# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2017

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

data_cu_khx26_0m
_database_code_depnum_ccdc_archive 'CCDC 1545247'
_audit_update_record             
;
2017-04-21 deposited with the CCDC.
2017-07-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H53 N O6'
_chemical_formula_sum            'C33 H53 N O6'
_chemical_formula_weight         559.76
_chemical_absolute_configuration ad

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_space_group_name_Hall  'P 2yb'

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

_cell_length_a                   9.5634(4)
_cell_length_b                   11.2799(5)
_cell_length_c                   14.9190(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.4570(10)
_cell_angle_gamma                90.00
_cell_volume                     1565.19(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9916
_cell_measurement_theta_min      4.75
_cell_measurement_theta_max      69.03

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             612
_exptl_absorpt_coefficient_mu    0.639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7242
_exptl_absorpt_correction_T_max  0.9216
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\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            11214
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_sigmaI/netI    0.0578
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         4.75
_diffrn_reflns_theta_max         69.10
_reflns_number_total             4428
_reflns_number_gt                4352
_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)+(0.2000P)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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.2(3)
_refine_ls_number_reflns         4428
_refine_ls_number_parameters     372
_refine_ls_number_restraints     241
_refine_ls_R_factor_all          0.1072
_refine_ls_R_factor_gt           0.1056
_refine_ls_wR_factor_ref         0.2950
_refine_ls_wR_factor_gt          0.2898
_refine_ls_goodness_of_fit_ref   1.492
_refine_ls_restrained_S_all      1.540
_refine_ls_shift/su_max          0.002
_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
O3 O 0.4975(3) 0.5719(3) 0.79705(19) 0.0160(7) Uani 1 1 d U . .
H3 H 0.5619 0.5318 0.8320 0.024 Uiso 1 1 calc R . .
O16 O 0.8860(3) 0.4100(2) 0.11882(18) 0.0123(6) Uani 1 1 d U . .
O24 O 0.8905(3) 0.3074(3) -0.0362(2) 0.0155(6) Uani 1 1 d U . .
O31 O 0.7204(3) 0.4465(3) -0.0832(2) 0.0224(7) Uani 1 1 d U . .
O25 O 1.2250(3) 0.4624(3) -0.0210(2) 0.0231(7) Uani 1 1 d U . .
C6 C 0.5031(4) 0.4227(4) 0.4782(3) 0.0152(8) Uani 1 1 d U . .
H6A H 0.5470 0.3450 0.4990 0.018 Uiso 1 1 calc R . .
H6B H 0.3973 0.4129 0.4626 0.018 Uiso 1 1 calc R . .
C8 C 0.7167(4) 0.4589(4) 0.4103(3) 0.0120(8) Uani 1 1 d U . .
H8 H 0.7447 0.3741 0.4232 0.014 Uiso 1 1 calc R . .
C3 C 0.5368(4) 0.5919(4) 0.7111(3) 0.0151(8) Uani 1 1 d U . .
H3A H 0.4780 0.6606 0.6811 0.018 Uiso 1 1 calc R . .
C4 C 0.4962(4) 0.4852(4) 0.6447(3) 0.0137(8) Uani 1 1 d U . .
C5 C 0.5467(4) 0.5136(4) 0.5557(3) 0.0126(8) Uani 1 1 d U . .
H5 H 0.4938 0.5876 0.5311 0.015 Uiso 1 1 calc R . .
C7 C 0.5527(4) 0.4634(4) 0.3932(3) 0.0146(8) Uani 1 1 d U . .
H7A H 0.5192 0.5455 0.3775 0.017 Uiso 1 1 calc R . .
H7B H 0.5096 0.4118 0.3403 0.017 Uiso 1 1 calc R . .
C14 C 0.7757(4) 0.4959(4) 0.3263(3) 0.0118(8) Uani 1 1 d U . .
C15 C 0.7643(4) 0.4026(4) 0.2510(3) 0.0130(8) Uani 1 1 d U . .
C16 C 0.9017(4) 0.4020(4) 0.2153(3) 0.0126(8) Uani 1 1 d U . .
