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

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

data_s1434
_database_code_depnum_ccdc_archive 'CCDC 1413286'
_audit_update_record             
;
2015-07-16 deposited with the CCDC.
2016-01-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H30 N2 O3'
_chemical_formula_weight         406.51

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           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                   22.546(14)
_cell_length_b                   9.314(10)
_cell_length_c                   10.283(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.43(6)
_cell_angle_gamma                90.00
_cell_volume                     2136(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2462
_cell_measurement_theta_min      2.75
_cell_measurement_theta_max      25.70

_exptl_crystal_description       prismatic
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10592
_diffrn_reflns_av_R_equivalents  0.0679
_diffrn_reflns_av_sigmaI/netI    0.0704
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         25.03
_reflns_number_total             3761
_reflns_number_gt                2457
_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)+(0.0457P)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         3761
_refine_ls_number_parameters     272
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0415
_refine_ls_wR_factor_ref         0.0974
_refine_ls_wR_factor_gt          0.0902
_refine_ls_goodness_of_fit_ref   0.869
_refine_ls_restrained_S_all      0.869
_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 0.27927(6) 0.02765(14) 0.01800(11) 0.0372(3) Uani 1 1 d . . .
H1 H 0.2734 -0.0074 0.0903 0.056 Uiso 1 1 calc R . .
O2 O 0.27084(5) 0.39100(13) -0.11433(10) 0.0281(3) Uani 1 1 d . . .
O3 O 0.26456(5) 0.59103(13) -0.23796(11) 0.0341(3) Uani 1 1 d . . .
N1 N 0.32706(6) 0.52623(16) 0.14829(13) 0.0291(4) Uani 1 1 d . . .
N2 N 0.22139(6) 0.57794(15) -0.04978(12) 0.0246(3) Uani 1 1 d . . .
C1 C 0.16003(8) 0.4576(2) 0.09871(16) 0.0309(5) Uani 1 1 d . . .
H1A H 0.1483 0.5456 0.1446 0.037 Uiso 1 1 calc R . .
C2 C 0.10752(8) 0.4114(2) -0.00614(18) 0.0389(5) Uani 1 1 d . . .
H2A H 0.0788 0.4897 -0.0344 0.047 Uiso 1 1 calc R . .
H2B H 0.1203 0.3626 -0.0829 0.047 Uiso 1 1 calc R . .
C3 C 0.08631(9) 0.3081(2) 0.0941(2) 0.0545(6) Uani 1 1 d . . .
H3A H 0.0527 0.3458 0.1360 0.065 Uiso 1 1 calc R . .
H3B H 0.0776 0.2099 0.0597 0.065 Uiso 1 1 calc R . .
C4 C 0.14783(9) 0.3230(2) 0.1796(2) 0.0491(6) Uani 1 1 d . . .
H4A H 0.1753 0.2419 0.1707 0.059 Uiso 1 1 calc R . .
H4B H 0.1456 0.3435 0.2733 0.059 Uiso 1 1 calc R . .
C5 C 0.22259(8) 0.47875(19) 0.06202(15) 0.0258(4) Uani 1 1 d . . .
C6 C 0.26624(8) 0.5326(2) 0.17934(16) 0.0291(4) Uani 1 1 d . . .
H6A H 0.2562 0.6327 0.2000 0.035 Uiso 1 1 calc R . .
H6B H 0.2630 0.4724 0.2573 0.035 Uiso 1 1 calc R . .
C7 C 0.34845(8) 0.3779(2) 0.14686(17) 0.0304(4) Uani 1 1 d . . .
H7A H 0.3666 0.3501 0.2369 0.037 Uiso 1 1 calc R . .
H7B H 0.3800 0.3715 0.0895 0.037 Uiso 1 1 calc R . .
C8 C 0.29781(7) 0.27310(19) 0.09737(16) 0.0264(4) Uani 1 1 d . . .
H8 H 0.2797 0.2421 0.1760 0.032 Uiso 1 1 calc R . .
C9 C 0.24842(8) 0.34310(19) 0.00423(15) 0.0262(4) Uani 1 1 d . . .
H9 H 0.2154 0.2722 -0.0203 0.031 Uiso 1 1 calc R . .
C10 C 0.32238(8) 0.1389(2) 0.04056(17) 0.0319(5) Uani 1 1 d . . .
H10A H 0.3365 0.1635 -0.0435 0.038 Uiso 1 1 calc R . .
H10B H 0.3573 0.1039 0.1020 0.038 Uiso 1 1 calc R . .
C11 C 0.36859(8) 0.6166(2) 0.23653(17) 0.0369(5) Uani 1 1 d . . .
H11A H 0.3705 0.5810 0.3278 0.044 Uiso 1 1 calc R . .
H11B H 0.3531 0.7161 0.2337 0.044 Uiso 1 1 calc R . .
C12 C 0.43085(9) 0.6167(2) 0.19922(18) 0.0372(5) Uani 1 1 d . . .
C13 C 0.47660(9) 0.5375(2) 0.2722(2) 0.0435(5) Uani 1 1 d . . .
H13 H 0.4684 0.4858 0.3472 0.052 Uiso 1 1 calc R . .
C14 C 0.53377(10) 0.5326(2) 0.2379(2) 0.0516(6) Uani 1 1 d . . .
H14 H 0.5642 0.4767 0.2882 0.062 Uiso 1 1 calc R . .
C15 C 0.54612(10) 0.6083(3) 0.1316(2) 0.0535(6) Uani 1 1 d . . .
H15 H 0.5855 0.6067 0.1090 0.064 Uiso 1 1 calc R . .
C16 C 0.50238(11) 0.6866(2) 0.0575(2) 0.0522(6) Uani 1 1 d . . .
H16 H 0.5113 0.7389 -0.0165 0.063 Uiso 1 1 calc R . .
