 O4 1.272(13) 7_565 ?
C19 C20 1.476(16) . ?
C20 C25 1.390(19) . ?
C20 C21 1.39(2) . ?
C21 C22 1.38(2) . ?
C21 H21 0.9400 . ?
C22 C23 1.39(3) . ?
C22 H22 0.9400 . ?
C23 C24 1.37(3) . ?
C23 H23 0.9400 . ?
C24 C25 1.37(2) . ?
C24 H24 0.9400 . ?
C25 H25 0.9400 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O1 H1 109.5 . . ?
C5 O2 H2 116.9 . . ?
C14 O3 H3A 109.5 . . ?
C17 O4 H4 109.5 . . ?
C19 O5 C18 117.0(8) . . ?
O1 C1 O1 122.4(15) . 7_565 ?
O1 C1 C2 118.8(8) . . ?
O1 C1 C2 118.8(8) 7_565 . ?
C3 C2 C3 119.0(14) . 7_565 ?
C3 C2 C1 120.5(7) . . ?
C3 C2 C1 120.5(7) 7_565 . ?
C4 C3 C2 121.4(10) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C3 C4 C5 118.0(10) . . ?
C3 C4 C6 121.1(9) . . ?
C5 C4 C6 120.8(10) . . ?
O2 C5 C4 118.9(7) . . ?
O2 C5 C4 118.9(7) . 7_565 ?
C4 C5 C4 122.1(13) . 7_565 ?
C7 C6 C4 111.2(9) . . ?
C7 C6 H6A 109.4 . . ?
C4 C6 H6A 109.4 . . ?
C7 C6 H6B 109.4 . . ?
C4 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
C8 C7 C18 117.6(10) . . ?
C8 C7 C6 119.7(10) . . ?
C18 C7 C6 122.6(10) . . ?
C9 C8 C7 121.1(11) . . ?
C9 C8 H8 119.5 . . ?
C7 C8 H8 119.5 . . ?
C8 C9 C10 119.9(11) . . ?
C8 C9 H9 120.0 . . ?
C10 C9 H9 120.0 . . ?
C11 C10 C9 121.2(11) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C10 C11 C18 116.9(10) . . ?
C10 C11 C12 121.0(10) . . ?
C18 C11 C12 122.0(10) . . ?
C13 C12 C11 112.9(9) . . ?
C13 C12 H12A 109.0 . . ?
C11 C12 H12A 109.0 . . ?
C13 C12 H12B 109.0 . . ?
C11 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
C15 C13 C14 117.8(11) . . ?
C15 C13 C12 121.6(10) . . ?
C14 C13 C12 120.6(10) . . ?
O3 C14 C13 118.8(7) . 7_565 ?
O3 C14 C13 118.8(7) . . ?
C13 C14 C13 122.4(14) 7_565 . ?
C13 C15 C16 121.3(11) . . ?
C13 C15 H15 119.3 . . ?
C16 C15 H15 119.3 . . ?
C15 C16 C15 119.4(15) . 7_565 ?
C15 C16 C17 120.3(8) . . ?
C15 C16 C17 120.3(8) 7_565 . ?
O4 C17 O4 123.3(16) 7_565 . ?
O4 C17 C16 118.3(8) 7_565 . ?
O4 C17 C16 118.3(8) . . ?
C7 C18 C11 123.3(10) . . ?
C7 C18 O5 116.4(9) . . ?
C11 C18 O5 120.2(10) . . ?
O6 C19 O5 122.9(10) . . ?
O6 C19 C20 124.9(11) . . ?
O5 C19 C20 112.2(10) . . ?
C25 C20 C21 119.8(12) . . ?
C25 C20 C19 117.6(12) . . ?
C21 C20 C19 122.6(12) . . ?
C22 C21 C20 120.1(15) . . ?
C22 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
C21 C22 C23 119.0(17) . . ?
C21 C22 H22 120.5 . . ?
C23 C22 H22 120.5 . . ?
C24 C23 C22 121.2(15) . . ?
C24 C23 H23 119.4 . . ?
C22 C23 H23 119.4 . . ?
C23 C24 C25 120.0(16) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C24 C25 C20 119.9(15) . . ?
C24 C25 H25 120.0 . . ?
C20 C25 H25 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 0(2) . . . . ?
O1 C1 C2 C3 -178.7(14) 7_565 . . . ?
O1 C1 C2 C3 178.7(14) . . . 7_565 ?
O1 C1 C2 C3 0(2) 7_565 . . 7_565 ?
C3 C2 C3 C4 2(2) 7_565 . . . ?
C1 C2 C3 C4 -179.7(13) . . . . ?
C2 C3 C4 C5 -0.1(17) . . . . ?
C2 C3 C4 C6 -177.2(11) . . . . ?
C3 C4 C5 O2 178.1(11) . . . . ?
C6 C4 C5 O2 -4.8(18) . . . . ?
C3 C4 C5 C4 -2(2) . . . 7_565 ?
C6 C4 C5 C4 175.6(9) . . . 7_565 ?
C3 C4 C6 C7 108.1(11) . . . . ?
C5 C4 C6 C7 -68.9(14) . . . . ?
C4 C6 C7 C8 -65.1(13) . . . . ?
C4 C6 C7 C18 111.4(12) . . . . ?
C18 C7 C8 C9 -1.3(17) . . . . ?
C6 C7 C8 C9 175.4(11) . . . . ?
C7 C8 C9 C10 -0.3(19) . . . . ?
C8 C9 C10 C11 0.4(19) . . . . ?
C9 C10 C11 C18 1.1(17) . . . . ?
C9 C10 C11 C12 -176.8(11) . . . . ?
C10 C11 C12 C13 119.0(11) . . . . ?
C18 C11 C12 C13 -58.8(14) . . . . ?
C11 C12 C13 C15 113.2(12) . . . . ?
C11 C12 C13 C14 -63.1(14) . . . . ?
C15 C13 C14 O3 178.8(12) . . . . ?
C12 C13 C14 O3 -4.7(19) . . . . ?
C15 C13 C14 C13 0(2) . . . 7_565 ?
C12 C13 C14 C13 177.0(9) . . . 7_565 ?
C14 C13 C15 C16 0.5(18) . . . . ?
C12 C13 C15 C16 -176.0(12) . . . . ?
C13 C15 C16 C15 -1(2) . . . 7_565 ?
C13 C15 C16 C17 176.7(14) . . . . ?
C15 C16 C17 O4 -179.3(16) . . . 7_565 ?
C15 C16 C17 O4 -1(3) 7_565 . . 7_565 ?
C15 C16 C17 O4 1(3) . . . . ?
C15 C16 C17 O4 179.3(16) 7_565 . . . ?
C8 C7 C18 C11 3.0(16) . . . . ?
C6 C7 C18 C11 -173.6(10) . . . . ?
C8 C7 C18 O5 179.1(9) . . . . ?
C6 C7 C18 O5 2.5(15) . . . . ?
C10 C11 C18 C7 -2.8(16) . . . . ?
C12 C11 C18 C7 175.0(10) . . . . ?
C10 C11 C18 O5 -178.8(9) . . . . ?
C12 C11 C18 O5 -0.9(16) . . . . ?
C19 O5 C18 C7 109.2(11) . . . . ?
C19 O5 C18 C11 -74.5(13) . . . . ?
C18 O5 C19 O6 9.1(16) . . . . ?
C18 O5 C19 C20 -170.2(9) . . . . ?
O6 C19 C20 C25 2.1(19) . . . . ?
O5 C19 C20 C25 -178.6(11) . . . . ?
O6 C19 C20 C21 -176.4(13) . . . . ?
O5 C19 C20 C21 2.9(17) . . . . ?
C25 C20 C21 C22 0(2) . . . . ?
C19 C20 C21 C22 178.1(15) . . . . ?
C20 C21 C22 C23 1(3) . . . . ?
C21 C22 C23 C24 -1(3) . . . . ?
C22 C23 C24 C25 0(3) . . . . ?
C23 C24 C25 C20 1(3) . . . . ?
C21 C20 C25 C24 -1(2) . . . . ?
C19 C20 C25 C24 -179.6(14) . . . . ?

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.408 0.750 -0.038 172.5 23.3
2 0.592 0.250 0.038 172.6 23.4
3 0.092 0.250 0.462 172.4 23.2
4 0.908 0.750 0.538 172.5 23.4
_platon_squeeze_details          
; 
;


_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.46
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.062
####################################################################### 
# 
# 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_6.MeOH
_database_code_depnum_ccdc_archive 'CCDC 1432499'
_audit_update_record             
;
2015-10-21 deposited with the CCDC.
2018-12-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H52 O11'
_chemical_formula_weight         756.86

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Fddd

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'

_cell_length_a                   22.73(2)
_cell_length_b                   26.88(2)
_cell_length_c                   28.36(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     17327(32)
_cell_formula_units_Z            16
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6464
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9752
_exptl_absorpt_correction_T_max  0.9796
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17504
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         23.10
_reflns_number_total             2943
_reflns_number_gt                2136
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 

 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2943
_refine_ls_number_parameters     271
_refine_ls_number_restraints     29
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0755
_refine_ls_wR_factor_ref         0.2927
_refine_ls_wR_factor_gt          0.2592
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_restrained_S_all      1.265
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.00264(15) 0.10325(13) 0.30183(14) 0.0645(10) Uani 1 1 d . B .
H1A H 1.0346 0.0795 0.3043 0.077 Uiso 1 1 calc R . .
H1B H 1.0118 0.1260 0.2763 0.077 Uiso 1 1 calc R . .
C2 C 0.94622(15) 0.07590(12) 0.29060(13) 0.0573(9) Uani 1 1 d . . .
C3 C 0.94298(16) 0.02483(13) 0.29522(13) 0.0624(10) Uani 1 1 d . . .
H3 H 0.9771 0.0068 0.3013 0.075 Uiso 1 1 calc R . .
C4 C 0.88948(15) -0.00016(12) 0.29098(14) 0.0618(10) Uani 1 1 d . . .
C5 C 0.83875(16) 0.02704(13) 0.28251(14) 0.0626(10) Uani 1 1 d . . .
H5 H 0.8030 0.0104 0.2804 0.075 Uiso 1 1 calc R . .
C6 C 0.83977(15) 0.07771(12) 0.27717(12) 0.0563(9) Uani 1 1 d . . .
C7 C 0.89454(15) 0.10192(12) 0.27946(12) 0.0562(9) Uani 1 1 d . . .
C8 C 0.78335(15) 0.10631(13) 0.27229(13) 0.0641(10) Uani 1 1 d . . .
H8A H 0.7517 0.0836 0.2641 0.077 Uiso 1 1 calc R . .
H8B H 0.7872 0.1304 0.2470 0.077 Uiso 1 1 calc R . .
C9 C 0.9119(4) 0.17362(18) 0.2298(2) 0.122(2) Uani 1 1 d D . .
H9 H 0.9547 0.1736 0.2345 0.146 Uiso 1 1 calc R . .
C10 C 0.9030(3) 0.2264(2) 0.2310(2) 0.127(2) Uani 1 1 d . . .
H10A H 0.9076 0.2406 0.2002 0.191 Uiso 1 1 d R . .
H10B H 0.9315 0.2406 0.2520 0.191 Uiso 1 1 d R . .
H10C H 0.8642 0.2332 0.2425 0.191 Uiso 1 1 d R . .
C11 C 0.9103(6) 0.1438(3) 0.1880(2) 0.210(5) Uani 1 1 d D . .
H11A H 0.8711 0.1316 0.1832 0.315 Uiso 1 1 calc R . .
H11B H 0.9369 0.1162 0.1914 0.315 Uiso 1 1 calc R . .
H11C H 0.9219 0.1636 0.1614 0.315 Uiso 1 1 calc R . .
C12 C 0.88487(18) -0.05474(14) 0.29676(16) 0.0732(11) Uani 1 1 d . . .
C13 C 0.99509(13) 0.10742(12) 0.39086(13) 0.0562(10) Uani 1 1 d . B .
C14 C 0.98164(14) 0.13292(12) 0.43236(14) 0.0599(10) Uani 1 1 d . . .
C15 C 0.97607(17) 0.18403(14) 0.43004(16) 0.0704(11) Uani 1 1 d . B .
H15 H 0.9683 0.2017 0.4575 0.084 Uiso 1 1 calc R . .
C16 C 0.98155(18) 0.20909(14) 0.38889(17) 0.0735(12) Uani 1 1 d . . .
H16 H 0.9788 0.2436 0.3884 0.088 Uiso 0.50 1 calc PR A 2
C17 C 0.99115(18) 0.18325(15) 0.34768(18) 0.0748(12) Uani 1 1 d . B .
H17 H 0.9933 0.2006 0.3194 0.090 Uiso 1 1 calc R . .
C18 C 0.99769(14) 0.13210(13) 0.34739(14) 0.0607(10) Uani 1 1 d . . .
C19 C 0.9719(4) 0.2670(2) 0.3885(3) 0.0690(15) Uani 0.50 1 d PU B 1
C20 C 1.0482(3) -0.02032(19) 0.3985(2) 0.122(2) Uani 1 1 d . . .
H20A H 1.0606 -0.0268 0.3667 0.183 Uiso 1 1 calc R . .
H20B H 1.0084 -0.0313 0.4026 0.183 Uiso 1 1 calc R . .
H20C H 1.0734 -0.0378 0.4200 0.183 Uiso 1 1 calc R . .
C21 C 1.0518(3) 0.0332(2) 0.4078(3) 0.151(3) Uani 1 1 d DU B .
H21 H 1.0459 0.0346 0.4421 0.181 Uiso 1 1 calc R . .
C22 C 1.1059(3) 0.0562(3) 0.4025(4) 0.203(4) Uani 1 1 d DU . .
H22A H 1.1152 0.0587 0.3696 0.304 Uiso 1 1 calc R . .
H22B H 1.1356 0.0369 0.4181 0.304 Uiso 1 1 calc R . .
H22C H 1.1044 0.0888 0.4161 0.304 Uiso 1 1 calc R . .
C23 C 0.8750 0.3750 0.2957(7) 0.192(5) Uani 1 2 d SU . .
H23A H 0.8760 0.4030 0.2747 0.230 Uiso 0.50 1 d PR . .
H23B H 0.8730 0.3460 0.2747 0.230 Uiso 0.50 1 d PR . .
H23C H 0.8440 0.3764 0.3187 0.230 Uiso 0.50 1 d PR . .
O1 O 0.89595(11) 0.15275(8) 0.27354(9) 0.0644(8) Uani 1 1 d . . .
O2 O 0.83651(14) -0.07530(10) 0.29662(15) 0.1000(12) Uani 1 1 d . . .
O3 O 0.93371(13) -0.07823(9) 0.30092(14) 0.0948(11) Uani 1 1 d . . .
H3A H 0.9272 -0.1082 0.3025 0.142 Uiso 1 1 calc R . .
O4 O 0.9696(3) 0.28656(19) 0.3533(2) 0.0886(16) Uani 0.50 1 d PU B 1
O5 O 0.9602(3) 0.28450(18) 0.4306(2) 0.0932(16) Uani 0.50 1 d PU B 1
H5A H 0.9325 0.3004 0.4288 0.112 Uiso 0.50 1 d PR B 1
O6 O 1.00137(10) 0.05656(9) 0.39097(9) 0.0631(8) Uani 1 1 d . . .
O7 O 0.9274(4) 0.3729(2) 0.3155(3) 0.122(3) Uani 0.50 1 d PU . .
H7A H 0.9353 0.3390 0.3241 0.146 Uiso 0.50 1 d PR . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C18 1.511(6) . ?
C1 C2 1.512(5) . ?
C2 C3 1.381(5) . ?
C2 C7 1.403(5) . ?
C3 C4 1.394(5) . ?
C4 C5 1.386(5) . ?
C4 C12 1.480(5) . ?
C5 C6 1.371(5) . ?
C6 C7 1.406(5) . ?
C6 C8 1.502(5) . ?
C7 O1 1.377(4) . ?
C8 C14 1.511(5) 3_655 ?
C9 O1 1.408(6) . ?
C9 C11 1.432(8) . ?
C9 C10 1.433(7) . ?
C12 O2 1.230(5) . ?
C12 O3 1.282(5) . ?
C13 O6 1.375(4) . ?
C13 C14 1.396(5) . ?
C13 C18 1.401(5) . ?
C14 C15 1.381(5) . ?
C14 C8 1.511(5) 3_655 ?
C15 C16 1.353(6) . ?
C16 C17 1.377(6) . ?
C16 C19 1.573(7) . ?
C17 C18 1.383(5) . ?
C19 O4 1.128(10) . ?
C19 O5 1.309(10) . ?
C20 C21 1.465(8) . ?
C21 C22 1.384(8) . ?
C21 O6 1.392(6) . ?
C23 O7 1.318(10) . ?
C23 O7 1.318(10) 2_655 ?