H16 H 0.9562 0.3278 0.2374 0.015 Uiso 1 1 calc R . .
C23 C 1.0268(4) 0.3934(4) 0.1009(3) 0.0141(8) Uani 1 1 d U . .
H23 H 1.0636 0.3133 0.1238 0.017 Uiso 1 1 calc R . .
C24 C 1.0006(4) 0.3953(4) -0.0042(3) 0.0152(8) Uani 1 1 d U . .
H24 H 0.9628 0.4750 -0.0273 0.018 Uiso 1 1 calc R . .
C31 C 0.7528(4) 0.3448(4) -0.0640(3) 0.0162(9) Uani 1 1 d U . .
C32 C 0.6515(4) 0.2446(4) -0.0644(3) 0.0186(9) Uani 1 1 d U . .
H32A H 0.6312 0.2369 -0.0032 0.028 Uiso 1 1 calc R . .
H32B H 0.6948 0.1710 -0.0801 0.028 Uiso 1 1 calc R . .
H32C H 0.5617 0.2599 -0.1102 0.028 Uiso 1 1 calc R . .
C2 C 0.6932(4) 0.6293(4) 0.7272(3) 0.0158(9) Uani 1 1 d U . .
H2A H 0.7550 0.5655 0.7607 0.019 Uiso 1 1 calc R . .
H2B H 0.7088 0.7012 0.7662 0.019 Uiso 1 1 calc R . .
C1 C 0.7370(4) 0.6549(4) 0.6369(3) 0.0149(8) Uani 1 1 d U . .
H1A H 0.8409 0.6737 0.6499 0.018 Uiso 1 1 calc R . .
H1B H 0.6831 0.7243 0.6062 0.018 Uiso 1 1 calc R . .
C10 C 0.7052(4) 0.5468(3) 0.5736(3) 0.0111(8) Uani 1 1 d U . .
C9 C 0.7891(4) 0.5300(3) 0.4989(3) 0.0108(8) Uani 1 1 d U . .
C19 C 0.8242(4) 0.4562(4) 0.5860(3) 0.0110(8) Uani 1 1 d U . .
H19A H 0.7967 0.3715 0.5811 0.013 Uiso 1 1 calc R . .
H19B H 0.9149 0.4738 0.6317 0.013 Uiso 1 1 calc R . .
C11 C 0.8911(4) 0.6322(4) 0.4897(3) 0.0158(8) Uani 1 1 d U . .
H11A H 0.9602 0.6419 0.5499 0.019 Uiso 1 1 calc R . .
H11B H 0.8333 0.7058 0.4780 0.019 Uiso 1 1 calc R . .
C12 C 0.9789(4) 0.6228(4) 0.4145(3) 0.0121(8) Uani 1 1 d U . .
H12A H 0.9583 0.6929 0.3736 0.015 Uiso 1 1 calc R . .
H12B H 1.0828 0.6235 0.4445 0.015 Uiso 1 1 calc R . .
C13 C 0.9440(4) 0.5113(4) 0.3571(3) 0.0111(8) Uani 1 1 d U . .
C18 C 1.0146(4) 0.4051(4) 0.4166(3) 0.0119(8) Uani 1 1 d U . .
H18A H 1.1192 0.4088 0.4247 0.018 Uiso 1 1 calc R . .
H18B H 0.9785 0.3307 0.3857 0.018 Uiso 1 1 calc R . .
H18C H 0.9908 0.4084 0.4769 0.018 Uiso 1 1 calc R . .
C17 C 0.9871(4) 0.5076(4) 0.2650(3) 0.0119(8) Uani 1 1 d U . .
H17 H 0.9445 0.5800 0.2305 0.014 Uiso 1 1 calc R . .
C25 C 1.1294(4) 0.3630(4) -0.0470(3) 0.0185(9) Uani 1 1 d U . .
C26 C 1.0761(5) 0.3603(5) -0.1522(4) 0.0312(11) Uani 1 1 d U . .
H26A H 1.0241 0.4338 -0.1732 0.047 Uiso 1 1 calc R . .
H26B H 1.0117 0.2924 -0.1701 0.047 Uiso 1 1 calc R . .