C17 C 0.44423(11) 0.6897(2) 0.0907(2) 0.0489(6) Uani 1 1 d . . .
H17 H 0.4138 0.7427 0.0378 0.059 Uiso 1 1 calc R . .
C18 C 0.25313(8) 0.5284(2) -0.14079(16) 0.0267(4) Uani 1 1 d . . .
C19 C 0.20699(8) 0.73016(19) -0.04415(16) 0.0286(4) Uani 1 1 d . . .
H19A H 0.2380 0.7855 -0.0815 0.034 Uiso 1 1 calc R . .
H19B H 0.2091 0.7584 0.0492 0.034 Uiso 1 1 calc R . .
C20 C 0.14617(8) 0.7722(2) -0.11595(16) 0.0318(5) Uani 1 1 d . . .
C21 C 0.11745(8) 0.6960(2) -0.22225(18) 0.0394(5) Uani 1 1 d . . .
H21 H 0.1357 0.6120 -0.2508 0.047 Uiso 1 1 calc R . .
C22 C 0.06229(9) 0.7407(3) -0.2878(2) 0.0562(7) Uani 1 1 d . . .
H22 H 0.0433 0.6880 -0.3614 0.067 Uiso 1 1 calc R . .
C23 C 0.03526(10) 0.8607(3) -0.2464(3) 0.0651(8) Uani 1 1 d . . .
H23 H -0.0028 0.8903 -0.2904 0.078 Uiso 1 1 calc R . .
C24 C 0.06347(12) 0.9389(3) -0.1405(2) 0.0741(9) Uani 1 1 d . . .
H24 H 0.0452 1.0227 -0.1118 0.089 Uiso 1 1 calc R . .
C25 C 0.11845(10) 0.8932(3) -0.07736(19) 0.0556(7) Uani 1 1 d . . .
H25 H 0.1378 0.9471 -0.0049 0.067 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 C10 1.416(2) . ?
O1 H1 0.8400 . ?
O2 C18 1.356(2) . ?
O2 C9 1.456(2) . ?
O3 C18 1.217(2) . ?
N1 C6 1.454(2) . ?
N1 C7 1.464(3) . ?
N1 C11 1.469(2) . ?
N2 C18 1.341(2) . ?
N2 C19 1.457(3) . ?
N2 C5 1.472(2) . ?
C1 C5 1.525(3) . ?
C1 C2 1.541(3) . ?
C1 C4 1.552(3) . ?
C1 H1A 1.0000 . ?
C2 C3 1.537(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.536(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.526(3) . ?
C5 C9 1.546(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.532(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.506(2) . ?
C8 C10 1.518(3) . ?
C8 H8 1.0000 . ?
C9 H9 1.0000 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.509(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C17 1.377(3) . ?
C12 C13 1.394(3) . ?
C13 C14 1.386(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.364(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.365(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.402(3) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C19 C20 1.511(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C25 1.375(3) . ?
C20 C21 1.382(3) . ?
C21 C22 1.389(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.370(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.385(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.379(3) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?

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
C10 O1 H1 109.5 . . ?
C18 O2 C9 109.20(13) . . ?
C6 N1 C7 111.33(14) . . ?
C6 N1 C11 112.15(15) . . ?
C7 N1 C11 111.44(15) . . ?
C18 N2 C19 120.50(14) . . ?
C18 N2 C5 112.24(15) . . ?
C19 N2 C5 123.93(14) . . ?
C5 C1 C2 120.42(15) . . ?
C5 C1 C4 118.69(16) . . ?
C2 C1 C4 88.36(15) . . ?
C5 C1 H1A 109.2 . . ?
C2 C1 H1A 109.2 . . ?
C4 C1 H1A 109.2 . . ?
C3 C2 C1 89.32(15) . . ?
C3 C2 H2A 113.8 . . ?
C1 C2 H2A 113.8 . . ?
C3 C2 H2B 113.8 . . ?
C1 C2 H2B 113.8 . . ?
H2A C2 H2B 111.0 . . ?
C4 C3 C2 89.09(15) . . ?
C4 C3 H3A 113.8 . . ?
C2 C3 H3A 113.8 . . ?
C4 C3 H3B 113.8 . . ?
C2 C3 H3B 113.8 . . ?
H3A C3 H3B 111.0 . . ?
C3 C4 C1 88.97(15) . . ?
C3 C4 H4A 113.8 . . ?
C1 C4 H4A 113.8 . . ?
C3 C4 H4B 113.8 . . ?
C1 C4 H4B 113.8 . . ?
H4A C4 H4B 111.0 . . ?
N2 C5 C1 111.25(14) . . ?
N2 C5 C6 110.30(15) . . ?
C1 C5 C6 111.08(14) . . ?
N2 C5 C9 100.22(14) . . ?
C1 C5 C9 113.81(16) . . ?
C6 C5 C9 109.70(15) . . ?
N1 C6 C5 109.43(14) . . ?
N1 C6 H6A 109.8 . . ?
C5 C6 H6A 109.8 . . ?
N1 C6 H6B 109.8 . . ?
C5 C6 H6B 109.8 . . ?
H6A C6 H6B 108.2 . . ?
N1 C7 C8 111.98(15) . . ?
N1 C7 H7A 109.2 . . ?
C8 C7 H7A 109.2 . . ?
N1 C7 H7B 109.2 . . ?
C8 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
C9 C8 C10 112.90(14) . . ?
C9 C8 C7 112.39(16) . . ?
C10 C8 C7 110.88(15) . . ?
C9 C8 H8 106.7 . . ?
C10 C8 H8 106.7 . . ?
C7 C8 H8 106.7 . . ?
O2 C9 C8 110.48(14) . . ?
O2 C9 C5 105.54(14) . . ?
C8 C9 C5 113.22(14) . . ?
O2 C9 H9 109.2 . . ?