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
C18 C1 C2 111.5(3) . . ?
C3 C2 C7 118.2(3) . . ?
C3 C2 C1 120.6(3) . . ?
C7 C2 C1 121.0(3) . . ?
C2 C3 C4 121.1(3) . . ?
C5 C4 C3 119.1(3) . . ?
C5 C4 C12 118.9(3) . . ?
C3 C4 C12 122.0(3) . . ?
C6 C5 C4 121.9(3) . . ?
C5 C6 C7 118.0(3) . . ?
C5 C6 C8 120.3(3) . . ?
C7 C6 C8 121.6(3) . . ?
O1 C7 C2 120.2(3) . . ?
O1 C7 C6 118.3(3) . . ?
C2 C7 C6 121.4(3) . . ?
C6 C8 C14 110.9(3) . 3_655 ?
O1 C9 C11 120.0(5) . . ?
O1 C9 C10 109.7(5) . . ?
C11 C9 C10 124.7(6) . . ?
O2 C12 O3 123.5(4) . . ?
O2 C12 C4 120.5(4) . . ?
O3 C12 C4 115.9(3) . . ?
O6 C13 C14 120.6(3) . . ?
O6 C13 C18 117.9(3) . . ?
C14 C13 C18 121.2(3) . . ?
C15 C14 C13 117.9(3) . . ?
C15 C14 C8 119.4(3) . 3_655 ?
C13 C14 C8 122.3(3) . 3_655 ?
C16 C15 C14 121.8(4) . . ?
C15 C16 C17 119.7(4) . . ?
C15 C16 C19 119.1(5) . . ?
C17 C16 C19 121.0(5) . . ?
C16 C17 C18 121.6(4) . . ?
C17 C18 C13 117.4(4) . . ?
C17 C18 C1 121.5(4) . . ?
C13 C18 C1 120.8(3) . . ?
O4 C19 O5 129.0(6) . . ?
O4 C19 C16 118.3(7) . . ?
O5 C19 C16 112.1(6) . . ?
C22 C21 O6 119.5(6) . . ?
C22 C21 C20 117.9(6) . . ?
O6 C21 C20 109.6(5) . . ?
O7 C23 O7 129.4(18) . 2_655 ?
C7 O1 C9 120.6(3) . . ?
C13 O6 C21 122.4(3) . . ?

_diffrn_measured_fraction_theta_max 0.961
_diffrn_reflns_theta_full        23.10
_diffrn_measured_fraction_theta_full 0.961
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.054

# start Validation Reply Form

_vrf_THETM01_6.MeOH              
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575   
RESPONSE: The data were cut around 0.90 angstroms as they were very weak at high
 resolution. The crystals used were very weakly diffracting. Several were
  tested and the best one used to acquire data (over 48 hours), however the 
  data set is still low resolution. 
;
####################################################################### 
# 
# 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_2.THF
_database_code_depnum_ccdc_archive 'CCDC 1432494'
_audit_update_record             
;
2015-10-21 deposited with the CCDC.
2018-12-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H36 O10, 2(C4 H8 O)'
_chemical_formula_sum            'C45 H52 O12'
_chemical_formula_weight         784.87

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/n  '