H26C H 1.1584 0.3529 -0.1805 0.047 Uiso 1 1 calc R . .
C27 C 1.1965(5) 0.2457(5) -0.0103(4) 0.0263(11) Uani 1 1 d U . .
H27A H 1.2641 0.2202 -0.0468 0.039 Uiso 1 1 calc R . .
H27B H 1.1209 0.1859 -0.0146 0.039 Uiso 1 1 calc R . .
H27C H 1.2480 0.2552 0.0543 0.039 Uiso 1 1 calc R . .
C33 C 1.3660(5) 0.4461(5) -0.0356(4) 0.0329(11) Uani 1 1 d U . .
H33A H 1.4228 0.3974 0.0141 0.049 Uiso 1 1 calc R . .
H33B H 1.4125 0.5234 -0.0363 0.049 Uiso 1 1 calc R . .
H33C H 1.3596 0.4062 -0.0948 0.049 Uiso 1 1 calc R . .
C22 C 1.1325(4) 0.4871(4) 0.1492(3) 0.0148(8) Uani 1 1 d U . .
H22A H 1.1049 0.5647 0.1192 0.018 Uiso 1 1 calc R . .
H22B H 1.2295 0.4673 0.1408 0.018 Uiso 1 1 calc R . .
C20 C 1.1400(4) 0.4993(4) 0.2532(3) 0.0122(8) Uani 1 1 d U . .
H20 H 1.1865 0.4268 0.2857 0.015 Uiso 1 1 calc R . .
C21 C 1.2311(4) 0.6078(4) 0.2905(3) 0.0161(8) Uani 1 1 d U . .
H21A H 1.1772 0.6801 0.2685 0.024 Uiso 1 1 calc R . .
H21B H 1.3203 0.6065 0.2689 0.024 Uiso 1 1 calc R . .
H21C H 1.2542 0.6063 0.3580 0.024 Uiso 1 1 calc R . .
C28 C 0.7012(4) 0.6087(4) 0.2813(3) 0.0152(8) Uani 1 1 d U . .
H28A H 0.7479 0.6355 0.2330 0.023 Uiso 1 1 calc R . .
H28B H 0.7084 0.6709 0.3281 0.023 Uiso 1 1 calc R . .
H28C H 0.5997 0.5917 0.2542 0.023 Uiso 1 1 calc R . .
C29 C 0.3323(4) 0.4721(4) 0.6237(3) 0.0203(9) Uani 1 1 d U . .
H29A H 0.3039 0.3987 0.5891 0.030 Uiso 1 1 calc R . .
H29B H 0.2874 0.5400 0.5870 0.030 Uiso 1 1 calc R . .
H29C H 0.3007 0.4693 0.6816 0.030 Uiso 1 1 calc R . .
C30 C 0.5637(4) 0.3707(4) 0.6910(3) 0.0170(8) Uani 1 1 d U . .
H30A H 0.5183 0.3498 0.7413 0.026 Uiso 1 1 calc R . .
H30B H 0.6670 0.3829 0.7157 0.026 Uiso 1 1 calc R . .
H30C H 0.5490 0.3065 0.6456 0.026 Uiso 1 1 calc R . .
N15 N 0.6633(3) 0.3255(3) 0.2350(2) 0.0160(8) Uani 1 1 d U . .
O15 O 0.6826(3) 0.2430(3) 0.1685(2) 0.0224(7) Uani 1 1 d U . .
H15 H 0.6195 0.1899 0.1630 0.034 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
O3 C3 1.435(5) . ?
O3 H3 0.8400 . ?
O16 C16 1.415(5) . ?
O16 C23 1.445(4) . ?
O24 C31 1.352(5) . ?
O24 C24 1.445(5) . ?
O31 C31 1.205(6) . ?
O25 C33 1.427(6) . ?
O25 C25 1.441(5) . ?
C6 C7 1.525(6) . ?
C6 C5 1.530(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C8 C7 1.531(5) . ?
C8 C14 1.546(5) . ?
C8 C9 1.563(5) . ?
C8 H8 1.0000 . ?
C3 C2 1.518(5) . ?