C8 C9 H9 109.2 . . ?
C5 C9 H9 109.2 . . ?
O1 C10 C8 112.64(16) . . ?
O1 C10 H10A 109.1 . . ?
C8 C10 H10A 109.1 . . ?
O1 C10 H10B 109.1 . . ?
C8 C10 H10B 109.1 . . ?
H10A C10 H10B 107.8 . . ?
N1 C11 C12 112.09(16) . . ?
N1 C11 H11A 109.2 . . ?
C12 C11 H11A 109.2 . . ?
N1 C11 H11B 109.2 . . ?
C12 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
C17 C12 C13 117.7(2) . . ?
C17 C12 C11 121.94(19) . . ?
C13 C12 C11 120.33(18) . . ?
C14 C13 C12 121.5(2) . . ?
C14 C13 H13 119.2 . . ?
C12 C13 H13 119.2 . . ?
C15 C14 C13 119.6(2) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C14 C15 C16 120.5(2) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 H15 119.7 . . ?
C15 C16 C17 120.0(2) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C12 C17 C16 120.7(2) . . ?
C12 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
O3 C18 N2 127.37(18) . . ?
O3 C18 O2 121.72(16) . . ?
N2 C18 O2 110.88(15) . . ?
N2 C19 C20 115.10(15) . . ?
N2 C19 H19A 108.5 . . ?
C20 C19 H19A 108.5 . . ?
N2 C19 H19B 108.5 . . ?
C20 C19 H19B 108.5 . . ?
H19A C19 H19B 107.5 . . ?
C25 C20 C21 117.97(19) . . ?
C25 C20 C19 119.33(18) . . ?
C21 C20 C19 122.67(18) . . ?
C20 C21 C22 120.8(2) . . ?
C20 C21 H21 119.6 . . ?
C22 C21 H21 119.6 . . ?
C23 C22 C21 120.1(2) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C24 119.9(2) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C25 C24 C23 119.1(3) . . ?
C25 C24 H24 120.5 . . ?
C23 C24 H24 120.5 . . ?
C20 C25 C24 122.1(2) . . ?
C20 C25 H25 118.9 . . ?
C24 C25 H25 118.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 C1 C2 C3 138.18(18) . . . . ?
C4 C1 C2 C3 15.49(15) . . . . ?
C1 C2 C3 C4 -15.65(16) . . . . ?
C2 C3 C4 C1 15.54(15) . . . . ?
C5 C1 C4 C3 -139.68(17) . . . . ?
C2 C1 C4 C3 -15.50(15) . . . . ?
C18 N2 C5 C1 -133.94(16) . . . . ?
C19 N2 C5 C1 66.7(2) . . . . ?
C18 N2 C5 C6 102.33(17) . . . . ?
C19 N2 C5 C6 -57.0(2) . . . . ?
C18 N2 C5 C9 -13.26(18) . . . . ?
C19 N2 C5 C9 -172.62(15) . . . . ?
C2 C1 C5 N2 53.4(2) . . . . ?
C4 C1 C5 N2 159.88(16) . . . . ?
C2 C1 C5 C6 176.69(16) . . . . ?
C4 C1 C5 C6 -76.8(2) . . . . ?
C2 C1 C5 C9 -58.9(2) . . . . ?
C4 C1 C5 C9 47.6(2) . . . . ?
C7 N1 C6 C5 -72.51(18) . . . . ?
C11 N1 C6 C5 161.87(15) . . . . ?
N2 C5 C6 N1 -66.60(18) . . . . ?
C1 C5 C6 N1 169.57(14) . . . . ?
C9 C5 C6 N1 42.87(19) . . . . ?
C6 N1 C7 C8 33.77(19) . . . . ?
C11 N1 C7 C8 159.79(14) . . . . ?
N1 C7 C8 C9 27.8(2) . . . . ?
N1 C7 C8 C10 155.21(14) . . . . ?
C18 O2 C9 C8 -131.77(15) . . . . ?
C18 O2 C9 C5 -9.03(17) . . . . ?
C10 C8 C9 O2 -62.61(19) . . . . ?
C7 C8 C9 O2 63.71(18) . . . . ?
C10 C8 C9 C5 179.26(14) . . . . ?
C7 C8 C9 C5 -54.42(19) . . . . ?
N2 C5 C9 O2 12.78(16) . . . . ?
C1 C5 C9 O2 131.60(14) . . . . ?
C6 C5 C9 O2 -103.26(15) . . . . ?
N2 C5 C9 C8 133.75(15) . . . . ?
C1 C5 C9 C8 -107.43(17) . . . . ?
C6 C5 C9 C8 17.71(19) . . . . ?
C9 C8 C10 O1 -64.7(2) . . . . ?
C7 C8 C10 O1 168.13(14) . . . . ?
C6 N1 C11 C12 -176.61(16) . . . . ?
C7 N1 C11 C12 57.8(2) . . . . ?
N1 C11 C12 C17 73.7(2) . . . . ?
N1 C11 C12 C13 -104.0(2) . . . . ?
C17 C12 C13 C14 0.4(3) . . . . ?
C11 C12 C13 C14 178.17(19) . . . . ?
C12 C13 C14 C15 1.0(3) . . . . ?
C13 C14 C15 C16 -1.3(3) . . . . ?
C14 C15 C16 C17 0.2(3) . . . . ?
C13 C12 C17 C16 -1.5(3) . . . . ?
C11 C12 C17 C16 -179.25(18) . . . . ?
C15 C16 C17 C12 1.3(3) . . . . ?
C19 N2 C18 O3 -13.2(3) . . . . ?
C5 N2 C18 O3 -173.37(17) . . . . ?
C19 N2 C18 O2 168.81(14) . . . . ?
C5 N2 C18 O2 8.65(19) . . . . ?