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

_cell_length_a                   10.6822(18)
_cell_length_b                   17.951(3)
_cell_length_c                   23.180(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.295(3)
_cell_angle_gamma                90.00
_cell_volume                     4425.9(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4365
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      22.65
_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1672
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9899
_exptl_absorpt_correction_T_max  0.9916
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27499
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         24.40
_reflns_number_total             7058
_reflns_number_gt                4092
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.8890P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7058
_refine_ls_number_parameters     548
_refine_ls_number_restraints     477
_refine_ls_R_factor_all          0.1457
_refine_ls_R_factor_gt           0.0975
_refine_ls_wR_factor_ref         0.3252
_refine_ls_wR_factor_gt          0.2736
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.093
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.9161(3) 0.5145(2) 0.38023(16) 0.0482(9) Uani 1 1 d U . .
C2 C 0.8836(4) 0.4770(2) 0.42994(16) 0.0512(10) Uani 1 1 d U . .
C3 C 0.9320(4) 0.4077(3) 0.44093(19) 0.0605(11) Uani 1 1 d U . .
H3 H 0.9139 0.3830 0.4745 0.073 Uiso 1 1 calc R . .
C4 C 1.0071(4) 0.3731(2) 0.4035(2) 0.0632(11) Uani 1 1 d U . .
C5 C 1.0298(4) 0.4084(2) 0.35245(19) 0.0577(11) Uani 1 1 d U . .
H5 H 1.0764 0.3840 0.3262 0.069 Uiso 1 1 calc R . .
C6 C 0.9850(3) 0.4787(2) 0.33979(17) 0.0525(10) Uani 1 1 d U . .
C7 C 0.9340(4) 0.6461(2) 0.4021(2) 0.0671(12) Uani 1 1 d U . .
H7 H 0.9353 0.6333 0.4432 0.081 Uiso 1 1 calc R . .
C8 C 0.8467(6) 0.7112(3) 0.3896(3) 0.112(2) Uani 1 1 d U . .
H8A H 0.8420 0.7229 0.3490 0.169 Uiso 1 1 calc R . .
H8B H 0.8780 0.7536 0.4117 0.169 Uiso 1 1 calc R . .
H8C H 0.7645 0.6986 0.4001 0.169 Uiso 1 1 calc R . .
C9 C 1.0639(5) 0.6584(3) 0.3879(3) 0.0960(18) Uani 1 1 d U . .
H9A H 1.1084 0.6119 0.3897 0.144 Uiso 1 1 calc R . .
H9B H 1.1052 0.6926 0.4153 0.144 Uiso 1 1 calc R . .
H9C H 1.0630 0.6788 0.3496 0.144 Uiso 1 1 calc R . .
C10 C 1.0608(5) 0.2989(3) 0.4187(3) 0.0880(16) Uani 1 1 d U . .
C11 C 1.0061(4) 0.5142(3) 0.28243(17) 0.0583(11) Uani 1 1 d U . .
H11A H 1.0906 0.5026 0.2730 0.070 Uiso 1 1 calc R . .
H11B H 1.0001 0.5679 0.2861 0.070 Uiso 1 1 calc R . .
C12 C 0.9126(4) 0.4884(2) 0.23286(16) 0.0523(10) Uani 1 1 d U . .
C13 C 0.9481(4) 0.4364(2) 0.19381(17) 0.0570(10) Uani 1 1 d U . .
H13 H 1.0289 0.4167 0.1984 0.068 Uiso 1 1 calc R . .
C14 C 0.8660(4) 0.4129(2) 0.14792(16) 0.0549(10) Uani 1 1 d U . .
C15 C 0.7450(4) 0.4424(2) 0.14128(17) 0.0612(11) Uani 1 1 d U . .
H15 H 0.6899 0.4272 0.1101 0.073 Uiso 1 1 calc R . .
C16 C 0.7055(4) 0.4933(2) 0.17943(17) 0.0578(11) Uani 1 1 d U . .
C17 C 0.7901(4) 0.5163(2) 0.22587(16) 0.0523(10) Uani 1 1 d U . .
C18 C 0.9055(5) 0.3575(3) 0.1067(2) 0.0648(12) Uani 1 1 d U . .
C19 C 0.5732(4) 0.5255(3) 0.17281(18) 0.0660(12) Uani 1 1 d U . .
H19A H 0.5767 0.5775 0.1841 0.079 Uiso 1 1 calc R . .
H19B H 0.5409 0.5232 0.1323 0.079 Uiso 1 1 calc R . .
C20 C 0.4835(4) 0.4850(3) 0.20872(18) 0.0611(11) Uani 1 1 d U . .
C21 C 0.4394(5) 0.4150(3) 0.1909(2) 0.0787(14) Uani 1 1 d U . .
H21 H 0.4588 0.3963 0.1553 0.094 Uiso 1 1 calc R . .
C22 C 0.3684(5) 0.3735(3) 0.2244(3) 0.0891(16) Uani 1 1 d U . .
H22 H 0.3376 0.3276 0.2109 0.107 Uiso 1 1 calc R . .
C23 C 0.3411(4) 0.3982(3) 0.2785(2) 0.0752(13) Uani 1 1 d U . .
H23 H 0.2957 0.3681 0.3017 0.090 Uiso 1 1 calc R . .
C24 C 0.3812(4) 0.4675(2) 0.29773(18) 0.0578(11) Uani 1 1 d U . .
C25 C 0.4474(4) 0.5116(2) 0.26152(18) 0.0550(10) Uani 1 1 d U . .
C26 C 0.4210(5) 0.6461(3) 0.2526(2) 0.0787(14) Uani 1 1 d U . .
H26 H 0.4095 0.6371 0.2107 0.094 Uiso 1 1 calc R . .
C27 C 0.5103(8) 0.7088(4) 0.2640(4) 0.131(3) Uani 1 1 d U . .
H27A H 0.5200 0.7193 0.3047 0.196 Uiso 1 1 calc R . .
H27B H 0.4783 0.7522 0.2433 0.196 Uiso 1 1 calc R . .
H27C H 0.5903 0.6956 0.2512 0.196 Uiso 1 1 calc R . .
C28 C 0.2974(7) 0.6585(4) 0.2737(4) 0.135(3) Uani 1 1 d U . .
H28A H 0.2500 0.6130 0.2709 0.202 Uiso 1 1 calc R . .
H28B H 0.2531 0.6963 0.2507 0.202 Uiso 1 1 calc R . .
H28C H 0.3082 0.6743 0.3135 0.202 Uiso 1 1 calc R . .
C29 C 0.3594(4) 0.4921(3) 0.35865(18) 0.0623(11) Uani 1 1 d U . .
H29A H 0.3589 0.5461 0.3600 0.075 Uiso 1 1 calc R . .
H29B H 0.2773 0.4749 0.3675 0.075 Uiso 1 1 calc R . .
C30 C 0.4570(4) 0.4635(2) 0.40444(17) 0.0531(10) Uani 1 1 d U . .
C31 C 0.4312(4) 0.4016(2) 0.43691(18) 0.0577(11) Uani 1 1 d U . .
H31 H 0.3540 0.3779 0.4298 0.069 Uiso 1 1 calc R . .
C32 C 0.5182(4) 0.3744(2) 0.47978(17) 0.0586(11) Uani 1 1 d U . .
C33 C 0.6323(4) 0.4105(2) 0.49025(16) 0.0565(10) Uani 1 1 d U . .
H33 H 0.6900 0.3927 0.5195 0.068 Uiso 1 1 calc R . .
C34 C 0.6634(4) 0.4710(2) 0.45926(16) 0.0518(10) Uani 1 1 d U . .
C35 C 0.5732(4) 0.4975(2) 0.41548(16) 0.0512(10) Uani 1 1 d U . .
C36 C 0.4896(4) 0.3083(3) 0.5141(2) 0.0637(11) Uani 1 1 d U . .
C37 C 0.7893(4) 0.5097(3) 0.46935(16) 0.0567(10) Uani 1 1 d U . .
H37A H 0.8218 0.5039 0.5096 0.068 Uiso 1 1 calc R . .
H37B H 0.7787 0.5626 0.4615 0.068 Uiso 1 1 calc R . .
C38 C 0.2408(14) 0.0776(9) 0.4271(8) 0.140(5) Uani 0.50 1 d PDU A 1
H38A H 0.1745 0.0468 0.4083 0.168 Uiso 0.50 1 calc PR A 1
H38B H 0.2230 0.0867 0.4668 0.168 Uiso 0.50 1 calc PR A 1
C39 C 0.3650(17) 0.0415(12) 0.4252(10) 0.179(6) Uani 0.50 1 d PDU A 1
H39A H 0.3995 0.0285 0.4641 0.215 Uiso 0.50 1 calc PR A 1
H39B H 0.3563 -0.0038 0.4024 0.215 Uiso 0.50 1 calc PR A 1
C40 C 0.447(2) 0.0928(12) 0.3995(11) 0.193(6) Uani 0.50 1 d PDU A 1
H40A H 0.4864 0.0684 0.3684 0.232 Uiso 0.50 1 calc PR A 1
H40B H 0.5135 0.1089 0.4284 0.232 Uiso 0.50 1 calc PR A 1
C41 C 0.3736(18) 0.1581(12) 0.3766(10) 0.188(6) Uani 0.50 1 d PDU A 1
H41A H 0.4098 0.2043 0.3920 0.226 Uiso 0.50 1 calc PR A 1
H41B H 0.3681 0.1596 0.3346 0.226 Uiso 0.50 1 calc PR A 1
C42 C 0.6312(14) 0.2361(7) 0.2719(4) 0.229(5) Uani 1 1 d DU . .
H42A H 0.5492 0.2394 0.2503 0.274 Uiso 1 1 calc R . .
H42B H 0.6765 0.1948 0.2565 0.274 Uiso 1 1 calc R . .
C43 C 0.7014(15) 0.3062(8) 0.2658(5) 0.239(5) Uani 1 1 d DU . .
H43A H 0.7889 0.2962 0.2608 0.287 Uiso 1 1 calc R . .
H43B H 0.6650 0.3349 0.2329 0.287 Uiso 1 1 calc R . .
C44 C 0.6894 0.3447 0.3188 0.264 Uani 1 1 d DU . .
H44A H 0.7662 0.3715 0.3310 0.317 Uiso 1 1 calc R . .
H44B H 0.6205 0.3801 0.3142 0.317 Uiso 1 1 calc R . .
C45 C 0.6659(15) 0.2907(6) 0.3595(5) 0.243(5) Uani 1 1 d DU . .
H45A H 0.6059 0.3100 0.3847 0.291 Uiso 1 1 calc R . .
H45B H 0.7432 0.2795 0.3832 0.291 Uiso 1 1 calc R . .
C46 C 0.800(2) 0.1443(13) 0.5478(9) 0.191(6) Uani 0.50 1 d PDU B 2
H46A H 0.8072 0.1860 0.5746 0.230 Uiso 0.50 1 calc PR B 2
H46B H 0.7416 0.1083 0.5616 0.230 Uiso 0.50 1 calc PR B 2
C47 C 0.756(2) 0.1697(13) 0.4894(8) 0.188(6) Uani 0.50 1 d PDU B 2
H47A H 0.6662 0.1617 0.4811 0.226 Uiso 0.50 1 calc PR B 2
H47B H 0.7745 0.2220 0.4842 0.226 Uiso 0.50 1 calc PR B 2
C48 C 0.826(2) 0.1241(13) 0.4544(9) 0.188(6) Uani 0.50 1 d PDU B 2
H48A H 0.8554 0.1540 0.4236 0.226 Uiso 0.50 1 calc PR B 2
H48B H 0.7712 0.0856 0.4367 0.226 Uiso 0.50 1 calc PR B 2
C49 C 0.932(2) 0.0897(16) 0.4875(9) 0.203(7) Uani 0.50 1 d PDU B 2
H49A H 0.9290 0.0359 0.4838 0.244 Uiso 0.50 1 calc PR B 2
H49B H 1.0108 0.1076 0.4749 0.244 Uiso 0.50 1 calc PR B 2
O1 O 0.8741(2) 0.58534(15) 0.36753(11) 0.0558(7) Uani 1 1 d U . .
O2 O 1.1345(5) 0.2730(2) 0.3810(2) 0.1227(15) Uani 1 1 d U . .
H2 H 1.1613 0.2319 0.3916 0.184 Uiso 1 1 calc R . .
O3 O 1.0380(5) 0.2659(3) 0.4623(2) 0.1258(16) Uani 1 1 d U . .
O4 O 0.7476(3) 0.56730(17) 0.26172(12) 0.0676(9) Uani 1 1 d U . .
H4 H 0.8034 0.5776 0.2872 0.101 Uiso 1 1 calc R . .
O5 O 1.0144(3) 0.3292(2) 0.11633(15) 0.0927(12) Uani 1 1 d U . .
H5A H 1.0259 0.2991 0.0908 0.139 Uiso 1 1 calc R . .
O6 O 0.8303(3) 0.3405(2) 0.06322(15) 0.0837(10) Uani 1 1 d U . .
O7 O 0.4846(3) 0.58190(16) 0.28069(12) 0.0590(7) Uani 1 1 d U . .
O8 O 0.6063(3) 0.55948(16) 0.38702(13) 0.0655(8) Uani 1 1 d U . .
H8 H 0.5482 0.5720 0.3635 0.098 Uiso 1 1 calc R . .
O9 O 0.5667(3) 0.2872(2) 0.55392(16) 0.0885(11) Uani 1 1 d U . .
O10 O 0.3827(3) 0.2781(2) 0.50194(14) 0.0915(11) Uani 1 1 d U . .
H10 H 0.3752 0.2424 0.5235 0.137 Uiso 1 1 calc R . .
O11 O 0.2511(10) 0.1444(5) 0.3974(5) 0.138(3) Uani 0.50 1 d PDU A 1
O12 O 0.6171 0.2237 0.3322 0.260 Uani 1 1 d DU . .
O13 O 0.9189(17) 0.1111(11) 0.5430(7) 0.221(6) Uani 0.50 1 d PDU B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.372(5) . ?
C1 C6 1.400(5) . ?
C1 C2 1.406(5) . ?
C2 C3 1.362(6) . ?
C2 C37 1.538(5) . ?
C3 C4 1.382(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.384(6) . ?
C4 C10 1.479(8) . ?
C5 C6 1.372(6) . ?
C5 H5 0.9300 . ?
C6 C11 1.510(6) . ?
C7 O1 1.465(5) . ?
C7 C9 1.473(7) . ?
C7 C8 1.506(8) . ?
C7 H7 0.9800 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 O3 1.216(7) . ?
C10 O2 1.315(7) . ?
C11 C12 1.523(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.377(5) . ?
C12 C17 1.397(6) . ?
C13 C14 1.381(6) . ?
C13 H13 0.9300 . ?
C14 C15 1.392(6) . ?
C14 C18 1.467(6) . ?
C15 C16 1.365(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.403(6) . ?
C16 C19 1.521(6) . ?
C17 O4 1.343(5) . ?
C18 O6 1.268(6) . ?
C18 O5 1.270(5) . ?
C19 C20 1.512(6) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.392(7) . ?
C20 C25 1.400(6) . ?
C21 C22 1.358(7) . ?
C21 H21 0.9300 . ?
C22 C23 1.385(7) . ?
C22 H22 0.9300 . ?
C23 C24 1.378(7) . ?
C23 H23 0.9300 . ?
C24 C25 1.392(6) . ?
C24 C29 1.518(6) . ?
C25 O7 1.385(5) . ?
C26 O7 1.461(5) . ?
C26 C28 1.468(8) . ?
C26 C27 1.483(9) . ?
C26 H26 0.9800 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 C30 1.507(6) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C31 1.383(6) . ?
C30 C35 1.386(6) . ?
C31 C32 1.386(6) . ?
C31 H31 0.9300 . ?
C32 C33 1.382(6) . ?
C32 C36 1.476(6) . ?
C33 C34 1.361(6) . ?
C33 H33 0.9300 . ?
C34 C35 1.416(6) . ?
C34 C37 1.512(6) . ?
C35 O8 1.357(5) . ?
C36 O9 1.238(5) . ?
C36 O10 1.272(5) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 O11 1.392(14) . ?
C38 C39 1.481(16) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 C40 1.441(17) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 C41 1.484(17) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 O11 1.457(15) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 O12 1.437(10) . ?