C3 C4 1.550(6) . ?
C3 H3A 1.0000 . ?
C4 C29 1.533(5) . ?
C4 C30 1.534(6) . ?
C4 C5 1.548(5) . ?
C5 C10 1.524(5) . ?
C5 H5 1.0000 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C14 C15 1.526(6) . ?
C14 C28 1.534(5) . ?
C14 C13 1.578(5) . ?
C15 N15 1.280(5) . ?
C15 C16 1.529(5) . ?
C16 C17 1.534(5) . ?
C16 H16 1.0000 . ?
C23 C22 1.524(5) . ?
C23 C24 1.529(6) . ?
C23 H23 1.0000 . ?
C24 C25 1.558(5) . ?
C24 H24 1.0000 . ?
C31 C32 1.488(6) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C2 C1 1.528(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C1 C10 1.529(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C10 C19 1.508(5) . ?
C10 C9 1.529(5) . ?
C9 C19 1.514(5) . ?
C9 C11 1.537(5) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C11 C12 1.553(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.515(5) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C17 1.524(5) . ?
C13 C18 1.549(5) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C17 C20 1.516(5) . ?
C17 H17 1.0000 . ?
C25 C27 1.516(7) . ?
C25 C26 1.533(7) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C22 C20 1.543(6) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C20 C21 1.530(6) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
N15 O15 1.403(5) . ?
O15 H15 0.8400 . ?

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
C3 O3 H3 109.5 . . ?
C16 O16 C23 107.3(3) . . ?
C31 O24 C24 118.0(3) . . ?
C33 O25 C25 114.9(3) . . ?
C7 C6 C5 110.1(3) . . ?
C7 C6 H6A 109.6 . . ?
C5 C6 H6A 109.6 . . ?
C7 C6 H6B 109.6 . . ?
C5 C6 H6B 109.6 . . ?
H6A C6 H6B 108.2 . . ?
C7 C8 C14 114.1(3) . . ?
C7 C8 C9 111.0(3) . . ?
C14 C8 C9 111.9(3) . . ?
C7 C8 H8 106.4 . . ?
C14 C8 H8 106.4 . . ?
C9 C8 H8 106.4 . . ?
O3 C3 C2 110.8(3) . . ?
O3 C3 C4 111.7(3) . . ?
C2 C3 C4 114.0(3) . . ?
O3 C3 H3A 106.6 . . ?
C2 C3 H3A 106.6 . . ?
C4 C3 H3A 106.6 . . ?
C29 C4 C30 108.3(3) . . ?
C29 C4 C5 110.7(3) . . ?
C30 C4 C5 112.2(3) . . ?
C29 C4 C3 107.3(3) . . ?
C30 C4 C3 110.4(3) . . ?
C5 C4 C3 107.8(3) . . ?
C10 C5 C6 112.4(3) . . ?
C10 C5 C4 113.4(3) . . ?
C6 C5 C4 115.1(3) . . ?
C10 C5 H5 104.9 . . ?
C6 C5 H5 104.9 . . ?
C4 C5 H5 104.9 . . ?
C6 C7 C8 110.9(3) . . ?
C6 C7 H7A 109.5 . . ?
C8 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
C15 C14 C28 107.7(3) . . ?
C15 C14 C8 115.7(3) . . ?
C28 C14 C8 111.0(3) . . ?
C15 C14 C13 100.5(3) . . ?
C28 C14 C13 112.0(3) . . ?
C8 C14 C13 109.5(3) . . ?
N15 C15 C14 121.9(3) . . ?
N15 C15 C16 127.2(4) . . ?
C14 C15 C16 109.9(3) . . ?
O16 C16 C15 117.2(3) . . ?
O16 C16 C17 111.1(3) . . ?
C15 C16 C17 103.5(3) . . ?
O16 C16 H16 108.2 . . ?
C15 C16 H16 108.2 . . ?
C17 C16 H16 108.2 . . ?
O16 C23 C22 111.5(3) . . ?
O16 C23 C24 104.5(3) . . ?
C22 C23 C24 114.0(3) . . ?
O16 C23 H23 108.9 . . ?