C9 O2 C18 O3 -177.38(16) . . . . ?
C9 O2 C18 N2 0.74(18) . . . . ?
C18 N2 C19 C20 95.29(19) . . . . ?
C5 N2 C19 C20 -106.95(18) . . . . ?
N2 C19 C20 C25 154.78(17) . . . . ?
N2 C19 C20 C21 -27.1(2) . . . . ?
C25 C20 C21 C22 0.0(3) . . . . ?
C19 C20 C21 C22 -178.17(17) . . . . ?
C20 C21 C22 C23 -0.8(3) . . . . ?
C21 C22 C23 C24 1.1(3) . . . . ?
C22 C23 C24 C25 -0.6(4) . . . . ?
C21 C20 C25 C24 0.5(3) . . . . ?
C19 C20 C25 C24 178.7(2) . . . . ?
C23 C24 C25 C20 -0.2(4) . . . . ?

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 O3 0.84 1.97 2.806(3) 176.7 4_566

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.189
_refine_diff_density_min         -0.183
_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_s1435m
_database_code_depnum_ccdc_archive 'CCDC 1413287'
_audit_update_record             
;
2015-07-16 deposited with the CCDC.
2016-01-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H31 N O4 Si'
_chemical_formula_weight         341.52

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'
Si Si 0.0817 0.0704 '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                   12.1292(18)
_cell_length_b                   14.039(2)
_cell_length_c                   12.6549(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.270(3)
_cell_angle_gamma                90.00
_cell_volume                     1948.7(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2366
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      26.06

_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             744
_exptl_absorpt_coefficient_mu    0.138
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9865
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_sigmaI/netI    0.0687
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         25.02
_reflns_number_total             3437
_reflns_number_gt                2372
_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)+(0.0474P)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         3437
_refine_ls_number_parameters     218
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0408
_refine_ls_wR_factor_ref         0.0961
_refine_ls_wR_factor_gt          0.0901
_refine_ls_goodness_of_fit_ref   0.896
_refine_ls_restrained_S_all      0.896
_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
Si1 Si 0.65788(5) 0.89787(4) 0.22837(5) 0.02515(17) Uani 1 1 d . . .
O1 O 0.95695(12) 0.77742(9) 0.56014(11) 0.0243(3) Uani 1 1 d . . .
O2 O 0.97923(13) 0.93067(9) 0.61579(12) 0.0288(4) Uani 1 1 d . . .
O3 O 0.85512(15) 0.59878(11) 0.51215(14) 0.0420(4) Uani 1 1 d . . .
O4 O 0.79177(11) 0.85698(9) 0.32093(11) 0.0240(3) Uani 1 1 d . . .
N1 N 1.03371(14) 0.87608(12) 0.47174(14) 0.0206(4) Uani 1 1 d . . .
H1N H 1.0333(17) 0.9318(14) 0.4429(16) 0.020(6) Uiso 1 1 d . . .
C1 C 1.09517(17) 0.76329(13) 0.35493(17) 0.0209(5) Uani 1 1 d . . .
H1 H 1.0620 0.7114 0.2955 0.025 Uiso 1 1 calc R . .
C2 C 1.22303(17) 0.73406(15) 0.44685(18) 0.0267(5) Uani 1 1 d . . .
H2A H 1.2478 0.7655 0.5236 0.032 Uiso 1 1 calc R . .
H2B H 1.2357 0.6643 0.4559 0.032 Uiso 1 1 calc R . .
C3 C 1.27652(19) 0.78068(15) 0.36855(19) 0.0311(5) Uani 1 1 d . . .
H3A H 1.2904 0.7355 0.3153 0.037 Uiso 1 1 calc R . .
H3B H 1.3499 0.8199 0.4119 0.037 Uiso 1 1 calc R . .
C4 C 1.15785(17) 0.83905(14) 0.30957(18) 0.0254(5) Uani 1 1 d . . .
H4A H 1.1252 0.8420 0.2234 0.030 Uiso 1 1 calc R . .
H4B H 1.1622 0.9032 0.3435 0.030 Uiso 1 1 calc R . .
C5 C 0.99679(17) 0.79408(13) 0.39302(17) 0.0192(4) Uani 1 1 d . . .
C6 C 0.98209(19) 0.72048(13) 0.47745(17) 0.0219(5) Uani 1 1 d . . .
H6 H 1.0627 0.6887 0.5211 0.026 Uiso 1 1 calc R . .
C7 C 0.98885(17) 0.86909(14) 0.55259(17) 0.0228(5) Uani 1 1 d . . .
C8 C 0.8871(2) 0.64369(14) 0.42638(18) 0.0281(5) Uani 1 1 d . . .
C9 C 0.7661(2) 0.65798(16) 0.4218(2) 0.0369(6) Uani 1 1 d . . .
H9A H 0.7473 0.7211 0.4450 0.044 Uiso 1 1 calc R . .
H9B H 0.6965 0.6259 0.3586 0.044 Uiso 1 1 calc R . .
C10 C 0.9088(2) 0.57305(16) 0.3482(2) 0.0435(6) Uani 1 1 d . . .
H10A H 0.9903 0.5453 0.3894 0.065 Uiso 1 1 calc R . .
H10B H 0.9029 0.6053 0.2773 0.065 Uiso 1 1 calc R . .
H10C H 0.8474 0.5225 0.3270 0.065 Uiso 1 1 calc R . .
C11 C 0.88015(17) 0.81859(14) 0.28583(17) 0.0227(5) Uani 1 1 d . . .
H11A H 0.8983 0.8657 0.2372 0.027 Uiso 1 1 calc R . .
H11B H 0.8471 0.7606 0.2383 0.027 Uiso 1 1 calc R . .
C12 C 0.58439(18) 0.94945(14) 0.32022(18) 0.0256(5) Uani 1 1 d . . .