C42 C43 1.478(14) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 C44 1.428(12) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 C45 1.391(12) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C45 O12 1.435(11) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 O13 1.421(16) . ?
C46 C47 1.463(17) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C47 C48 1.412(16) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 C49 1.450(17) . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C49 O13 1.361(16) . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
O2 H2 0.8200 . ?
O4 H4 0.8200 . ?
O5 H5A 0.8200 . ?
O8 H8 0.8200 . ?
O10 H10 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C6 117.7(3) . . ?
O1 C1 C2 121.3(3) . . ?
C6 C1 C2 120.9(4) . . ?
C3 C2 C1 118.2(4) . . ?
C3 C2 C37 119.7(4) . . ?
C1 C2 C37 121.9(4) . . ?
C2 C3 C4 121.7(4) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 H3 119.2 . . ?
C3 C4 C5 119.3(4) . . ?
C3 C4 C10 119.3(5) . . ?
C5 C4 C10 121.4(5) . . ?
C6 C5 C4 121.3(4) . . ?
C6 C5 H5 119.4 . . ?
C4 C5 H5 119.4 . . ?
C5 C6 C1 118.3(4) . . ?
C5 C6 C11 119.9(4) . . ?
C1 C6 C11 121.7(4) . . ?
O1 C7 C9 111.3(4) . . ?
O1 C7 C8 104.0(4) . . ?
C9 C7 C8 114.9(5) . . ?
O1 C7 H7 108.8 . . ?
C9 C7 H7 108.8 . . ?
C8 C7 H7 108.8 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O3 C10 O2 123.9(6) . . ?
O3 C10 C4 122.3(5) . . ?
O2 C10 C4 113.8(6) . . ?
C6 C11 C12 113.3(3) . . ?
C6 C11 H11A 108.9 . . ?
C12 C11 H11A 108.9 . . ?
C6 C11 H11B 108.9 . . ?
C12 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
C13 C12 C17 118.6(4) . . ?
C13 C12 C11 120.1(4) . . ?
C17 C12 C11 121.4(3) . . ?
C12 C13 C14 121.3(4) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
C13 C14 C15 119.1(4) . . ?
C13 C14 C18 120.5(4) . . ?
C15 C14 C18 120.4(4) . . ?
C16 C15 C14 121.5(4) . . ?
C16 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
C15 C16 C17 118.5(4) . . ?
C15 C16 C19 121.9(4) . . ?
C17 C16 C19 119.6(4) . . ?
O4 C17 C12 122.7(4) . . ?
O4 C17 C16 116.4(4) . . ?
C12 C17 C16 120.9(4) . . ?
O6 C18 O5 123.1(4) . . ?
O6 C18 C14 118.8(4) . . ?
O5 C18 C14 118.1(4) . . ?
C20 C19 C16 113.1(4) . . ?
C20 C19 H19A 109.0 . . ?
C16 C19 H19A 109.0 . . ?
C20 C19 H19B 109.0 . . ?
C16 C19 H19B 109.0 . . ?
H19A C19 H19B 107.8 . . ?
C21 C20 C25 117.0(4) . . ?
C21 C20 C19 119.0(4) . . ?
C25 C20 C19 123.8(4) . . ?
C22 C21 C20 121.1(5) . . ?
C22 C21 H21 119.4 . . ?
C20 C21 H21 119.4 . . ?
C21 C22 C23 121.2(5) . . ?
C21 C22 H22 119.4 . . ?
C23 C22 H22 119.4 . . ?
C24 C23 C22 119.8(5) . . ?
C24 C23 H23 120.1 . . ?
C22 C23 H23 120.1 . . ?
C23 C24 C25 118.6(4) . . ?
C23 C24 C29 119.6(4) . . ?
C25 C24 C29 121.7(4) . . ?
O7 C25 C24 118.1(4) . . ?
O7 C25 C20 119.8(4) . . ?
C24 C25 C20 122.0(4) . . ?
O7 C26 C28 111.5(5) . . ?
O7 C26 C27 104.8(5) . . ?
C28 C26 C27 114.2(6) . . ?
O7 C26 H26 108.7 . . ?
C28 C26 H26 108.7 . . ?
C27 C26 H26 108.7 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 C24 113.6(3) . . ?
C30 C29 H29A 108.8 . . ?
C24 C29 H29A 108.8 . . ?
C30 C29 H29B 108.8 . . ?
C24 C29 H29B 108.8 . . ?
H29A C29 H29B 107.7 . . ?
C31 C30 C35 118.2(4) . . ?
C31 C30 C29 119.8(4) . . ?
C35 C30 C29 122.0(4) . . ?
C30 C31 C32 121.4(4) . . ?
C30 C31 H31 119.3 . . ?
C32 C31 H31 119.3 . . ?
C33 C32 C31 118.8(4) . . ?
C33 C32 C36 120.3(4) . . ?
C31 C32 C36 120.8(4) . . ?
C34 C33 C32 122.4(4) . . ?
C34 C33 H33 118.8 . . ?
C32 C33 H33 118.8 . . ?
C33 C34 C35 117.6(4) . . ?
C33 C34 C37 122.8(4) . . ?
C35 C34 C37 119.6(4) . . ?
O8 C35 C30 122.7(4) . . ?
O8 C35 C34 115.6(3) . . ?
C30 C35 C34 121.6(4) . . ?
O9 C36 O10 123.8(4) . . ?
O9 C36 C32 119.4(4) . . ?
O10 C36 C32 116.7(4) . . ?
C34 C37 C2 110.8(3) . . ?
C34 C37 H37A 109.5 . . ?
C2 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C2 C37 H37B 109.5 . . ?
H37A C37 H37B 108.1 . . ?
O11 C38 C39 104.5(13) . . ?
O11 C38 H38A 110.8 . . ?
C39 C38 H38A 110.8 . . ?
O11 C38 H38B 110.8 . . ?
C39 C38 H38B 110.8 . . ?
H38A C38 H38B 108.9 . . ?
C40 C39 C38 108.4(16) . . ?
C40 C39 H39A 110.0 . . ?
C38 C39 H39A 110.0 . . ?
C40 C39 H39B 110.0 . . ?
C38 C39 H39B 110.0 . . ?
H39A C39 H39B 108.4 . . ?
C39 C40 C41 109.1(18) . . ?
C39 C40 H40A 109.9 . . ?
C41 C40 H40A 109.9 . . ?
C39 C40 H40B 109.9 . . ?
C41 C40 H40B 109.9 . . ?
H40A C40 H40B 108.3 . . ?
O11 C41 C40 102.3(16) . . ?
O11 C41 H41A 111.3 . . ?
C40 C41 H41A 111.3 . . ?
O11 C41 H41B 111.3 . . ?
C40 C41 H41B 111.3 . . ?
H41A C41 H41B 109.2 . . ?
O12 C42 C43 108.9(9) . . ?
O12 C42 H42A 109.9 . . ?
C43 C42 H42A 109.9 . . ?
O12 C42 H42B 109.9 . . ?
C43 C42 H42B 109.9 . . ?
H42A C42 H42B 108.3 . . ?
C44 C43 C42 104.1(9) . . ?
C44 C43 H43A 110.9 . . ?
C42 C43 H43A 110.9 . . ?
C44 C43 H43B 110.9 . . ?
C42 C43 H43B 110.9 . . ?
H43A C43 H43B 108.9 . . ?
C45 C44 C43 106.4(8) . . ?
C45 C44 H44A 110.5 . . ?
C43 C44 H44A 110.5 . . ?
C45 C44 H44B 110.5 . . ?
C43 C44 H44B 110.5 . . ?
H44A C44 H44B 108.6 . . ?
C44 C45 O12 111.4(8) . . ?
C44 C45 H45A 109.3 . . ?
O12 C45 H45A 109.3 . . ?
C44 C45 H45B 109.3 . . ?
O12 C45 H45B 109.3 . . ?
H45A C45 H45B 108.0 . . ?
O13 C46 C47 105.6(18) . . ?
O13 C46 H46A 110.6 . . ?
C47 C46 H46A 110.6 . . ?
O13 C46 H46B 110.6 . . ?
C47 C46 H46B 110.6 . . ?
H46A C46 H46B 108.7 . . ?
C48 C47 C46 102.2(18) . . ?
C48 C47 H47A 111.3 . . ?
C46 C47 H47A 111.3 . . ?
C48 C47 H47B 111.3 . . ?
C46 C47 H47B 111.3 . . ?
H47A C47 H47B 109.2 . . ?
C47 C48 C49 111.8(19) . . ?
C47 C48 H48A 109.3 . . ?
C49 C48 H48A 109.3 . . ?
C47 C48 H48B 109.3 . . ?
C49 C48 H48B 109.3 . . ?
H48A C48 H48B 107.9 . . ?
O13 C49 C48 103.6(18) . . ?
O13 C49 H49A 111.0 . . ?
C48 C49 H49A 111.0 . . ?
O13 C49 H49B 111.0 . . ?
C48 C49 H49B 111.0 . . ?
H49A C49 H49B 109.0 . . ?
C1 O1 C7 117.1(3) . . ?
C10 O2 H2 109.5 . . ?
C17 O4 H4 109.5 . . ?
C18 O5 H5A 109.5 . . ?
C25 O7 C26 118.0(3) . . ?
C35 O8 H8 109.5 . . ?
C36 O10 H10 109.5 . . ?
C38 O11 C41 115.0(12) . . ?
C45 O12 C42 103.5(7) . . ?
C49 O13 C46 111.4(18) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 -177.9(3) . . . . ?
C6 C1 C2 C3 6.8(5) . . . . ?
O1 C1 C2 C37 6.2(5) . . . . ?
C6 C1 C2 C37 -169.1(3) . . . . ?
C1 C2 C3 C4 -2.5(6) . . . . ?
C37 C2 C3 C4 173.5(4) . . . . ?
C2 C3 C4 C5 -2.6(6) . . . . ?
C2 C3 C4 C10 177.8(4) . . . . ?
C3 C4 C5 C6 3.6(6) . . . . ?
C10 C4 C5 C6 -176.8(4) . . . . ?
C4 C5 C6 C1 0.6(6) . . . . ?
C4 C5 C6 C11 -177.1(4) . . . . ?
O1 C1 C6 C5 178.7(3) . . . . ?
C2 C1 C6 C5 -5.8(5) . . . . ?
O1 C1 C6 C11 -3.7(5) . . . . ?
C2 C1 C6 C11 171.7(3) . . . . ?
C3 C4 C10 O3 2.5(8) . . . . ?
C5 C4 C10 O3 -177.1(5) . . . . ?
C3 C4 C10 O2 -177.5(4) . . . . ?
C5 C4 C10 O2 2.9(7) . . . . ?
C5 C6 C11 C12 81.0(5) . . . . ?
C1 C6 C11 C12 -96.5(4) . . . . ?
C6 C11 C12 C13 -102.1(4) . . . . ?
C6 C11 C12 C17 77.8(5) . . . . ?
C17 C12 C13 C14 1.2(6) . . . . ?
C11 C12 C13 C14 -178.9(4) . . . . ?
C12 C13 C14 C15 -0.1(6) . . . . ?
C12 C13 C14 C18 179.9(4) . . . . ?
C13 C14 C15 C16 -0.8(6) . . . . ?
C18 C14 C15 C16 179.2(4) . . . . ?
C14 C15 C16 C17 0.6(6) . . . . ?
C14 C15 C16 C19 -179.5(4) . . . . ?
C13 C12 C17 O4 -179.8(4) . . . . ?
C11 C12 C17 O4 0.3(6) . . . . ?
C13 C12 C17 C16 -1.4(6) . . . . ?
C11 C12 C17 C16 178.7(4) . . . . ?
C15 C16 C17 O4 179.0(4) . . . . ?
C19 C16 C17 O4 -0.9(6) . . . . ?
C15 C16 C17 C12 0.5(6) . . . . ?
C19 C16 C17 C12 -179.4(4) . . . . ?
C13 C14 C18 O6 -175.9(4) . . . . ?
C15 C14 C18 O6 4.2(6) . . . . ?
C13 C14 C18 O5 3.6(6) . . . . ?
C15 C14 C18 O5 -176.3(4) . . . . ?
C15 C16 C19 C20 95.7(5) . . . . ?
C17 C16 C19 C20 -84.4(5) . . . . ?
C16 C19 C20 C21 -74.4(5) . . . . ?
C16 C19 C20 C25 101.4(5) . . . . ?
C25 C20 C21 C22 -2.4(7) . . . . ?
C19 C20 C21 C22 173.7(5) . . . . ?
C20 C21 C22 C23 -2.3(8) . . . . ?
C21 C22 C23 C24 3.1(8) . . . . ?
C22 C23 C24 C25 0.8(7) . . . . ?
C22 C23 C24 C29 -175.5(4) . . . . ?
C23 C24 C25 O7 178.4(4) . . . . ?
C29 C24 C25 O7 -5.3(5) . . . . ?
C23 C24 C25 C20 -5.6(6) . . . . ?
C29 C24 C25 C20 170.7(4) . . . . ?
C21 C20 C25 O7 -177.8(4) . . . . ?
C19 C20 C25 O7 6.4(6) . . . . ?
C21 C20 C25 C24 6.4(6) . . . . ?
C19 C20 C25 C24 -169.5(4) . . . . ?
C23 C24 C29 C30 82.5(5) . . . . ?
C25 C24 C29 C30 -93.7(5) . . . . ?
C24 C29 C30 C31 -99.3(4) . . . . ?
C24 C29 C30 C35 80.8(5) . . . . ?
C35 C30 C31 C32 0.6(6) . . . . ?
C29 C30 C31 C32 -179.3(4) . . . . ?
C30 C31 C32 C33 0.5(6) . . . . ?
C30 C31 C32 C36 -180.0(4) . . . . ?
C31 C32 C33 C34 -1.2(6) . . . . ?
C36 C32 C33 C34 179.2(4) . . . . ?
C32 C33 C34 C35 0.8(6) . . . . ?
C32 C33 C34 C37 -178.4(4) . . . . ?
C31 C30 C35 O8 -178.4(3) . . . . ?
C29 C30 C35 O8 1.5(6) . . . . ?
C31 C30 C35 C34 -1.0(6) . . . . ?
C29 C30 C35 C34 178.9(3) . . . . ?
C33 C34 C35 O8 177.8(3) . . . . ?
C37 C34 C35 O8 -2.9(5) . . . . ?
C33 C34 C35 C30 0.3(6) . . . . ?
C37 C34 C35 C30 179.6(3) . . . . ?
C33 C32 C36 O9 2.8(6) . . . . ?
C31 C32 C36 O9 -176.7(4) . . . . ?
C33 C32 C36 O10 -180.0(4) . . . . ?
C31 C32 C36 O10 0.5(6) . . . . ?
C33 C34 C37 C2 91.5(4) . . . . ?
C35 C34 C37 C2 -87.7(5) . . . . ?
C3 C2 C37 C34 -72.1(5) . . . . ?
C1 C2 C37 C34 103.8(4) . . . . ?
O11 C38 C39 C40 6(2) . . . . ?
C38 C39 C40 C41 -8(3) . . . . ?
C39 C40 C41 O11 7(3) . . . . ?
O12 C42 C43 C44 -18.8(15) . . . . ?
C42 C43 C44 C45 23.8(14) . . . . ?
C43 C44 C45 O12 -21.2(13) . . . . ?
O13 C46 C47 C48 22(3) . . . . ?
C46 C47 C48 C49 -17(3) . . . . ?
C47 C48 C49 O13 4(3) . . . . ?
C6 C1 O1 C7 -109.8(4) . . . . ?
C2 C1 O1 C7 74.8(4) . . . . ?
C9 C7 O1 C1 70.6(5) . . . . ?
C8 C7 O1 C1 -165.2(4) . . . . ?
C24 C25 O7 C26 -109.1(4) . . . . ?
C20 C25 O7 C26 74.9(5) . . . . ?
C28 C26 O7 C25 78.3(6) . . . . ?
C27 C26 O7 C25 -157.7(5) . . . . ?
C39 C38 O11 C41 -2(2) . . . . ?
C40 C41 O11 C38 -3(2) . . . . ?
C44 C45 O12 C42 8.9(12) . . . . ?
C43 C42 O12 C45 6.5(14) . . . . ?
C48 C49 O13 C46 11(3) . . . . ?
C47 C46 O13 C49 -22(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.969
_diffrn_reflns_theta_full        24.40
_diffrn_measured_fraction_theta_full 0.969
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.083
####################################################################### 
# 
# 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_2.THF.MeOH
_database_code_depnum_ccdc_archive 'CCDC 1432495'
_audit_update_record             
;
2015-10-21 deposited with the CCDC.
2018-12-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(C37 H36 O10), 0.75(C4 H8 O), 2.25 (C H4 O)'
_chemical_formula_sum            'C42.25 H51 O13'
_chemical_formula_weight         766.83