C22 C23 H23 108.9 . . ?
C24 C23 H23 108.9 . . ?
O24 C24 C23 105.2(3) . . ?
O24 C24 C25 106.8(3) . . ?
C23 C24 C25 117.4(3) . . ?
O24 C24 H24 109.0 . . ?
C23 C24 H24 109.0 . . ?
C25 C24 H24 109.0 . . ?
O31 C31 O24 123.2(4) . . ?
O31 C31 C32 126.2(4) . . ?
O24 C31 C32 110.5(4) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C3 C2 C1 112.1(3) . . ?
C3 C2 H2A 109.2 . . ?
C1 C2 H2A 109.2 . . ?
C3 C2 H2B 109.2 . . ?
C1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
C2 C1 C10 109.7(3) . . ?
C2 C1 H1A 109.7 . . ?
C10 C1 H1A 109.7 . . ?
C2 C1 H1B 109.7 . . ?
C10 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
C19 C10 C5 123.2(3) . . ?
C19 C10 C9 59.8(2) . . ?
C5 C10 C9 120.8(3) . . ?
C19 C10 C1 115.3(3) . . ?
C5 C10 C1 110.5(3) . . ?
C9 C10 C1 119.1(3) . . ?
C19 C9 C10 59.4(2) . . ?
C19 C9 C11 118.1(3) . . ?
C10 C9 C11 115.1(3) . . ?
C19 C9 C8 114.2(3) . . ?
C10 C9 C8 118.4(3) . . ?
C11 C9 C8 118.4(3) . . ?
C10 C19 C9 60.8(2) . . ?
C10 C19 H19A 117.7 . . ?
C9 C19 H19A 117.7 . . ?
C10 C19 H19B 117.7 . . ?
C9 C19 H19B 117.7 . . ?
H19A C19 H19B 114.8 . . ?
C9 C11 C12 118.3(3) . . ?
C9 C11 H11A 107.7 . . ?
C12 C11 H11A 107.7 . . ?
C9 C11 H11B 107.7 . . ?
C12 C11 H11B 107.7 . . ?
H11A C11 H11B 107.1 . . ?
C13 C12 C11 112.4(3) . . ?
C13 C12 H12A 109.1 . . ?
C11 C12 H12A 109.1 . . ?
C13 C12 H12B 109.1 . . ?
C11 C12 H12B 109.1 . . ?
H12A C12 H12B 107.9 . . ?
C12 C13 C17 117.6(3) . . ?
C12 C13 C18 108.0(3) . . ?
C17 C13 C18 108.8(3) . . ?
C12 C13 C14 109.3(3) . . ?
C17 C13 C14 101.9(3) . . ?
C18 C13 C14 111.1(3) . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C13 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C17 C13 125.2(3) . . ?
C20 C17 C16 108.4(3) . . ?
C13 C17 C16 103.4(3) . . ?
C20 C17 H17 106.2 . . ?
C13 C17 H17 106.2 . . ?
C16 C17 H17 106.2 . . ?
O25 C25 C27 113.1(3) . . ?
O25 C25 C26 109.3(4) . . ?
C27 C25 C26 111.4(4) . . ?
O25 C25 C24 102.7(3) . . ?
C27 C25 C24 111.3(4) . . ?
C26 C25 C24 108.5(3) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O25 C33 H33A 109.5 . . ?
O25 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
O25 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C23 C22 C20 114.1(3) . . ?
C23 C22 H22A 108.7 . . ?
C20 C22 H22A 108.7 . . ?
C23 C22 H22B 108.7 . . ?
C20 C22 H22B 108.7 . . ?
H22A C22 H22B 107.6 . . ?
C17 C20 C21 113.0(3) . . ?
C17 C20 C22 107.6(3) . . ?
C21 C20 C22 109.0(3) . . ?
C17 C20 H20 109.0 . . ?
C21 C20 H20 109.0 . . ?
C22 C20 H20 109.0 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C14 C28 H28A 109.5 . . ?
C14 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C14 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C4 C29 H29A 109.5 . . ?
C4 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C4 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C4 C30 H30A 109.5 . . ?