C13 C 0.44562(19) 0.95465(18) 0.2465(2) 0.0410(6) Uani 1 1 d . . .
H13A H 0.4126 0.8901 0.2265 0.061 Uiso 1 1 calc R . .
H13B H 0.4282 0.9905 0.1747 0.061 Uiso 1 1 calc R . .
H13C H 0.4076 0.9867 0.2914 0.061 Uiso 1 1 calc R . .
C14 C 0.6092(2) 0.88841(18) 0.4283(2) 0.0401(6) Uani 1 1 d . . .
H14A H 0.6972 0.8847 0.4766 0.060 Uiso 1 1 calc R . .
H14B H 0.5766 0.8242 0.4037 0.060 Uiso 1 1 calc R . .
H14C H 0.5695 0.9172 0.4736 0.060 Uiso 1 1 calc R . .
C15 C 0.6328(2) 1.05003(17) 0.3605(2) 0.0470(7) Uani 1 1 d . . .
H15A H 0.5967 1.0751 0.4108 0.071 Uiso 1 1 calc R . .
H15B H 0.6111 1.0914 0.2921 0.071 Uiso 1 1 calc R . .
H15C H 0.7217 1.0479 0.4042 0.071 Uiso 1 1 calc R . .
C16 C 0.5668(2) 0.79786(18) 0.1362(2) 0.0499(7) Uani 1 1 d . . .
H16A H 0.6138 0.7656 0.1002 0.075 Uiso 1 1 calc R . .
H16B H 0.4909 0.8227 0.0750 0.075 Uiso 1 1 calc R . .
H16C H 0.5477 0.7525 0.1848 0.075 Uiso 1 1 calc R . .
C17 C 0.6798(2) 0.99186(17) 0.1354(2) 0.0426(6) Uani 1 1 d . . .
H17A H 0.7431 1.0364 0.1848 0.064 Uiso 1 1 calc R . .
H17B H 0.6031 1.0264 0.0936 0.064 Uiso 1 1 calc R . .
H17C H 0.7047 0.9623 0.0789 0.064 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
Si1 O4 1.6477(14) . ?
Si1 C16 1.858(2) . ?
Si1 C17 1.861(2) . ?
Si1 C12 1.885(2) . ?
O1 C7 1.359(2) . ?
O1 C6 1.449(2) . ?
O2 C7 1.217(2) . ?
O3 C8 1.444(2) . ?
O3 C9 1.452(3) . ?
O4 C11 1.430(2) . ?
N1 C7 1.352(3) . ?
N1 C5 1.462(2) . ?
N1 H1N 0.86(2) . ?
C1 C5 1.528(3) . ?
C1 C2 1.545(3) . ?
C1 C4 1.553(3) . ?
C1 H1 1.0000 . ?
C2 C3 1.543(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.544(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C11 1.524(3) . ?
C5 C6 1.550(3) . ?
C6 C8 1.507(3) . ?
C6 H6 1.0000 . ?
C8 C9 1.458(3) . ?
C8 C10 1.501(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C15 1.531(3) . ?
C12 C14 1.531(3) . ?
C12 C13 1.539(3) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?

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
O4 Si1 C16 108.93(9) . . ?
O4 Si1 C17 109.46(9) . . ?
C16 Si1 C17 110.25(12) . . ?
O4 Si1 C12 106.10(8) . . ?
C16 Si1 C12 111.50(11) . . ?
C17 Si1 C12 110.49(10) . . ?
C7 O1 C6 108.53(15) . . ?
C8 O3 C9 60.44(13) . . ?
C11 O4 Si1 123.56(12) . . ?
C7 N1 C5 110.69(16) . . ?
C7 N1 H1N 117.0(13) . . ?
C5 N1 H1N 118.8(13) . . ?
C5 C1 C2 120.39(16) . . ?
C5 C1 C4 119.63(16) . . ?
C2 C1 C4 88.15(14) . . ?
C5 C1 H1 109.0 . . ?
C2 C1 H1 109.0 . . ?
C4 C1 H1 109.0 . . ?
C3 C2 C1 88.05(15) . . ?
C3 C2 H2A 114.0 . . ?
C1 C2 H2A 114.0 . . ?
C3 C2 H2B 114.0 . . ?
C1 C2 H2B 114.0 . . ?
H2A C2 H2B 111.2 . . ?
C2 C3 C4 88.56(15) . . ?
C2 C3 H3A 113.9 . . ?
C4 C3 H3A 113.9 . . ?
C2 C3 H3B 113.9 . . ?
C4 C3 H3B 113.9 . . ?
H3A C3 H3B 111.1 . . ?
C3 C4 C1 87.72(15) . . ?
C3 C4 H4A 114.0 . . ?
C1 C4 H4A 114.0 . . ?
C3 C4 H4B 114.0 . . ?
C1 C4 H4B 114.0 . . ?
H4A C4 H4B 111.2 . . ?
N1 C5 C11 109.07(15) . . ?
N1 C5 C1 112.61(16) . . ?
C11 C5 C1 109.66(16) . . ?
N1 C5 C6 98.46(15) . . ?
C11 C5 C6 115.33(16) . . ?
C1 C5 C6 111.34(15) . . ?
O1 C6 C8 110.27(16) . . ?
O1 C6 C5 104.57(14) . . ?
C8 C6 C5 118.22(16) . . ?
O1 C6 H6 107.8 . . ?
C8 C6 H6 107.8 . . ?
C5 C6 H6 107.8 . . ?
O2 C7 N1 128.93(19) . . ?
O2 C7 O1 121.11(19) . . ?
N1 C7 O1 109.91(17) . . ?
O3 C8 C9 60.05(14) . . ?
O3 C8 C10 112.68(17) . . ?
C9 C8 C10 121.43(19) . . ?
O3 C8 C6 113.04(16) . . ?