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/n  '

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

_cell_length_a                   10.6209(14)
_cell_length_b                   17.125(2)
_cell_length_c                   22.296(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.218(2)
_cell_angle_gamma                90.00
_cell_volume                     4038.4(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4365
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      22.65
_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1634
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9744
_exptl_absorpt_correction_T_max  0.9807
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27522
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         25.10
_reflns_number_total             7071
_reflns_number_gt                5166
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1373P)²+6.5726P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7071
_refine_ls_number_parameters     543
_refine_ls_number_restraints     949
_refine_ls_R_factor_all          0.1129
_refine_ls_R_factor_gt           0.0869
_refine_ls_wR_factor_ref         0.2495
_refine_ls_wR_factor_gt          0.2315
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5802(3) 0.53128(19) 0.11975(15) 0.0237(7) Uani 1 1 d U A 1
C2 C 0.6163(3) 0.4900(2) 0.06958(15) 0.0245(7) Uani 1 1 d U A 1
C3 C 0.5696(3) 0.4145(2) 0.06058(15) 0.0264(7) Uani 1 1 d U A 1
H3 H 0.5918 0.3861 0.0276 0.032 Uiso 1 1 calc R A 1
C4 C 0.4899(3) 0.3802(2) 0.09995(17) 0.0305(8) Uani 1 1 d U A 1
C5 C 0.4633(3) 0.4217(2) 0.15088(16) 0.0299(8) Uani 1 1 d U A 1
H5 H 0.4145 0.3980 0.1783 0.036 Uiso 1 1 calc R A 1
C6 C 0.5067(3) 0.4966(2) 0.16211(15) 0.0267(7) Uani 1 1 d U A 1
C7 C 0.5671(3) 0.6694(2) 0.09386(16) 0.0300(8) Uani 1 1 d U A 1
H7 H 0.5704 0.6549 0.0506 0.036 Uiso 1 1 d R A 1
C8 C 0.6500(5) 0.7380(2) 0.1081(2) 0.0517(11) Uani 1 1 d U A 1
H8A H 0.6509 0.7501 0.1502 0.078 Uiso 1 1 calc R A 1
H8B H 0.6183 0.7820 0.0847 0.078 Uiso 1 1 calc R A 1
H8C H 0.7343 0.7262 0.0986 0.078 Uiso 1 1 calc R A 1
C9 C 0.4303(4) 0.6830(3) 0.1058(2) 0.0433(10) Uani 1 1 d U A 1
H9A H 0.3834 0.6353 0.0992 0.065 Uiso 1 1 calc R A 1
H9B H 0.3943 0.7227 0.0791 0.065 Uiso 1 1 calc R A 1
H9C H 0.4268 0.6995 0.1468 0.065 Uiso 1 1 calc R A 1
C10 C 0.4396(4) 0.3009(3) 0.0873(2) 0.0435(10) Uani 1 1 d U A 1
C11 C 0.4812(3) 0.5381(2) 0.21943(16) 0.0305(8) Uani 1 1 d U A 1
H11A H 0.3959 0.5262 0.2288 0.037 Uiso 1 1 calc R A 1
H11B H 0.4867 0.5940 0.2133 0.037 Uiso 1 1 calc R A 1
C12 C 0.5743(3) 0.5145(2) 0.27258(15) 0.0272(7) Uani 1 1 d U A 1
C13 C 0.5394(3) 0.4603(2) 0.31406(15) 0.0273(7) Uani 1 1 d U A 1
H13 H 0.4590 0.4383 0.3091 0.033 Uiso 1 1 calc R A 1
C14 C 0.6222(3) 0.4380(2) 0.36306(16) 0.0299(8) Uani 1 1 d U A 1
C15 C 0.7429(3) 0.4708(2) 0.37055(15) 0.0291(8) Uani 1 1 d U A 1
H15 H 0.7979 0.4561 0.4035 0.035 Uiso 1 1 calc R A 1
C16 C 0.7824(3) 0.5247(2) 0.32996(15) 0.0277(7) Uani 1 1 d U A 1
C17 C 0.6968(3) 0.5466(2) 0.28071(15) 0.0265(7) Uani 1 1 d U A 1
C18 C 0.5836(3) 0.3802(2) 0.40629(16) 0.0323(8) Uani 1 1 d U A 1
C19 C 0.9146(3) 0.5595(2) 0.33732(15) 0.0299(8) Uani 1 1 d U A 1
H19A H 0.9115 0.6127 0.3223 0.036 Uiso 1 1 calc R A 1
H19B H 0.9441 0.5611 0.3798 0.036 Uiso 1 1 calc R A 1
C20 C 1.0075(3) 0.5127(2) 0.30378(15) 0.0284(7) Uani 1 1 d U A 1
C21 C 1.0537(3) 0.4419(2) 0.32758(17) 0.0362(9) Uani 1 1 d U A 1
H21 H 1.0326 0.4265 0.3654 0.043 Uiso 1 1 calc R A 1
C22 C 1.1307(4) 0.3938(2) 0.29636(18) 0.0364(9) Uani 1 1 d U A 1
H22 H 1.1635 0.3479 0.3138 0.044 Uiso 1 1 calc R A 1
C23 C 1.1578(3) 0.4151(2) 0.23888(17) 0.0316(8) Uani 1 1 d U A 1
H23 H 1.2048 0.3815 0.2169 0.038 Uiso 1 1 calc R A 1
C24 C 1.1161(3) 0.4858(2) 0.21354(15) 0.0247(7) Uani 1 1 d U A 1
C25 C 1.0454(3) 0.53548(19) 0.24756(15) 0.0241(7) Uani 1 1 d U A 1
C26 C 1.0647(3) 0.6768(2) 0.24882(17) 0.0331(8) Uani 1 1 d U A 1
H26 H 1.0777 0.6705 0.2935 0.040 Uiso 1 1 d R A 1
C27 C 0.9695(4) 0.7410(2) 0.2340(2) 0.0474(10) Uani 1 1 d U A 1
H27A H 0.9501 0.7438 0.1911 0.071 Uiso 1 1 calc R A 1
H27B H 1.0042 0.7900 0.2485 0.071 Uiso 1 1 calc R A 1
H27C H 0.8937 0.7301 0.2529 0.071 Uiso 1 1 calc R A 1
C28 C 1.1894(4) 0.6921(3) 0.2247(2) 0.0489(11) Uani 1 1 d U A 1
H28A H 1.2444 0.6483 0.2333 0.073 Uiso 1 1 calc R A 1
H28B H 1.2269 0.7381 0.2433 0.073 Uiso 1 1 calc R A 1
H28C H 1.1768 0.6997 0.1819 0.073 Uiso 1 1 calc R A 1
C29 C 1.1416(3) 0.5064(2) 0.14943(15) 0.0250(7) Uani 1 1 d U A 1
H29A H 1.2247 0.4873 0.1420 0.030 Uiso 1 1 calc R A 1
H29B H 1.1422 0.5628 0.1452 0.030 Uiso 1 1 calc R A 1
C30 C 1.0439(3) 0.47216(19) 0.10242(14) 0.0222(7) Uani 1 1 d U A 1
C31 C 1.0688(3) 0.4036(2) 0.07333(14) 0.0250(7) Uani 1 1 d U A 1
H31 H 1.1447 0.3776 0.0835 0.030 Uiso 1 1 calc R A 1
C32 C 0.9818(3) 0.3725(2) 0.02876(15) 0.0270(7) Uani 1 1 d U A 1
C33 C 0.8685(3) 0.4115(2) 0.01386(14) 0.0246(7) Uani 1 1 d U A 1
H33 H 0.8111 0.3913 -0.0161 0.030 Uiso 1 1 calc R A 1
C34 C 0.8394(3) 0.47987(19) 0.04274(14) 0.0229(7) Uani 1 1 d U A 1
C35 C 0.9281(3) 0.51045(19) 0.08731(14) 0.0220(7) Uani 1 1 d U A 1
C36 C 1.0098(3) 0.3007(2) -0.00293(16) 0.0325(8) Uani 1 1 d U A 1
C37 C 0.7123(3) 0.5201(2) 0.02867(14) 0.0238(7) Uani 1 1 d U A 1
H37A H 0.7225 0.5760 0.0341 0.029 Uiso 1 1 calc R A 1
H37B H 0.6818 0.5105 -0.0130 0.029 Uiso 1 1 calc R A 1
C38 C 0.5404(9) 0.7457(5) 0.2959(5) 0.101(3) Uani 0.75 1 d PDU B 1
H38A H 0.4674 0.7773 0.2826 0.121 Uiso 0.75 1 calc PR B 1
H38B H 0.5669 0.7157 0.2623 0.121 Uiso 0.75 1 calc PR B 1
C39 C 0.5181(12) 0.6967(9) 0.3470(6) 0.150(4) Uani 0.75 1 d PDU B 1
H39A H 0.4420 0.7132 0.3644 0.180 Uiso 0.75 1 calc PR B 1
H39B H 0.5079 0.6426 0.3344 0.180 Uiso 0.75 1 calc PR B 1
C40 C 0.6262(10) 0.7046(8) 0.3904(6) 0.139(3) Uani 0.75 1 d PDU B 1
H40A H 0.6596 0.6528 0.3993 0.166 Uiso 0.75 1 calc PR B 1
H40B H 0.5968 0.7249 0.4273 0.166 Uiso 0.75 1 calc PR B 1
C41 C 0.7319(7) 0.7546(4) 0.3744(3) 0.073(2) Uani 0.75 1 d PDU B 1
H41A H 0.8003 0.7256 0.3588 0.087 Uiso 0.75 1 calc PR B 1
H41B H 0.7639 0.7894 0.4065 0.087 Uiso 0.75 1 calc PR B 1
C42 C 0.628(2) 0.8013(11) 0.2755(12) 0.025(5) Uani 0.125 1 d PDU C 2
H42A H 0.6752 0.7567 0.2908 0.038 Uiso 0.125 1 calc PR C 2
H42B H 0.6033 0.7940 0.2334 0.038 Uiso 0.125 1 calc PR C 2
H42C H 0.5539 0.8072 0.2967 0.038 Uiso 0.125 1 calc PR C 2
C42' C 0.710(2) 0.8207(12) 0.3379(8) 0.017(4) Uani 0.125 1 d PDU D 4
H42D H 0.7528 0.7727 0.3306 0.025 Uiso 0.125 1 calc PR D 4
H42E H 0.6256 0.8096 0.3476 0.025 Uiso 0.125 1 calc PR D 4
H42F H 0.7550 0.8477 0.3710 0.025 Uiso 0.125 1 calc PR D 4
C43 C 0.8266(11) 0.9055(8) 0.8760(7) 0.143(5) Uani 0.75 1 d PDU E 3
H43A H 0.8217 0.9566 0.8934 0.215 Uiso 0.75 1 d PR E 3
H43B H 0.8248 0.9101 0.8330 0.215 Uiso 0.75 1 d PR E 3
H43C H 0.9039 0.8808 0.8914 0.215 Uiso 0.75 1 d PR E 3
C44 C 0.6024(16) 0.9049(15) 0.9865(10) 0.223(8) Uani 0.75 1 d PDU F 1
H44A H 0.6039 0.9565 0.9698 0.335 Uiso 0.75 1 d PR F 1
H44B H 0.6107 0.8671 0.9553 0.335 Uiso 0.75 1 d PR F 1
H44C H 0.6711 0.8991 1.0172 0.335 Uiso 0.75 1 d PR F 1
C45 C 0.723(3) 1.0800(14) 0.9832(15) 0.221(11) Uani 0.50 1 d PDU G 2
H45A H 0.6850 1.1166 1.0089 0.332 Uiso 0.50 1 d PR G 2
H45B H 0.7335 1.1043 0.9452 0.332 Uiso 0.50 1 d PR G 2
H45C H 0.8034 1.0639 1.0019 0.332 Uiso 0.50 1 d PR G 2
O2 O 0.3558(3) 0.27779(19) 0.12343(15) 0.0557(8) Uani 1 1 d U . .
H2A H 0.3242 0.2365 0.1111 0.084 Uiso 1 1 calc R A 1
O3 O 0.4733(3) 0.26098(18) 0.04579(16) 0.0565(8) Uani 1 1 d U . .
O4 O 0.7394(2) 0.60045(16) 0.24377(11) 0.0345(6) Uani 1 1 d U . .
H4 H 0.6836 0.6110 0.2171 0.052 Uiso 1 1 calc R A 1
O5 O 0.4722(3) 0.34963(18) 0.39481(13) 0.0472(7) Uani 1 1 d U . .
H5A H 0.4592 0.3182 0.4213 0.071 Uiso 1 1 calc R A 1
O1 O 0.6232(2) 0.60601(13) 0.13172(10) 0.0253(5) Uani 1 1 d U . .
O6 O 0.6563(3) 0.36064(16) 0.45120(12) 0.0398(6) Uani 1 1 d U . .
O11 O 0.6470(11) 0.7937(7) 0.3267(5) 0.188(4) Uani 0.75 1 d PDU B 1
O12 O 0.7050(8) 0.8699(5) 0.2837(5) 0.033(2) Uani 0.125 1 d PDU C 2
H12A H 0.6514 0.9152 0.2813 0.040 Uiso 0.25 1 d PR C 2
O12' O 0.7050(8) 0.8699(5) 0.2837(5) 0.033(2) Uani 0.125 1 d PU D 4
O13 O 0.7232(7) 0.8652(4) 0.8932(3) 0.117(3) Uani 0.75 1 d PDU E 3
H13A H 0.7020 0.8783 0.9329 0.140 Uiso 0.75 1 d PR E 3
O14 O 0.4859(12) 0.8912(6) 1.0132(4) 0.158(3) Uani 0.75 1 d PDU F 1
H14A H 0.4402 0.8515 0.9898 0.190 Uiso 0.75 1 d PR F 1
O15 O 0.6682(15) 1.0031(9) 0.9739(6) 0.150(5) Uani 0.50 1 d PDU G 2
H15A H 0.6696 0.9808 0.9345 0.179 Uiso 0.50 1 d PR G 2
O7 O 1.0059 0.6061 0.2222 0.025 Uani 1 1 d U . .
O8 O 0.8962 0.5790 0.1116 0.027 Uani 1 1 d U . .
H8 H 0.9540 0.5938 0.1358 0.041 Uiso 1 1 calc R A 1
O9 O 0.9282(2) 0.27224(17) -0.04170(13) 0.0441(7) Uani 1 1 d U . .
O10 O 1.1186(3) 0.26895(17) 0.01065(13) 0.0441(7) Uani 1 1 d U . .
H10 H 1.1243 0.2291 -0.0093 0.066 Uiso 1 1 calc R A 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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.377(4) . ?
C1 C2 1.406(5) . ?
C1 C6 1.410(5) . ?
C2 C3 1.392(5) . ?
C2 C37 1.519(4) . ?
C3 C4 1.402(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.390(6) . ?
C4 C10 1.478(6) . ?
C5 C6 1.379(5) . ?
C5 H5 0.9300 . ?
C6 C11 1.508(5) . ?
C7 O1 1.467(4) . ?
C7 C8 1.485(6) . ?
C7 C9 1.519(5) . ?
C7 H7 1.0000 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 O3 1.229(6) . ?
C10 O2 1.314(5) . ?
C11 C12 1.527(5) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.385(5) . ?
C12 C17 1.409(5) . ?
C13 C14 1.392(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.396(5) . ?
C14 C18 1.466(5) . ?
C15 C16 1.384(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.411(5) . ?
C16 C19 1.520(5) . ?
C17 O4 1.342(4) . ?
C18 O6 1.253(4) . ?
C18 O5 1.298(5) . ?
C19 C20 1.519(5) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.394(5) . ?
C20 C25 1.406(5) . ?
C21 C22 1.392(6) . ?
C21 H21 0.9300 . ?
C22 C23 1.388(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.391(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.402(5) . ?
C24 C29 1.520(5) . ?
C25 O7 1.383(3) . ?
C26 O7 1.464(3) . ?
C26 C28 1.497(5) . ?
C26 C27 1.509(6) . ?
C26 H26 1.0000 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 C30 1.524(4) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C31 1.378(5) . ?
C30 C35 1.408(4) . ?
C31 C32 1.400(5) . ?
C31 H31 0.9300 . ?
C32 C33 1.390(5) . ?
C32 C36 1.462(5) . ?
C33 C34 1.384(5) . ?
C33 H33 0.9300 . ?
C34 C35 1.407(5) . ?
C34 C37 1.522(4) . ?
C35 O8 1.349(3) . ?
C36 O9 1.265(4) . ?
C36 O10 1.288(4) . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 C39 1.451(9) . ?
C38 O11 1.513(9) . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 C40 1.439(9) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 C41 1.481(9) . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C41 O11 1.488(8) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 O12 1.434(10) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C42' H42D 0.9600 . ?
C42' H42E 0.9600 . ?
C42' H42F 0.9600 . ?
C43 O13 1.381(8) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 O14 1.440(10) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 O15 1.446(10) . ?
C45 H45A 0.9601 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
O2 H2A 0.8200 . ?
O4 H4 0.8200 . ?
O5 H5A 0.8200 . ?
O12 H12A 0.9600 . ?
O13 H13A 0.9600 . ?
O14 H14A 0.9600 . ?
O15 H44A 1.0488 . ?
O15 H15A 0.9600 . ?
O8 H8 0.8200 . ?
O10 H10 0.8200 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 120.8(3) . . ?
O1 C1 C6 117.1(3) . . ?
C2 C1 C6 121.9(3) . . ?
C3 C2 C1 117.5(3) . . ?
C3 C2 C37 118.6(3) . . ?
C1 C2 C37 123.6(3) . . ?
C2 C3 C4 121.7(3) . . ?
C2 C3 H3 119.1 . . ?
C4 C3 H3 119.1 . . ?
C5 C4 C3 118.5(3) . . ?
C5 C4 C10 121.9(3) . . ?
C3 C4 C10 119.6(4) . . ?
C6 C5 C4 122.3(3) . . ?
C6 C5 H5 118.9 . . ?
C4 C5 H5 118.9 . . ?
C5 C6 C1 117.8(3) . . ?
C5 C6 C11 120.6(3) . . ?
C1 C6 C11 121.5(3) . . ?
O1 C7 C8 105.1(3) . . ?
O1 C7 C9 110.9(3) . . ?
C8 C7 C9 113.5(3) . . ?
O1 C7 H7 108.9 . . ?
C8 C7 H7 109.3 . . ?
C9 C7 H7 109.0 . . ?
O3 C10 O2 123.6(4) . . ?
O3 C10 C4 122.0(4) . . ?
O2 C10 C4 114.4(4) . . ?
C6 C11 C12 112.3(3) . . ?
C6 C11 H11A 109.1 . . ?
C12 C11 H11A 109.1 . . ?
C6 C11 H11B 109.1 . . ?
C12 C11 H11B 109.1 . . ?
H11A C11 H11B 107.9 . . ?
C13 C12 C17 118.4(3) . . ?
C13 C12 C11 120.2(3) . . ?
C17 C12 C11 121.4(3) . . ?
C12 C13 C14 121.3(3) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
C13 C14 C15 119.4(3) . . ?
C13 C14 C18 120.5(3) . . ?
C15 C14 C18 120.1(3) . . ?
C16 C15 C14 121.3(3) . . ?
C16 C15 H15 119.3 . . ?
C14 C15 H15 119.3 . . ?
C15 C16 C17 118.3(3) . . ?
C15 C16 C19 121.5(3) . . ?
C17 C16 C19 120.2(3) . . ?
O4 C17 C12 123.2(3) . . ?
O4 C17 C16 115.5(3) . . ?
C12 C17 C16 121.2(3) . . ?
O6 C18 O5 122.3(3) . . ?
O6 C18 C14 121.1(3) . . ?
O5 C18 C14 116.5(3) . . ?
C20 C19 C16 112.0(3) . . ?
C20 C19 H19A 109.2 . . ?
C16 C19 H19A 109.2 . . ?
C20 C19 H19B 109.2 . . ?
C16 C19 H19B 109.2 . . ?
H19A C19 H19B 107.9 . . ?
C21 C20 C25 117.4(3) . . ?
C21 C20 C19 119.5(3) . . ?
C25 C20 C19 123.0(3) . . ?
C22 C21 C20 121.8(3) . . ?
C22 C21 H21 119.1 . . ?
C20 C21 H21 119.1 . . ?
C23 C22 C21 119.1(3) . . ?
C23 C22 H22 120.5 . . ?
C21 C22 H22 120.5 . . ?
C22 C23 C24 121.3(3) . . ?
C22 C23 H23 119.4 . . ?
C24 C23 H23 119.4 . . ?
C23 C24 C25 118.3(3) . . ?
C23 C24 C29 120.4(3) . . ?
C25 C24 C29 121.2(3) . . ?
O7 C25 C24 117.8(3) . . ?
O7 C25 C20 120.4(3) . . ?
C24 C25 C20 121.7(3) . . ?
O7 C26 C28 110.9(3) . . ?
O7 C26 C27 105.2(3) . . ?
C28 C26 C27 113.0(4) . . ?
O7 C26 H26 109.3 . . ?
C28 C26 H26 109.3 . . ?
C27 C26 H26 109.1 . . ?
C24 C29 C30 112.9(3) . . ?
C24 C29 H29A 109.0 . . ?
C30 C29 H29A 109.0 . . ?
C24 C29 H29B 109.0 . . ?
C30 C29 H29B 109.0 . . ?
H29A C29 H29B 107.8 . . ?
C31 C30 C35 119.0(3) . . ?
C31 C30 C29 120.3(3) . . ?
C35 C30 C29 120.7(3) . . ?
C30 C31 C32 121.1(3) . . ?
C30 C31 H31 119.5 . . ?
C32 C31 H31 119.5 . . ?
C33 C32 C31 119.2(3) . . ?
C33 C32 C36 119.9(3) . . ?
C31 C32 C36 120.9(3) . . ?
C34 C33 C32 121.3(3) . . ?
C34 C33 H33 119.3 . . ?
C32 C33 H33 119.3 . . ?
C33 C34 C35 118.7(3) . . ?
C33 C34 C37 121.2(3) . . ?
C35 C34 C37 120.1(3) . . ?
O8 C35 C34 115.6(3) . . ?
O8 C35 C30 123.7(3) . . ?
C34 C35 C30 120.7(3) . . ?
O9 C36 O10 122.8(3) . . ?
O9 C36 C32 119.8(3) . . ?
O10 C36 C32 117.3(3) . . ?
C2 C37 C34 110.7(3) . . ?
C2 C37 H37A 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C2 C37 H37B 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 108.1 . . ?
C39 C38 O11 97.3(10) . . ?
C39 C38 H38A 112.3 . . ?
O11 C38 H38A 112.3 . . ?
C39 C38 H38B 112.3 . . ?
O11 C38 H38B 112.3 . . ?
H38A C38 H38B 109.9 . . ?
C40 C39 C38 107.2(11) . . ?
C40 C39 H39A 110.3 . . ?
C38 C39 H39A 110.3 . . ?
C40 C39 H39B 110.3 . . ?
C38 C39 H39B 110.3 . . ?
H39A C39 H39B 108.5 . . ?
C39 C40 C41 117.9(11) . . ?
C39 C40 H40A 107.8 . . ?
C41 C40 H40A 107.8 . . ?
C39 C40 H40B 107.8 . . ?
C41 C40 H40B 107.8 . . ?
H40A C40 H40B 107.2 . . ?
C40 C41 O11 90.5(8) . . ?
C40 C41 H41A 113.5 . . ?
O11 C41 H41A 113.5 . . ?
C40 C41 H41B 113.5 . . ?
O11 C41 H41B 113.5 . . ?
H41A C41 H41B 110.8 . . ?
O12 C42 H42A 109.5 . . ?
O12 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
O12 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O13 C43 H43A 105.6 . . ?
O13 C43 H43B 111.9 . . ?
H43A C43 H43B 109.5 . . ?
O13 C43 H43C 110.8 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O14 C44 H44A 110.8 . . ?
O14 C44 H44B 109.3 . . ?
H44A C44 H44B 109.5 . . ?
O14 C44 H44C 108.3 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O15 C45 H45A 119.8 . . ?
O15 C45 H45B 110.3 . . ?
H45A C45 H45B 109.5 . . ?
O15 C45 H45C 97.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C17 O4 H4 109.5 . . ?
C18 O5 H5A 109.5 . . ?
C1 O1 C7 117.7(2) . . ?
C41 O11 C38 117.3(9) . . ?
C42 O12 H12A 109.1 . . ?
C43 O13 H13A 113.5 . . ?
C44 O14 H14A 107.5 . . ?
C45 O15 H44A 162.6 . . ?
C45 O15 H15A 117.0 . . ?
H44A O15 H15A 71.4 . . ?
C25 O7 C26 117.1(2) . . ?
C35 O8 H8 109.5 . . ?
C36 O10 H10 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 C3 179.7(3) . . . . ?
C6 C1 C2 C3 4.3(4) . . . . ?
O1 C1 C2 C37 5.7(5) . . . . ?
C6 C1 C2 C37 -169.6(3) . . . . ?
C1 C2 C3 C4 -0.3(5) . . . . ?
C37 C2 C3 C4 174.0(3) . . . . ?
C2 C3 C4 C5 -3.5(5) . . . . ?
C2 C3 C4 C10 178.0(3) . . . . ?
C3 C4 C5 C6 3.6(5) . . . . ?
C10 C4 C5 C6 -178.0(3) . . . . ?
C4 C5 C6 C1 0.2(5) . . . . ?
C4 C5 C6 C11 -176.9(3) . . . . ?
O1 C1 C6 C5 -179.8(3) . . . . ?
C2 C1 C6 C5 -4.3(5) . . . . ?
O1 C1 C6 C11 -2.7(4) . . . . ?
C2 C1 C6 C11 172.8(3) . . . . ?
C5 C4 C10 O3 -172.3(4) . . . . ?
C3 C4 C10 O3 6.0(5) . . . . ?
C5 C4 C10 O2 8.4(5) . . . . ?
C3 C4 C10 O2 -173.2(3) . . . . ?
C5 C6 C11 C12 81.6(4) . . . . ?
C1 C6 C11 C12 -95.4(4) . . . . ?
C6 C11 C12 C13 -100.0(4) . . . . ?
C6 C11 C12 C17 79.8(4) . . . . ?
C17 C12 C13 C14 0.5(5) . . . . ?
C11 C12 C13 C14 -179.7(3) . . . . ?
C12 C13 C14 C15 -0.1(5) . . . . ?
C12 C13 C14 C18 -179.7(3) . . . . ?
C13 C14 C15 C16 -0.5(5) . . . . ?
C18 C14 C15 C16 179.1(3) . . . . ?
C14 C15 C16 C17 0.6(5) . . . . ?
C14 C15 C16 C19 -178.9(3) . . . . ?
C13 C12 C17 O4 -178.9(3) . . . . ?
C11 C12 C17 O4 1.3(5) . . . . ?
C13 C12 C17 C16 -0.3(5) . . . . ?
C11 C12 C17 C16 179.9(3) . . . . ?
C15 C16 C17 O4 178.4(3) . . . . ?
C19 C16 C17 O4 -2.0(5) . . . . ?
C15 C16 C17 C12 -0.3(5) . . . . ?
C19 C16 C17 C12 179.3(3) . . . . ?
C13 C14 C18 O6 -178.7(3) . . . . ?
C15 C14 C18 O6 1.8(5) . . . . ?
C13 C14 C18 O5 2.6(5) . . . . ?
C15 C14 C18 O5 -176.9(3) . . . . ?
C15 C16 C19 C20 91.7(4) . . . . ?
C17 C16 C19 C20 -87.9(4) . . . . ?
C16 C19 C20 C21 -76.1(4) . . . . ?
C16 C19 C20 C25 100.8(4) . . . . ?
C25 C20 C21 C22 -2.4(5) . . . . ?
C19 C20 C21 C22 174.7(3) . . . . ?
C20 C21 C22 C23 -2.8(6) . . . . ?
C21 C22 C23 C24 4.0(6) . . . . ?
C22 C23 C24 C25 0.0(5) . . . . ?
C22 C23 C24 C29 -177.1(3) . . . . ?
C23 C24 C25 O7 179.2(3) . . . . ?
C29 C24 C25 O7 -3.8(4) . . . . ?
C23 C24 C25 C20 -5.4(5) . . . . ?
C29 C24 C25 C20 171.7(3) . . . . ?
C21 C20 C25 O7 -178.1(3) . . . . ?
C19 C20 C25 O7 4.9(5) . . . . ?
C21 C20 C25 C24 6.5(5) . . . . ?
C19 C20 C25 C24 -170.4(3) . . . . ?
C23 C24 C29 C30 84.1(4) . . . . ?
C25 C24 C29 C30 -92.9(4) . . . . ?
C24 C29 C30 C31 -97.7(4) . . . . ?
C24 C29 C30 C35 83.3(4) . . . . ?
C35 C30 C31 C32 0.9(5) . . . . ?
C29 C30 C31 C32 -178.1(3) . . . . ?
C30 C31 C32 C33 -0.1(5) . . . . ?
C30 C31 C32 C36 178.6(3) . . . . ?
C31 C32 C33 C34 -0.9(5) . . . . ?
C36 C32 C33 C34 -179.6(3) . . . . ?
C32 C33 C34 C35 1.0(5) . . . . ?
C32 C33 C34 C37 -176.7(3) . . . . ?
C33 C34 C35 O8 177.1(3) . . . . ?
C37 C34 C35 O8 -5.2(4) . . . . ?
C33 C34 C35 C30 -0.2(5) . . . . ?
C37 C34 C35 C30 177.5(3) . . . . ?
C31 C30 C35 O8 -177.8(3) . . . . ?
C29 C30 C35 O8 1.2(5) . . . . ?
C31 C30 C35 C34 -0.7(5) . . . . ?
C29 C30 C35 C34 178.3(3) . . . . ?
C33 C32 C36 O9 -3.5(5) . . . . ?
C31 C32 C36 O9 177.8(3) . . . . ?
C33 C32 C36 O10 176.8(3) . . . . ?
C31 C32 C36 O10 -1.9(5) . . . . ?
C3 C2 C37 C34 -71.4(4) . . . . ?
C1 C2 C37 C34 102.5(4) . . . . ?
C33 C34 C37 C2 90.0(4) . . . . ?
C35 C34 C37 C2 -87.7(4) . . . . ?
O11 C38 C39 C40 -15.6(14) . . . . ?
C38 C39 C40 C41 -2.3(17) . . . . ?
C39 C40 C41 O11 18.9(13) . . . . ?
C2 C1 O1 C7 74.9(4) . . . . ?
C6 C1 O1 C7 -109.6(3) . . . . ?
C8 C7 O1 C1 -167.9(3) . . . . ?
C9 C7 O1 C1 69.1(4) . . . . ?
C40 C41 O11 C38 -31.0(12) . . . . ?
C39 C38 O11 C41 32.0(14) . . . . ?
C24 C25 O7 C26 -110.8(3) . . . . ?
C20 C25 O7 C26 73.7(3) . . . . ?
C28 C26 O7 C25 82.5(4) . . . . ?
C27 C26 O7 C25 -155.0(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.785
_refine_diff_density_rms         0.085
####################################################################### 
# 
# 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_7.Py
_database_code_depnum_ccdc_archive 'CCDC 1432500'
_audit_update_record             
;
2015-10-21 deposited with the CCDC.
2018-12-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H48 O12.4(C5 H5 N)'
_chemical_formula_sum            'C64 H68 N4 O12'
_chemical_formula_weight         1085.22