C4 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C4 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C15 N15 O15 111.4(3) . . ?
N15 O15 H15 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
O3 C3 C4 C29 62.4(4) . . . . ?
C2 C3 C4 C29 -170.9(3) . . . . ?
O3 C3 C4 C30 -55.4(4) . . . . ?
C2 C3 C4 C30 71.2(4) . . . . ?
O3 C3 C4 C5 -178.3(3) . . . . ?
C2 C3 C4 C5 -51.7(4) . . . . ?
C7 C6 C5 C10 -50.8(4) . . . . ?
C7 C6 C5 C4 177.3(3) . . . . ?
C29 C4 C5 C10 171.0(3) . . . . ?
C30 C4 C5 C10 -67.9(4) . . . . ?
C3 C4 C5 C10 53.9(4) . . . . ?
C29 C4 C5 C6 -57.6(4) . . . . ?
C30 C4 C5 C6 63.6(4) . . . . ?
C3 C4 C5 C6 -174.6(3) . . . . ?
C5 C6 C7 C8 69.0(4) . . . . ?
C14 C8 C7 C6 178.5(4) . . . . ?
C9 C8 C7 C6 -53.9(4) . . . . ?
C7 C8 C14 C15 -77.9(4) . . . . ?
C9 C8 C14 C15 154.9(3) . . . . ?
C7 C8 C14 C28 45.1(4) . . . . ?
C9 C8 C14 C28 -82.0(4) . . . . ?
C7 C8 C14 C13 169.3(3) . . . . ?
C9 C8 C14 C13 42.2(4) . . . . ?
C28 C14 C15 N15 -94.9(4) . . . . ?
C8 C14 C15 N15 30.0(5) . . . . ?
C13 C14 C15 N15 147.8(4) . . . . ?
C28 C14 C15 C16 96.2(3) . . . . ?
C8 C14 C15 C16 -138.9(3) . . . . ?
C13 C14 C15 C16 -21.1(4) . . . . ?
C23 O16 C16 C15 -173.1(3) . . . . ?
C23 O16 C16 C17 68.2(4) . . . . ?
N15 C15 C16 O16 63.1(5) . . . . ?
C14 C15 C16 O16 -128.7(4) . . . . ?
N15 C15 C16 C17 -174.2(4) . . . . ?
C14 C15 C16 C17 -6.0(4) . . . . ?
C16 O16 C23 C22 -59.8(4) . . . . ?
C16 O16 C23 C24 176.6(3) . . . . ?
C31 O24 C24 C23 97.5(4) . . . . ?
C31 O24 C24 C25 -137.0(4) . . . . ?
O16 C23 C24 O24 -53.6(4) . . . . ?
C22 C23 C24 O24 -175.6(3) . . . . ?
O16 C23 C24 C25 -172.2(3) . . . . ?
C22 C23 C24 C25 65.8(5) . . . . ?
C24 O24 C31 O31 17.3(6) . . . . ?
C24 O24 C31 C32 -161.1(4) . . . . ?
O3 C3 C2 C1 -178.3(3) . . . . ?
C4 C3 C2 C1 54.6(5) . . . . ?
C3 C2 C1 C10 -55.6(4) . . . . ?
C6 C5 C10 C19 -49.2(5) . . . . ?
C4 C5 C10 C19 83.6(5) . . . . ?
C6 C5 C10 C9 22.7(5) . . . . ?
C4 C5 C10 C9 155.5(3) . . . . ?
C6 C5 C10 C1 168.5(3) . . . . ?
C4 C5 C10 C1 -58.7(4) . . . . ?
C2 C1 C10 C19 -88.2(4) . . . . ?
C2 C1 C10 C5 57.3(4) . . . . ?
C2 C1 C10 C9 -156.3(3) . . . . ?
C5 C10 C9 C19 -113.0(4) . . . . ?
C1 C10 C9 C19 104.1(4) . . . . ?
C19 C10 C9 C11 -109.1(4) . . . . ?
C5 C10 C9 C11 138.0(4) . . . . ?
C1 C10 C9 C11 -5.0(5) . . . . ?
C19 C10 C9 C8 102.8(4) . . . . ?