C9 C8 C6 119.39(18) . . ?
C10 C8 C6 116.00(18) . . ?
O3 C9 C8 59.51(13) . . ?
O3 C9 H9A 117.8 . . ?
C8 C9 H9A 117.8 . . ?
O3 C9 H9B 117.8 . . ?
C8 C9 H9B 117.8 . . ?
H9A C9 H9B 115.0 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O4 C11 C5 110.06(15) . . ?
O4 C11 H11A 109.6 . . ?
C5 C11 H11A 109.6 . . ?
O4 C11 H11B 109.6 . . ?
C5 C11 H11B 109.6 . . ?
H11A C11 H11B 108.2 . . ?
C15 C12 C14 108.56(19) . . ?
C15 C12 C13 108.85(18) . . ?
C14 C12 C13 108.36(18) . . ?
C15 C12 Si1 110.13(15) . . ?
C14 C12 Si1 111.80(14) . . ?
C13 C12 Si1 109.08(14) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si1 C16 H16A 109.5 . . ?
Si1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Si1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si1 C17 H17A 109.5 . . ?
Si1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 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
C16 Si1 O4 C11 64.81(17) . . . . ?
C17 Si1 O4 C11 -55.80(17) . . . . ?
C12 Si1 O4 C11 -175.04(14) . . . . ?
C5 C1 C2 C3 -144.17(18) . . . . ?
C4 C1 C2 C3 -20.50(15) . . . . ?
C1 C2 C3 C4 20.63(15) . . . . ?
C2 C3 C4 C1 -20.52(15) . . . . ?
C5 C1 C4 C3 144.82(18) . . . . ?
C2 C1 C4 C3 20.49(15) . . . . ?
C7 N1 C5 C11 93.50(19) . . . . ?
C7 N1 C5 C1 -144.52(16) . . . . ?
C7 N1 C5 C6 -27.10(19) . . . . ?
C2 C1 C5 N1 58.6(2) . . . . ?
C4 C1 C5 N1 -48.3(2) . . . . ?
C2 C1 C5 C11 -179.80(16) . . . . ?
C4 C1 C5 C11 73.3(2) . . . . ?
C2 C1 C5 C6 -50.9(2) . . . . ?
C4 C1 C5 C6 -157.83(16) . . . . ?
C7 O1 C6 C8 -144.68(16) . . . . ?
C7 O1 C6 C5 -16.58(19) . . . . ?
N1 C5 C6 O1 25.25(17) . . . . ?
C11 C5 C6 O1 -90.59(18) . . . . ?
C1 C5 C6 O1 143.64(15) . . . . ?
N1 C5 C6 C8 148.32(17) . . . . ?
C11 C5 C6 C8 32.5(2) . . . . ?
C1 C5 C6 C8 -93.3(2) . . . . ?
C5 N1 C7 O2 -163.6(2) . . . . ?
C5 N1 C7 O1 19.0(2) . . . . ?
C6 O1 C7 O2 -178.13(17) . . . . ?
C6 O1 C7 N1 -0.4(2) . . . . ?
C9 O3 C8 C10 -114.3(2) . . . . ?
C9 O3 C8 C6 111.7(2) . . . . ?
O1 C6 C8 O3 -41.7(2) . . . . ?
C5 C6 C8 O3 -161.88(17) . . . . ?
O1 C6 C8 C9 25.8(3) . . . . ?
C5 C6 C8 C9 -94.4(2) . . . . ?
O1 C6 C8 C10 -174.06(17) . . . . ?
C5 C6 C8 C10 65.8(2) . . . . ?
C10 C8 C9 O3 99.8(2) . . . . ?
C6 C8 C9 O3 -101.2(2) . . . . ?
Si1 O4 C11 C5 175.92(12) . . . . ?
N1 C5 C11 O4 -50.2(2) . . . . ?
C1 C5 C11 O4 -173.93(15) . . . . ?
C6 C5 C11 O4 59.4(2) . . . . ?
O4 Si1 C12 C15 81.56(16) . . . . ?
C16 Si1 C12 C15 -159.97(17) . . . . ?
C17 Si1 C12 C15 -37.00(18) . . . . ?
O4 Si1 C12 C14 -39.21(17) . . . . ?
C16 Si1 C12 C14 79.25(18) . . . . ?
C17 Si1 C12 C14 -157.77(16) . . . . ?
O4 Si1 C12 C13 -159.04(14) . . . . ?
C16 Si1 C12 C13 -40.57(18) . . . . ?
C17 Si1 C12 C13 82.40(17) . . . . ?

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
N1 H1N O2 0.86(2) 2.05(2) 2.909(2) 173.4(19) 3_776

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.045
####################################################################### 
# 
# 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_s1859m
_database_code_depnum_ccdc_archive 'CCDC 1413288'
_audit_update_record             
;
2015-07-16 deposited with the CCDC.
2016-01-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H33 N O5'
_chemical_formula_weight         439.53

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           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                   10.4841(7)
_cell_length_b                   13.2138(9)
_cell_length_c                   33.919(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.4940(10)
_cell_angle_gamma                90.00
_cell_volume                     4690.3(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4109
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      26.01

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1888
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26481
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0865
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         1.20
_diffrn_reflns_theta_max         26.38
_reflns_number_total             9533
_reflns_number_gt                5315
_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)+(0.0521P)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         9533
_refine_ls_number_parameters     581
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_gt           0.0449
_refine_ls_wR_factor_ref         0.1167
_refine_ls_wR_factor_gt          0.0962
_refine_ls_goodness_of_fit_ref   0.870
_refine_ls_restrained_S_all      0.870
_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
O1 O -0.13143(13) 0.35547(10) 0.30383(4) 0.0221(3) Uani 1 1 d . . .
O2 O -0.19757(14) 0.20289(11) 0.32317(4) 0.0265(4) Uani 1 1 d . . .