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'


loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+1/4, x+3/4, z+3/4'
'y+1/4, -x+1/4, z+1/4'
'-x, -y+1/2, z'
'x+1/2, y+1/2, z+1/2'
'-y+3/4, x+5/4, z+5/4'
'y+3/4, -x+3/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'-x, -y, -z'
'y-1/4, -x-3/4, -z-3/4'
'-y-1/4, x-1/4, -z-1/4'
'x, y-1/2, -z'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/4, -x-1/4, -z-1/4'
'-y+1/4, x+1/4, -z+1/4'
'x+1/2, y, -z+1/2'

_cell_length_a                   18.745(7)
_cell_length_b                   18.745(7)
_cell_length_c                   16.688(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5864(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6070
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      30.74

_exptl_crystal_description       colorless
_exptl_crystal_colour            plate
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2304
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.9899
_exptl_absorpt_correction_T_max  0.9915
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18832
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.63
_diffrn_reflns_theta_max         25.99
_reflns_number_total             2872
_reflns_number_gt                2213
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0799P)²+1.3963P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0010(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2872
_refine_ls_number_parameters     187
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0468
_refine_ls_wR_factor_ref         0.1486
_refine_ls_wR_factor_gt          0.1394
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.107
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.39767(8) 0.82146(8) 0.29398(9) 0.0402(4) Uani 1 1 d . . .
C2 C 0.43733(8) 0.87403(8) 0.25638(8) 0.0405(4) Uani 1 1 d . . .
H2 H 0.4688 0.9028 0.2872 0.049 Uiso 1 1 calc R . .
C3 C 0.43198(8) 0.88550(8) 0.17451(8) 0.0374(4) Uani 1 1 d . . .
C4 C 0.38437(8) 0.84323(8) 0.13109(8) 0.0366(4) Uani 1 1 d . . .
C5 C 0.34861(8) 0.78577(8) 0.16635(8) 0.0378(4) Uani 1 1 d . . .
C6 C 0.35492(8) 0.77676(8) 0.24847(9) 0.0392(4) Uani 1 1 d . . .
H6 H 0.3295 0.7393 0.2740 0.047 Uiso 1 1 calc R . .
C7 C 0.31080(8) 0.72987(8) 0.11674(9) 0.0416(4) Uani 1 1 d . . .
H7A H 0.2805 0.7535 0.0761 0.050 Uiso 1 1 calc R . .
H7B H 0.2796 0.7008 0.1518 0.050 Uiso 1 1 calc R . .
C8 C 0.39901(10) 0.81114(9) 0.38211(10) 0.0482(4) Uani 1 1 d . . .
C9 C 0.31121(10) 0.88984(10) 0.02503(10) 0.0548(5) Uani 1 1 d . . .
H9 H 0.2700 0.8629 0.0482 0.066 Uiso 1 1 calc R . .
C10 C 0.30701(13) 0.96598(13) 0.05141(15) 0.0769(6) Uani 1 1 d . . .
H10A H 0.3132 0.9686 0.1097 0.115 Uiso 1 1 calc R . .
H10B H 0.2604 0.9857 0.0368 0.115 Uiso 1 1 calc R . .
H10C H 0.3447 0.9936 0.0251 0.115 Uiso 1 1 calc R . .
C11 C 0.31028(14) 0.88216(15) -0.06507(13) 0.0873(8) Uani 1 1 d . . .
H11A H 0.3532 0.9041 -0.0877 0.131 Uiso 1 1 calc R . .
H11B H 0.2679 0.9059 -0.0867 0.131 Uiso 1 1 calc R . .
H11C H 0.3091 0.8314 -0.0793 0.131 Uiso 1 1 calc R . .
C12 C 0.82025(13) 0.86330(13) 0.92651(13) 0.0768(7) Uani 1 1 d . . .
H12 H 0.7976 0.8668 0.9773 0.092 Uiso 1 1 calc R . .
C13 C 0.77881(13) 0.85549(16) 0.86097(15) 0.0934(8) Uani 1 1 d . . .
H13 H 0.7283 0.8541 0.8660 0.112 Uiso 1 1 calc R . .
C14 C 0.80966(14) 0.84965(15) 0.78823(14) 0.0869(7) Uani 1 1 d . . .
H14 H 0.7814 0.8427 0.7416 0.104 Uiso 1 1 calc R . .
C15 C 0.88099(14) 0.85390(14) 0.78296(12) 0.0814(7) Uani 1 1 d . . .
H15 H 0.9043 0.8510 0.7325 0.098 Uiso 1 1 calc R . .
C16 C 0.91922(12) 0.86256(13) 0.85227(13) 0.0751(6) Uani 1 1 d . . .
H16 H 0.9697 0.8661 0.8486 0.090 Uiso 1 1 calc R . .
N1 N 0.88953(10) 0.86625(10) 0.92403(9) 0.0684(5) Uani 1 1 d . . .
O1 O 0.43743(9) 0.85928(8) 0.42101(7) 0.0721(5) Uani 1 1 d D . .
H1 H 0.4290(15) 0.8565(15) 0.4718(10) 0.108 Uiso 1 1 d D . .
O2 O 0.36579(8) 0.76461(7) 0.41613(7) 0.0659(4) Uani 1 1 d . . .
O3 O 0.37736(6) 0.85590(6) 0.05003(6) 0.0430(3) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.385(2) . ?
C1 C6 1.386(2) . ?
C1 C8 1.484(2) . ?
C2 C3 1.387(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.396(2) . ?
C3 C7 1.514(2) 10_576 ?
C4 O3 1.3796(17) . ?
C4 C5 1.398(2) . ?
C5 C6 1.386(2) . ?
C5 C7 1.512(2) . ?
C6 H6 0.9500 . ?
C7 C3 1.514(2) 15_655 ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 O2 1.213(2) . ?
C8 O1 1.325(2) . ?
C9 O3 1.455(2) . ?
C9 C10 1.496(3) . ?
C9 C11 1.511(3) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 N1 1.300(3) . ?
C12 C13 1.349(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.349(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.342(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.370(3) . ?
C15 H15 0.9500 . ?
C16 N1 1.322(3) . ?
C16 H16 0.9500 . ?
O1 H1 0.864(17) . ?

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
C2 C1 C6 119.50(14) . . ?
C2 C1 C8 122.20(14) . . ?
C6 C1 C8 118.30(14) . . ?
C1 C2 C3 121.19(14) . . ?
C1 C2 H2 119.4 . . ?
C3 C2 H2 119.4 . . ?
C2 C3 C4 118.00(13) . . ?
C2 C3 C7 120.54(13) . 10_576 ?
C4 C3 C7 121.35(13) . 10_576 ?
O3 C4 C3 118.16(13) . . ?
O3 C4 C5 119.96(13) . . ?
C3 C4 C5 121.68(13) . . ?
C6 C5 C4 117.97(14) . . ?
C6 C5 C7 119.80(14) . . ?
C4 C5 C7 121.88(13) . . ?
C5 C6 C1 121.17(14) . . ?
C5 C6 H6 119.4 . . ?
C1 C6 H6 119.4 . . ?
C5 C7 C3 110.38(12) . 15_655 ?
C5 C7 H7A 109.6 . . ?
C3 C7 H7A 109.6 15_655 . ?
C5 C7 H7B 109.6 . . ?
C3 C7 H7B 109.6 15_655 . ?
H7A C7 H7B 108.1 . . ?
O2 C8 O1 122.66(15) . . ?
O2 C8 C1 123.31(15) . . ?
O1 C8 C1 113.96(14) . . ?
O3 C9 C10 112.20(16) . . ?
O3 C9 C11 104.69(15) . . ?
C10 C9 C11 112.54(17) . . ?
O3 C9 H9 109.1 . . ?
C10 C9 H9 109.1 . . ?
C11 C9 H9 109.1 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N1 C12 C13 123.6(2) . . ?
N1 C12 H12 118.2 . . ?
C13 C12 H12 118.2 . . ?
C14 C13 C12 119.4(2) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C15 C14 C13 118.8(2) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
C14 C15 C16 118.2(2) . . ?
C14 C15 H15 120.9 . . ?
C16 C15 H15 120.9 . . ?
N1 C16 C15 123.4(2) . . ?
N1 C16 H16 118.3 . . ?
C15 C16 H16 118.3 . . ?
C12 N1 C16 116.55(18) . . ?
C8 O1 H1 109.9(19) . . ?
C4 O3 C9 115.96(11) . . ?