C5 C10 C9 C8 -10.2(5) . . . . ?
C1 C10 C9 C8 -153.1(3) . . . . ?
C7 C8 C9 C19 91.9(4) . . . . ?
C14 C8 C9 C19 -139.3(3) . . . . ?
C7 C8 C9 C10 25.0(5) . . . . ?
C14 C8 C9 C10 153.7(3) . . . . ?
C7 C8 C9 C11 -122.1(4) . . . . ?
C14 C8 C9 C11 6.7(5) . . . . ?
C5 C10 C19 C9 109.1(4) . . . . ?
C1 C10 C19 C9 -110.3(4) . . . . ?
C11 C9 C19 C10 104.1(4) . . . . ?
C8 C9 C19 C10 -109.9(3) . . . . ?
C19 C9 C11 C12 113.5(4) . . . . ?
C10 C9 C11 C12 -179.3(3) . . . . ?
C8 C9 C11 C12 -31.1(5) . . . . ?
C9 C11 C12 C13 2.3(5) . . . . ?
C11 C12 C13 C17 162.4(3) . . . . ?
C11 C12 C13 C18 -74.0(4) . . . . ?
C11 C12 C13 C14 47.0(4) . . . . ?
C15 C14 C13 C12 165.4(3) . . . . ?
C28 C14 C13 C12 51.4(4) . . . . ?
C8 C14 C13 C12 -72.3(4) . . . . ?
C15 C14 C13 C17 40.3(4) . . . . ?
C28 C14 C13 C17 -73.7(4) . . . . ?
C8 C14 C13 C17 162.6(3) . . . . ?
C15 C14 C13 C18 -75.4(4) . . . . ?
C28 C14 C13 C18 170.5(3) . . . . ?
C8 C14 C13 C18 46.8(4) . . . . ?
C12 C13 C17 C20 70.6(5) . . . . ?
C18 C13 C17 C20 -52.5(5) . . . . ?
C14 C13 C17 C20 -170.0(4) . . . . ?
C12 C13 C17 C16 -165.0(3) . . . . ?
C18 C13 C17 C16 71.9(3) . . . . ?
C14 C13 C17 C16 -45.6(3) . . . . ?
O16 C16 C17 C20 -66.7(4) . . . . ?
C15 C16 C17 C20 166.7(3) . . . . ?
O16 C16 C17 C13 158.6(3) . . . . ?
C15 C16 C17 C13 32.0(4) . . . . ?
C33 O25 C25 C27 48.0(5) . . . . ?
C33 O25 C25 C26 -76.7(5) . . . . ?
C33 O25 C25 C24 168.2(4) . . . . ?
O24 C24 C25 O25 173.1(3) . . . . ?
C23 C24 C25 O25 -69.1(4) . . . . ?
O24 C24 C25 C27 -65.5(4) . . . . ?
C23 C24 C25 C27 52.3(5) . . . . ?
O24 C24 C25 C26 57.5(4) . . . . ?
C23 C24 C25 C26 175.3(4) . . . . ?
O16 C23 C22 C20 52.3(4) . . . . ?
C24 C23 C22 C20 170.3(3) . . . . ?
C13 C17 C20 C21 -64.4(5) . . . . ?
C16 C17 C20 C21 173.4(3) . . . . ?
C13 C17 C20 C22 175.2(4) . . . . ?
C16 C17 C20 C22 53.0(4) . . . . ?
C23 C22 C20 C17 -48.5(4) . . . . ?
C23 C22 C20 C21 -171.4(3) . . . . ?
C14 C15 N15 O15 -174.7(3) . . . . ?
C16 C15 N15 O15 -7.8(5) . . . . ?

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
O3 H3 O31 0.84 1.98 2.822(4) 176.5 1_556
O15 H15 O3 0.84 1.92 2.714(4) 156.9 2_646

_diffrn_measured_fraction_theta_max 0.939
_diffrn_reflns_theta_full        69.10
_diffrn_measured_fraction_theta_full 0.939
_refine_diff_density_max         0.900
_refine_diff_density_min         -1.295
_refine_diff_density_rms         0.155