O3 O 0.12975(15) 0.26639(11) 0.26799(4) 0.0271(4) Uani 1 1 d . . .
H3 H 0.1132 0.2054 0.2725 0.041 Uiso 1 1 calc R . .
O4 O 0.04263(14) 0.63403(11) 0.30779(4) 0.0274(4) Uani 1 1 d . . .
O5 O -0.09524(14) 0.56225(11) 0.21706(4) 0.0252(4) Uani 1 1 d . . .
H5 H -0.1580 0.5539 0.2008 0.038 Uiso 1 1 calc R . .
N1 N 0.00284(16) 0.26242(12) 0.34165(5) 0.0181(4) Uani 1 1 d . . .
C1 C -0.1133(2) 0.26743(16) 0.32319(6) 0.0198(5) Uani 1 1 d . . .
C2 C 0.08521(19) 0.34809(15) 0.33100(6) 0.0186(5) Uani 1 1 d . . .
C3 C -0.01898(19) 0.41959(15) 0.31142(6) 0.0186(5) Uani 1 1 d . . .
H3A H -0.0404 0.4713 0.3315 0.022 Uiso 1 1 calc R . .
C4 C 0.0453(2) 0.16569(15) 0.36015(6) 0.0210(5) Uani 1 1 d . . .
H4A H 0.1384 0.1583 0.3575 0.025 Uiso 1 1 calc R . .
H4B H 0.0023 0.1094 0.3454 0.025 Uiso 1 1 calc R . .
C5 C 0.0188(2) 0.15569(15) 0.40337(6) 0.0217(5) Uani 1 1 d . . .
C6 C 0.1114(2) 0.11427(17) 0.42949(7) 0.0306(6) Uani 1 1 d . . .
H6 H 0.1916 0.0951 0.4203 0.037 Uiso 1 1 calc R . .
C7 C 0.0881(2) 0.10050(19) 0.46899(7) 0.0383(6) Uani 1 1 d . . .
H7 H 0.1524 0.0718 0.4865 0.046 Uiso 1 1 calc R . .
C8 C -0.0271(3) 0.12803(19) 0.48287(7) 0.0386(6) Uani 1 1 d . . .
H8 H -0.0421 0.1201 0.5100 0.046 Uiso 1 1 calc R . .
C9 C -0.1217(2) 0.16762(18) 0.45688(7) 0.0346(6) Uani 1 1 d . . .
H9 H -0.2023 0.1855 0.4662 0.041 Uiso 1 1 calc R . .
C10 C -0.0990(2) 0.18117(17) 0.41759(7) 0.0279(5) Uani 1 1 d . . .
H10 H -0.1644 0.2082 0.4000 0.033 Uiso 1 1 calc R . .
C11 C 0.15032(19) 0.40091(16) 0.36706(6) 0.0223(5) Uani 1 1 d . . .
H11 H 0.1858 0.4668 0.3583 0.027 Uiso 1 1 calc R . .
C12 C 0.2537(2) 0.34796(17) 0.39452(7) 0.0303(6) Uani 1 1 d . . .
H12A H 0.2476 0.2732 0.3944 0.036 Uiso 1 1 calc R . .
H12B H 0.3420 0.3704 0.3904 0.036 Uiso 1 1 calc R . .
C13 C 0.1950(2) 0.39805(19) 0.43015(7) 0.0374(6) Uani 1 1 d . . .
H13A H 0.2412 0.4594 0.4399 0.045 Uiso 1 1 calc R . .
H13B H 0.1809 0.3507 0.4521 0.045 Uiso 1 1 calc R . .
C14 C 0.0732(2) 0.42086(17) 0.40373(7) 0.0300(6) Uani 1 1 d . . .
H14A H 0.0426 0.4914 0.4058 0.036 Uiso 1 1 calc R . .
H14B H 0.0030 0.3720 0.4069 0.036 Uiso 1 1 calc R . .
C15 C 0.1854(2) 0.31157(16) 0.30273(6) 0.0230(5) Uani 1 1 d . . .
H15A H 0.2381 0.3699 0.2953 0.028 Uiso 1 1 calc R . .
H15B H 0.2426 0.2619 0.3167 0.028 Uiso 1 1 calc R . .
C16 C 0.00755(19) 0.47587(15) 0.27319(6) 0.0198(5) Uani 1 1 d . . .
H16 H 0.0481 0.4276 0.2550 0.024 Uiso 1 1 calc R . .
C17 C 0.0977(2) 0.56575(16) 0.28084(6) 0.0227(5) Uani 1 1 d . . .
H17A H 0.1815 0.5416 0.2921 0.027 Uiso 1 1 calc R . .
H17B H 0.1114 0.6010 0.2557 0.027 Uiso 1 1 calc R . .
C18 C 0.1019(2) 0.73158(16) 0.30749(7) 0.0304(6) Uani 1 1 d . . .
H18A H 0.0876 0.7626 0.2810 0.036 Uiso 1 1 calc R . .
H18B H 0.1952 0.7245 0.3133 0.036 Uiso 1 1 calc R . .
C19 C 0.0463(2) 0.79840(17) 0.33801(8) 0.0349(6) Uani 1 1 d . . .
H19A H -0.0480 0.7935 0.3355 0.042 Uiso 1 1 calc R . .
H19B H 0.0700 0.8696 0.3330 0.042 Uiso 1 1 calc R . .
C20 C 0.0933(2) 0.76936(19) 0.37981(8) 0.0378(7) Uani 1 1 d . . .
C21 C 0.0262(3) 0.7032(2) 0.40232(9) 0.0549(8) Uani 1 1 d . . .
H21 H -0.0533 0.6771 0.3918 0.066 Uiso 1 1 calc R . .
C22 C 0.0719(4) 0.6736(2) 0.43997(10) 0.0679(10) Uani 1 1 d . . .