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
C6 C1 C2 C3 3.8(2) . . . . ?
C8 C1 C2 C3 -176.07(14) . . . . ?
C1 C2 C3 C4 1.1(2) . . . . ?
C1 C2 C3 C7 -175.19(13) . . . 10_576 ?
C2 C3 C4 O3 178.12(12) . . . . ?
C7 C3 C4 O3 -5.6(2) 10_576 . . . ?
C2 C3 C4 C5 -6.9(2) . . . . ?
C7 C3 C4 C5 169.33(13) 10_576 . . . ?
O3 C4 C5 C6 -177.47(12) . . . . ?
C3 C4 C5 C6 7.7(2) . . . . ?
O3 C4 C5 C7 9.3(2) . . . . ?
C3 C4 C5 C7 -165.57(13) . . . . ?
C4 C5 C6 C1 -2.6(2) . . . . ?
C7 C5 C6 C1 170.77(13) . . . . ?
C2 C1 C6 C5 -3.0(2) . . . . ?
C8 C1 C6 C5 176.86(14) . . . . ?
C6 C5 C7 C3 -100.45(16) . . . 15_655 ?
C4 C5 C7 C3 72.66(18) . . . 15_655 ?
C2 C1 C8 O2 -178.54(17) . . . . ?
C6 C1 C8 O2 1.6(3) . . . . ?
C2 C1 C8 O1 4.2(2) . . . . ?
C6 C1 C8 O1 -175.62(15) . . . . ?
N1 C12 C13 C14 0.6(4) . . . . ?
C12 C13 C14 C15 -1.9(4) . . . . ?
C13 C14 C15 C16 1.3(4) . . . . ?
C14 C15 C16 N1 0.7(4) . . . . ?
C13 C12 N1 C16 1.3(4) . . . . ?
C15 C16 N1 C12 -1.9(4) . . . . ?
C3 C4 O3 C9 -107.53(16) . . . . ?
C5 C4 O3 C9 77.42(17) . . . . ?
C10 C9 O3 C4 70.00(19) . . . . ?
C11 C9 O3 C4 -167.65(16) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 N1 0.864(17) 1.898(18) 2.740(2) 165(3) 16_456

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.183
_refine_diff_density_min         -0.191
_refine_diff_density_rms         0.037
####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1432498'
_audit_update_record             
;
2015-10-21 deposited with the CCDC.
2018-12-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H48 O12'
_chemical_formula_sum            'C44 H48 O12'
_chemical_formula_weight         768.82

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   'P -4'
_symmetry_space_group_name_Hall  'P -4'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'y, -x, -z'
'-y, x, -z'
'-x, -y, z'

_cell_length_a                   17.9565(16)
_cell_length_b                   17.9565(16)
_cell_length_c                   12.1543(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3919.0(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4870
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      23.57

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1632
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  0.9813
_exptl_absorpt_correction_T_max  0.9906
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23011
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_sigmaI/netI    0.0456
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.13
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6901
_reflns_number_gt                5381
_reflns_threshold_expression     >2sigma(I)

_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          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0505P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.4(13)
_refine_ls_number_reflns         6901
_refine_ls_number_parameters     522
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_ref         0.0958
_refine_ls_wR_factor_gt          0.0880
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.001
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0316(2) 0.1528(2) 0.9335(3) 0.0315(10) Uani 1 1 d . . .
C2 C 0.0249(2) 0.1379(2) 0.8211(3) 0.0347(10) Uani 1 1 d . . .
H2 H -0.0152 0.1589 0.7807 0.042 Uiso 1 1 calc R . .
C3 C 0.0760(2) 0.0932(2) 0.7683(3) 0.0357(10) Uani 1 1 d . . .
C4 C 0.1336(2) 0.0606(2) 0.8261(4) 0.0370(11) Uani 1 1 d . . .
H4A H 0.1680 0.0294 0.7887 0.044 Uiso 1 1 calc R . .
C5 C 0.1418(2) 0.0728(2) 0.9374(4) 0.0344(10) Uani 1 1 d . . .
C6 C 0.0930(2) 0.1225(2) 0.9881(3) 0.0322(10) Uani 1 1 d . . .
C7 C 0.0662(2) 0.0774(3) 0.6475(3) 0.0394(10) Uani 1 1 d . . .
C8 C -0.0274(2) 0.1977(2) 0.9960(3) 0.0381(10) Uani 1 1 d . . .
H8A H -0.0034 0.2343 1.0454 0.046 Uiso 1 1 calc R . .
H8B H -0.0599 0.2248 0.9438 0.046 Uiso 1 1 calc R . .
C9 C 0.1491(3) 0.2009(2) 1.1201(3) 0.0487(12) Uani 1 1 d . . .
H9A H 0.1363 0.2417 1.0687 0.058 Uiso 1 1 calc R . .
H9B H 0.2018 0.1869 1.1079 0.058 Uiso 1 1 calc R . .
C10 C 0.1386(3) 0.2260(2) 1.2352(4) 0.0562(13) Uani 1 1 d . . .
H10A H 0.0857 0.2402 1.2453 0.067 Uiso 1 1 calc R . .
H10B H 0.1690 0.2712 1.2471 0.067 Uiso 1 1 calc R . .
C11 C 0.1588(4) 0.1692(3) 1.3225(4) 0.0784(17) Uani 1 1 d . . .
H11A H 0.1241 0.1271 1.3188 0.118 Uiso 1 1 calc R . .
H11B H 0.1558 0.1924 1.3954 0.118 Uiso 1 1 calc R . .
H11C H 0.2097 0.1514 1.3098 0.118 Uiso 1 1 calc R . .
C12 C 0.8571(2) 0.5670(2) 0.4789(3) 0.0345(9) Uani 1 1 d . . .
C13 C 0.8671(2) 0.5535(3) 0.3674(3) 0.0396(11) Uani 1 1 d . . .
H13 H 0.8354 0.5192 0.3307 0.048 Uiso 1 1 calc R . .
C14 C 0.9231(2) 0.5899(2) 0.3088(3) 0.0357(9) Uani 1 1 d . . .
C15 C 0.9705(3) 0.6387(2) 0.3627(3) 0.0371(10) Uani 1 1 d . . .
H15 H 1.0092 0.6623 0.3224 0.045 Uiso 1 1 calc R . .
C16 C 0.9629(2) 0.6538(2) 0.4725(3) 0.0353(10) Uani 1 1 d . . .
C17 C 0.9035(2) 0.6190(2) 0.5289(3) 0.0367(11) Uani 1 1 d . . .
C18 C 0.8035(2) 0.5197(2) 0.5459(3) 0.0375(9) Uani 1 1 d . . .
H18A H 0.7665 0.4961 0.4967 0.045 Uiso 1 1 calc R . .
H18B H 0.7765 0.5515 0.5992 0.045 Uiso 1 1 calc R . .
C19 C 0.8474(2) 0.4600(2) 0.6070(3) 0.0352(10) Uani 1 1 d . . .
C20 C 0.8812(2) 0.4009(2) 0.5515(3) 0.0339(9) Uani 1 1 d . . .
C21 C 0.9317(2) 0.3530(2) 0.6016(4) 0.0358(10) Uani 1 1 d . . .
C22 C 0.9451(2) 0.3632(2) 0.7155(3) 0.0370(10) Uani 1 1 d . . .
H22 H 0.9786 0.3310 0.7528 0.044 Uiso 1 1 calc R . .
C23 C 0.9099(2) 0.4194(2) 0.7727(3) 0.0360(10) Uani 1 1 d . . .
C24 C 0.8629(2) 0.4683(2) 0.7196(3) 0.0384(10) Uani 1 1 d . . .
H24 H 0.8407 0.5080 0.7596 0.046 Uiso 1 1 calc R . .
C25 C 0.9785(2) 0.3014(2) 0.5349(3) 0.0402(10) Uani 1 1 d . . .
H25A H 0.9468 0.2738 0.4821 0.048 Uiso 1 1 calc R . .
H25B H 1.0032 0.2647 0.5836 0.048 Uiso 1 1 calc R . .
C26 C 0.9342(3) 0.5759(3) 0.1910(3) 0.0424(10) Uani 1 1 d . . .
C27 C 0.8454(3) 0.6989(3) 0.6582(3) 0.0549(14) Uani 1 1 d . . .
H27A H 0.7941 0.6876 0.6333 0.066 Uiso 1 1 calc R . .
H27B H 0.8640 0.7420 0.6156 0.066 Uiso 1 1 calc R . .
C28 C 0.8452(3) 0.7168(3) 0.7768(4) 0.0686(15) Uani 1 1 d . . .
H28A H 0.8969 0.7286 0.7991 0.082 Uiso 1 1 calc R . .
H28B H 0.8152 0.7625 0.7876 0.082 Uiso 1 1 calc R . .
C29 C 0.8170(4) 0.6601(4) 0.8502(4) 0.107(2) Uani 1 1 d . . .
H29A H 0.7649 0.6496 0.8322 0.161 Uiso 1 1 calc R . .
H29B H 0.8204 0.6778 0.9264 0.161 Uiso 1 1 calc R . .
H29C H 0.8466 0.6146 0.8419 0.161 Uiso 1 1 calc R . .
C30 C 0.9244(2) 0.4314(3) 0.8909(3) 0.0430(10) Uani 1 1 d . . .
C31 C 0.8044(2) 0.3429(3) 0.4187(3) 0.0560(12) Uani 1 1 d . . .
H31A H 0.7631 0.3533 0.4703 0.067 Uiso 1 1 calc R . .
H31B H 0.8202 0.2905 0.4287 0.067 Uiso 1 1 calc R . .
C32 C 0.7790(3) 0.3551(3) 0.3025(3) 0.0634(14) Uani 1 1 d . . .
H32A H 0.7347 0.3236 0.2893 0.076 Uiso 1 1 calc R . .
H32B H 0.7633 0.4077 0.2949 0.076 Uiso 1 1 calc R . .
C33 C 0.8343(4) 0.3390(4) 0.2160(3) 0.0828(17) Uani 1 1 d . . .
H33A H 0.8764 0.3733 0.2231 0.124 Uiso 1 1 calc R . .
H33B H 0.8111 0.3453 0.1435 0.124 Uiso 1 1 calc R . .
H33C H 0.8519 0.2876 0.2238 0.124 Uiso 1 1 calc R . .
C34 C 0.3495(2) 0.5473(2) 0.0668(3) 0.0247(9) Uani 1 1 d . . .
C35 C 0.3632(2) 0.5378(2) 0.1775(3) 0.0256(9) Uani 1 1 d . . .
H35 H 0.3377 0.4999 0.2169 0.031 Uiso 1 1 calc R . .
C36 C 0.4139(2) 0.5830(2) 0.2319(3) 0.0278(9) Uani 1 1 d . . .
C37 C 0.4538(2) 0.6372(2) 0.1737(3) 0.0272(9) Uani 1 1 d . . .
H37 H 0.4897 0.6670 0.2107 0.033 Uiso 1 1 calc R . .
C38 C 0.4412(2) 0.6475(2) 0.0623(3) 0.0253(9) Uani 1 1 d . . .
C39 C 0.3864(2) 0.6041(2) 0.0114(3) 0.0253(8) Uani 1 1 d . . .
C40 C 0.3010(2) 0.4918(2) 0.0045(3) 0.0269(8) Uani 1 1 d . . .
H40A H 0.2664 0.5186 -0.0451 0.032 Uiso 1 1 calc R . .
H40B H 0.2712 0.4619 0.0569 0.032 Uiso 1 1 calc R . .
C41 C 0.4292(2) 0.5709(2) 0.3494(3) 0.0317(10) Uani 1 1 d . . .
C42 C 0.3095(2) 0.6637(3) -0.1199(3) 0.0435(11) Uani 1 1 d . . .
H42A H 0.3232 0.7156 -0.1013 0.052 Uiso 1 1 calc R . .
H42B H 0.2671 0.6489 -0.0729 0.052 Uiso 1 1 calc R . .
C43 C 0.2875(3) 0.6591(3) -0.2382(3) 0.0502(12) Uani 1 1 d . . .
H43A H 0.2437 0.6916 -0.2503 0.060 Uiso 1 1 calc R . .
H43B H 0.2722 0.6074 -0.2548 0.060 Uiso 1 1 calc R . .
C44 C 0.3484(3) 0.6816(3) -0.3178(3) 0.0667(17) Uani 1 1 d . . .
H44A H 0.3722 0.7275 -0.2919 0.100 Uiso 1 1 calc R . .
H44B H 0.3267 0.6901 -0.3908 0.100 Uiso 1 1 calc R . .
H44C H 0.3856 0.6418 -0.3223 0.100 Uiso 1 1 calc R . .
O1 O 0.11767(19) 0.03580(19) 0.6041(3) 0.0596(9) Uani 1 1 d . . .
O2 O 0.0130(2) 0.1024(2) 0.5974(3) 0.0608(10) Uani 1 1 d D . .
H2A H 0.001(3) 0.103(3) 0.524(2) 0.091 Uiso 1 1 d D . .
O3 O 0.10121(16) 0.13703(14) 1.1001(2) 0.0385(7) Uani 1 1 d . . .
O4 O 0.8842(2) 0.5310(2) 0.1461(2) 0.0634(10) Uani 1 1 d D . .
H4 H 0.886(3) 0.516(3) 0.080(2) 0.095 Uiso 1 1 d D . .
O5 O 0.9848(2) 0.6033(2) 0.1387(2) 0.0675(10) Uani 1 1 d . . .
O6 O 0.89321(14) 0.63459(15) 0.6397(2) 0.0416(7) Uani 1 1 d . . .
O7 O 0.9710(2) 0.3832(2) 0.9338(2) 0.0623(10) Uani 1 1 d D . .
H7 H 0.981(3) 0.400(3) 0.994(2) 0.093 Uiso 1 1 d D . .
O8 O 0.8979(2) 0.48265(19) 0.9428(3) 0.0655(10) Uani 1 1 d . . .
O9 O 0.86606(15) 0.39237(15) 0.44067(19) 0.0384(7) Uani 1 1 d . . .
O10 O 0.48082(19) 0.6114(2) 0.3925(2) 0.0572(10) Uani 1 1 d D . .
H10 H 0.491(3) 0.609(3) 0.4615(19) 0.086 Uiso 1 1 d D . .
O11 O 0.3921(2) 0.52516(17) 0.4030(2) 0.0563(9) Uani 1 1 d . . .
O12 O 0.37182(13) 0.61529(14) -0.09983(17) 0.0291(6) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.396(6) . ?
C1 C2 1.398(5) . ?
C1 C8 1.533(5) . ?
C2 C3 1.377(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.380(6) . ?
C3 C7 1.505(6) . ?
C4 C5 1.378(6) . ?
C4 H4A 0.9500 . ?
C5 C6 1.394(6) . ?
C5 C8 1.526(6) 2_557 ?
C6 O3 1.394(5) . ?
C7 O2 1.218(5) . ?
C7 O1 1.301(6) . ?
C8 C5 1.526(6) 3_557 ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 O3 1.453(5) . ?
C9 C10 1.482(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.516(7) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.387(6) . ?
C12 C17 1.393(6) . ?
C12 C18 1.520(5) . ?
C13 C14 1.395(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.386(6) . ?
C14 C26 1.467(5) . ?
C15 C16 1.368(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.413(6) . ?
C16 C25 1.527(6) 4_765 ?
C17 O6 1.387(4) . ?
C18 C19 1.524(6) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.396(6) . ?
C19 C24 1.405(6) . ?
C20 O9 1.382(4) . ?
C20 C21 1.391(6) . ?
C21 C22 1.416(6) . ?
C21 C25 1.491(6) . ?
C22 C23 1.379(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.378(6) . ?
C23 C30 1.476(5) . ?
C24 H24 0.9500 . ?
C25 C16 1.527(6) 4_765 ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 O5 1.213(5) . ?
C26 O4 1.325(6) . ?
C27 O6 1.456(5) . ?
C27 C28 1.478(6) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.445(7) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 O8 1.213(5) . ?
C30 O7 1.313(6) . ?
C31 O9 1.444(4) . ?
C31 C32 1.500(5) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.474(8) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.378(5) . ?
C34 C39 1.391(5) . ?
C34 C40 1.523(5) . ?
C35 C36 1.387(5) . ?
C35 H35 0.9500 . ?
C36 C37 1.401(5) . ?
C36 C41 1.471(5) . ?
C37 C38 1.386(5) . ?
C37 H37 0.9500 . ?
C38 C39 1.399(6) . ?
C38 C40 1.530(5) 2_565 ?
C39 O12 1.392(4) . ?
C40 C38 1.530(5) 3_655 ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 O11 1.242(5) . ?
C41 O10 1.288(5) . ?
C42 O12 1.438(5) . ?
C42 C43 1.493(5) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.515(6) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
O2 H2A 0.919(19) . ?
O4 H4 0.844(19) . ?
O7 H7 0.807(19) . ?
O10 H10 0.860(19) . ?

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
C6 C1 C2 117.3(4) . . ?
C6 C1 C8 121.0(3) . . ?
C2 C1 C8 121.7(3) . . ?
C3 C2 C1 120.6(4) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C2 C3 C4 120.6(4) . . ?
C2 C3 C7 119.1(4) . . ?
C4 C3 C7 120.3(4) . . ?
C5 C4 C3 120.8(4) . . ?
C5 C4 H4A 119.6 . . ?
C3 C4 H4A 119.6 . . ?
C4 C5 C6 118.0(4) . . ?
C4 C5 C8 120.4(4) . 2_557 ?
C6 C5 C8 121.4(4) . 2_557 ?
O3 C6 C5 119.0(3) . . ?
O3 C6 C1 118.4(3) . . ?
C5 C6 C1 122.3(4) . . ?
O2 C7 O1 124.5(4) . . ?
O2 C7 C3 120.6(4) . . ?
O1 C7 C3 114.9(4) . . ?
C5 C8 C1 106.7(3) 3_557 . ?
C5 C8 H8A 110.4 3_557 . ?
C1 C8 H8A 110.4 . . ?
C5 C8 H8B 110.4 3_557 . ?
C1 C8 H8B 110.4 . . ?
H8A C8 H8B 108.6 . . ?
O3 C9 C10 108.8(4) . . ?
O3 C9 H9A 109.9 . . ?
C10 C9 H9A 109.9 . . ?
O3 C9 H9B 109.9 . . ?
C10 C9 H9B 109.9 . . ?
H9A C9 H9B 108.3 . . ?
C9 C10 C11 115.2(4) . . ?
C9 C10 H10A 108.5 . . ?
C11 C10 H10A 108.5 . . ?
C9 C10 H10B 108.5 . . ?
C11 C10 H10B 108.5 . . ?
H10A C10 H10B 107.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 C17 117.8(4) . . ?
C13 C12 C18 120.5(4) . . ?
C17 C12 C18 121.3(3) . . ?
C12 C13 C14 120.7(4) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 H13 119.7 . . ?
C15 C14 C13 119.9(3) . . ?
C15 C14 C26 119.1(4) . . ?
C13 C14 C26 121.0(4) . . ?
C16 C15 C14 121.6(4) . . ?
C16 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
C15 C16 C17 117.5(4) . . ?
C15 C16 C25 121.3(4) . 4_765 ?
C17 C16 C25 120.8(3) . 4_765 ?
O6 C17 C12 118.6(4) . . ?
O6 C17 C16 118.9(4) . . ?
C12 C17 C16 122.4(3) . . ?
C12 C18 C19 109.0(3) . . ?
C12 C18 H18A 109.9 . . ?
C19 C18 H18A 109.9 . . ?
C12 C18 H18B 109.9 . . ?
C19 C18 H18B 109.9 . . ?
H18A C18 H18B 108.3 . . ?
C20 C19 C24 117.7(4) . . ?
C20 C19 C18 121.6(4) . . ?
C24 C19 C18 120.2(4) . . ?
O9 C20 C21 119.1(4) . . ?
O9 C20 C19 118.0(3) . . ?
C21 C20 C19 122.8(3) . . ?
C20 C21 C22 117.3(4) . . ?
C20 C21 C25 120.9(4) . . ?
C22 C21 C25 121.1(4) . . ?
C23 C22 C21 120.7(4) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C24 C23 C22 120.7(3) . . ?
C24 C23 C30 118.0(4) . . ?
C22 C23 C30 121.2(4) . . ?
C23 C24 C19 120.6(4) . . ?
C23 C24 H24 119.7 . . ?
C19 C24 H24 119.7 . . ?
C21 C25 C16 109.3(3) . 4_765 ?
C21 C25 H25A 109.8 . . ?
C16 C25 H25A 109.8 4_765 . ?
C21 C25 H25B 109.8 . . ?
C16 C25 H25B 109.8 4_765 . ?
H25A C25 H25B 108.3 . . ?
O5 C26 O4 122.6(4) . . ?
O5 C26 C14 122.9(5) . . ?
O4 C26 C14 114.5(4) . . ?
O6 C27 C28 109.0(4) . . ?
O6 C27 H27A 109.9 . . ?
C28 C27 H27A 109.9 . . ?
O6 C27 H27B 109.9 . . ?
C28 C27 H27B 109.9 . . ?
H27A C27 H27B 108.3 . . ?
C29 C28 C27 116.7(4) . . ?
C29 C28 H28A 108.1 . . ?
C27 C28 H28A 108.1 . . ?
C29 C28 H28B 108.1 . . ?
C27 C28 H28B 108.1 . . ?
H28A C28 H28B 107.3 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O8 C30 O7 122.9(4) . . ?
O8 C30 C23 123.3(4) . . ?
O7 C30 C23 113.8(4) . . ?
O9 C31 C32 108.5(4) . . ?
O9 C31 H31A 110.0 . . ?
C32 C31 H31A 110.0 . . ?
O9 C31 H31B 110.0 . . ?
C32 C31 H31B 110.0 . . ?
H31A C31 H31B 108.4 . . ?
C33 C32 C31 116.0(5) . . ?
C33 C32 H32A 108.3 . . ?
C31 C32 H32A 108.3 . . ?
C33 C32 H32B 108.3 . . ?
C31 C32 H32B 108.3 . . ?
H32A C32 H32B 107.4 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 C39 118.5(3) . . ?
C35 C34 C40 120.4(3) . . ?
C39 C34 C40 120.7(3) . . ?
C34 C35 C36 120.7(4) . . ?
C34 C35 H35 119.6 . . ?
C36 C35 H35 119.6 . . ?
C35 C36 C37 120.1(3) . . ?
C35 C36 C41 120.0(4) . . ?
C37 C36 C41 119.8(4) . . ?
C38 C37 C36 120.2(4) . . ?
C38 C37 H37 119.9 . . ?
C36 C37 H37 119.9 . . ?
C37 C38 C39 118.2(3) . . ?
C37 C38 C40 120.1(3) . 2_565 ?
C39 C38 C40 121.4(3) . 2_565 ?
C34 C39 O12 119.1(3) . . ?
C34 C39 C38 122.0(3) . . ?
O12 C39 C38 118.8(3) . . ?
C34 C40 C38 107.9(3) . 3_655 ?
C34 C40 H40A 110.1 . . ?
C38 C40 H40A 110.1 3_655 . ?
C34 C40 H40B 110.1 . . ?
C38 C40 H40B 110.1 3_655 . ?
H40A C40 H40B 108.4 . . ?
O11 C41 O10 123.1(4) . . ?
O11 C41 C36 120.4(4) . . ?
O10 C41 C36 116.5(4) . . ?
O12 C42 C43 109.7(3) . . ?
O12 C42 H42A 109.7 . . ?
C43 C42 H42A 109.7 . . ?
O12 C42 H42B 109.7 . . ?
C43 C42 H42B 109.7 . . ?
H42A C42 H42B 108.2 . . ?
C42 C43 C44 114.2(4) . . ?
C42 C43 H43A 108.7 . . ?
C44 C43 H43A 108.7 . . ?
C42 C43 H43B 108.7 . . ?
C44 C43 H43B 108.7 . . ?
H43A C43 H43B 107.6 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C7 O2 H2A 133(4) . . ?
C6 O3 C9 111.9(3) . . ?
C26 O4 H4 124(4) . . ?
C17 O6 C27 112.9(3) . . ?
C30 O7 H7 105(4) . . ?
C20 O9 C31 113.5(3) . . ?
C41 O10 H10 122(4) . . ?
C39 O12 C42 113.5(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 2.1(5) . . . . ?
C8 C1 C2 C3 -175.5(4) . . . . ?
C1 C2 C3 C4 1.6(6) . . . . ?
C1 C2 C3 C7 179.0(4) . . . . ?
C2 C3 C4 C5 -0.7(6) . . . . ?
C7 C3 C4 C5 -178.0(4) . . . . ?
C3 C4 C5 C6 -3.9(6) . . . . ?
C3 C4 C5 C8 170.3(4) . . . 2_557 ?
C4 C5 C6 O3 -178.6(4) . . . . ?
C8 C5 C6 O3 7.2(6) 2_557 . . . ?
C4 C5 C6 C1 7.9(6) . . . . ?
C8 C5 C6 C1 -166.3(4) 2_557 . . . ?
C2 C1 C6 O3 179.5(3) . . . . ?
C8 C1 C6 O3 -3.0(5) . . . . ?
C2 C1 C6 C5 -6.9(6) . . . . ?
C8 C1 C6 C5 170.6(4) . . . . ?
C2 C3 C7 O2 -1.8(6) . . . . ?
C4 C3 C7 O2 175.6(4) . . . . ?
C2 C3 C7 O1 178.8(4) . . . . ?
C4 C3 C7 O1 -3.8(6) . . . . ?
C6 C1 C8 C5 -73.4(5) . . . 3_557 ?
C2 C1 C8 C5 104.0(4) . . . 3_557 ?
O3 C9 C10 C11 61.5(5) . . . . ?
C17 C12 C13 C14 1.5(5) . . . . ?
C18 C12 C13 C14 -171.5(4) . . . . ?
C12 C13 C14 C15 1.6(6) . . . . ?
C12 C13 C14 C26 179.8(4) . . . . ?
C13 C14 C15 C16 -1.5(6) . . . . ?
C26 C14 C15 C16 -179.8(4) . . . . ?
C14 C15 C16 C17 -1.5(6) . . . . ?
C14 C15 C16 C25 171.2(4) . . . 4_765 ?
C13 C12 C17 O6 178.4(3) . . . . ?
C18 C12 C17 O6 -8.7(5) . . . . ?
C13 C12 C17 C16 -4.7(5) . . . . ?
C18 C12 C17 C16 168.2(4) . . . . ?
C15 C16 C17 O6 -178.4(3) . . . . ?
C25 C16 C17 O6 8.9(5) 4_765 . . . ?
C15 C16 C17 C12 4.7(5) . . . . ?
C25 C16 C17 C12 -168.1(4) 4_765 . . . ?
C13 C12 C18 C19 98.5(4) . . . . ?
C17 C12 C18 C19 -74.2(5) . . . . ?
C12 C18 C19 C20 -69.6(5) . . . . ?
C12 C18 C19 C24 102.3(4) . . . . ?
C24 C19 C20 O9 179.9(3) . . . . ?
C18 C19 C20 O9 -8.0(5) . . . . ?
C24 C19 C20 C21 -3.3(5) . . . . ?
C18 C19 C20 C21 168.8(4) . . . . ?
O9 C20 C21 C22 -179.4(3) . . . . ?
C19 C20 C21 C22 3.9(5) . . . . ?
O9 C20 C21 C25 10.0(5) . . . . ?
C19 C20 C21 C25 -166.8(4) . . . . ?
C20 C21 C22 C23 -1.1(5) . . . . ?
C25 C21 C22 C23 169.5(4) . . . . ?
C21 C22 C23 C24 -2.0(6) . . . . ?
C21 C22 C23 C30 -178.9(4) . . . . ?
C22 C23 C24 C19 2.6(6) . . . . ?
C30 C23 C24 C19 179.6(3) . . . . ?
C20 C19 C24 C23 0.0(5) . . . . ?
C18 C19 C24 C23 -172.2(4) . . . . ?
C20 C21 C25 C16 71.0(5) . . . 4_765 ?
C22 C21 C25 C16 -99.2(4) . . . 4_765 ?
C15 C14 C26 O5 2.5(6) . . . . ?
C13 C14 C26 O5 -175.7(4) . . . . ?
C15 C14 C26 O4 -177.3(4) . . . . ?
C13 C14 C26 O4 4.5(5) . . . . ?
O6 C27 C28 C29 -61.6(6) . . . . ?
C24 C23 C30 O8 -1.2(6) . . . . ?
C22 C23 C30 O8 175.7(4) . . . . ?
C24 C23 C30 O7 -178.6(4) . . . . ?
C22 C23 C30 O7 -1.6(5) . . . . ?
O9 C31 C32 C33 61.9(6) . . . . ?
C39 C34 C35 C36 -1.2(5) . . . . ?
C40 C34 C35 C36 172.6(3) . . . . ?
C34 C35 C36 C37 -2.4(5) . . . . ?
C34 C35 C36 C41 -178.5(4) . . . . ?
C35 C36 C37 C38 2.1(6) . . . . ?
C41 C36 C37 C38 178.2(3) . . . . ?
C36 C37 C38 C39 1.8(5) . . . . ?
C36 C37 C38 C40 -171.7(3) . . . 2_565 ?
C35 C34 C39 O12 -178.6(3) . . . . ?
C40 C34 C39 O12 7.5(5) . . . . ?
C35 C34 C39 C38 5.3(6) . . . . ?
C40 C34 C39 C38 -168.5(3) . . . . ?
C37 C38 C39 C34 -5.6(5) . . . . ?
C40 C38 C39 C34 167.8(4) 2_565 . . . ?
C37 C38 C39 O12 178.3(3) . . . . ?
C40 C38 C39 O12 -8.3(5) 2_565 . . . ?
C35 C34 C40 C38 -102.7(4) . . . 3_655 ?
C39 C34 C40 C38 71.0(4) . . . 3_655 ?
C35 C36 C41 O11 -6.8(6) . . . . ?
C37 C36 C41 O11 177.0(4) . . . . ?
C35 C36 C41 O10 175.1(4) . . . . ?
C37 C36 C41 O10 -1.1(6) . . . . ?
O12 C42 C43 C44 -60.0(5) . . . . ?
C5 C6 O3 C9 91.9(4) . . . . ?
C1 C6 O3 C9 -94.4(4) . . . . ?
C10 C9 O3 C6 164.2(3) . . . . ?
C12 C17 O6 C27 -94.2(4) . . . . ?
C16 C17 O6 C27 88.7(4) . . . . ?
C28 C27 O6 C17 -173.0(4) . . . . ?
C21 C20 O9 C31 90.5(4) . . . . ?
C19 C20 O9 C31 -92.6(4) . . . . ?
C32 C31 O9 C20 163.6(4) . . . . ?
C34 C39 O12 C42 87.2(4) . . . . ?
C38 C39 O12 C42 -96.6(4) . . . . ?
C43 C42 O12 C39 -167.5(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.144
_refine_diff_density_min         -0.157
_refine_diff_density_rms         0.033