H22 H 0.0226 0.6295 0.4551 0.082 Uiso 1 1 calc R . .
C23 C 0.1881(4) 0.7082(3) 0.45529(10) 0.0659(10) Uani 1 1 d . . .
H23 H 0.2212 0.6865 0.4806 0.079 Uiso 1 1 calc R . .
C24 C 0.2554(3) 0.7743(3) 0.43348(10) 0.0780(12) Uani 1 1 d . . .
H24 H 0.3355 0.7993 0.4438 0.094 Uiso 1 1 calc R . .
C25 C 0.2074(3) 0.8051(3) 0.39639(9) 0.0649(10) Uani 1 1 d . . .
H25 H 0.2548 0.8523 0.3820 0.078 Uiso 1 1 calc R . .
C26 C -0.1191(2) 0.51218(16) 0.25333(6) 0.0222(5) Uani 1 1 d . . .
H26A H -0.1767 0.4537 0.2480 0.027 Uiso 1 1 calc R . .
H26B H -0.1614 0.5594 0.2711 0.027 Uiso 1 1 calc R . .
O6 O 0.62002(13) 0.40051(10) 0.18884(4) 0.0224(4) Uani 1 1 d . . .
O7 O 0.68971(14) 0.55027(11) 0.16741(4) 0.0278(4) Uani 1 1 d . . .
O8 O 0.38790(15) 0.50250(11) 0.22984(4) 0.0276(4) Uani 1 1 d . . .
H8A H 0.4022 0.5638 0.2253 0.041 Uiso 1 1 calc R . .
O9 O 0.44723(14) 0.12852(10) 0.18798(4) 0.0259(4) Uani 1 1 d . . .
O10 O 0.57856(14) 0.20815(11) 0.28045(4) 0.0243(4) Uani 1 1 d . . .
H10A H 0.6445 0.2112 0.2958 0.036 Uiso 1 1 calc R . .
N2 N 0.48505(16) 0.49504(12) 0.15127(5) 0.0184(4) Uani 1 1 d . . .
C27 C 0.6035(2) 0.48802(16) 0.16897(6) 0.0206(5) Uani 1 1 d . . .
C28 C 0.39923(19) 0.41535(15) 0.16605(6) 0.0179(5) Uani 1 1 d . . .
C29 C 0.50296(19) 0.34013(15) 0.18364(6) 0.0181(5) Uani 1 1 d . . .
H29 H 0.5169 0.2873 0.1632 0.022 Uiso 1 1 calc R . .
C30 C 0.4432(2) 0.59603(15) 0.13769(6) 0.0216(5) Uani 1 1 d . . .
H30A H 0.4822 0.6468 0.1562 0.026 Uiso 1 1 calc R . .
H30B H 0.3494 0.6003 0.1393 0.026 Uiso 1 1 calc R . .
C31 C 0.47500(19) 0.62498(15) 0.09602(6) 0.0197(5) Uani 1 1 d . . .
C32 C 0.4460(2) 0.72308(16) 0.08367(7) 0.0257(5) Uani 1 1 d . . .
H32 H 0.4061 0.7679 0.1011 0.031 Uiso 1 1 calc R . .
C33 C 0.4740(2) 0.75669(18) 0.04662(7) 0.0317(6) Uani 1 1 d . . .
H33 H 0.4535 0.8241 0.0388 0.038 Uiso 1 1 calc R . .
C34 C 0.5318(2) 0.69259(18) 0.02098(7) 0.0309(6) Uani 1 1 d . . .
H34 H 0.5512 0.7154 -0.0045 0.037 Uiso 1 1 calc R . .
C35 C 0.5613(2) 0.59464(18) 0.03286(7) 0.0316(6) Uani 1 1 d . . .
H35 H 0.6009 0.5500 0.0154 0.038 Uiso 1 1 calc R . .
C36 C 0.5334(2) 0.56129(17) 0.07023(7) 0.0281(6) Uani 1 1 d . . .
H36 H 0.5545 0.4941 0.0781 0.034 Uiso 1 1 calc R . .
C37 C 0.3152(2) 0.36310(16) 0.13347(6) 0.0213(5) Uani 1 1 d . . .
H37 H 0.2612 0.3117 0.1462 0.026 Uiso 1 1 calc R . .
C38 C 0.2279(2) 0.42323(17) 0.10303(7) 0.0296(6) Uani 1 1 d . . .
H38A H 0.1363 0.4223 0.1086 0.036 Uiso 1 1 calc R . .
H38B H 0.2575 0.4931 0.0984 0.036 Uiso 1 1 calc R . .
C39 C 0.2630(2) 0.3476(2) 0.07111(8) 0.0479(7) Uani 1 1 d . . .
H39A H 0.2882 0.3799 0.0464 0.057 Uiso 1 1 calc R . .
H39B H 0.1974 0.2947 0.0654 0.057 Uiso 1 1 calc R . .
C40 C 0.3774(2) 0.31149(19) 0.09848(7) 0.0333(6) Uani 1 1 d . . .
H40A H 0.4602 0.3416 0.0922 0.040 Uiso 1 1 calc R . .
H40B H 0.3841 0.2370 0.1009 0.040 Uiso 1 1 calc R . .
C41 C 0.3145(2) 0.45965(16) 0.19724(6) 0.0213(5) Uani 1 1 d . . .
H41A H 0.2585 0.5125 0.1848 0.026 Uiso 1 1 calc R . .
H41B H 0.2592 0.4055 0.2070 0.026 Uiso 1 1 calc R . .
C42 C 0.47875(19) 0.28590(15) 0.22247(6) 0.0177(5) Uani 1 1 d . . .
H42 H 0.4367 0.3346 0.2402 0.021 Uiso 1 1 calc R . .
C43 C 0.3906(2) 0.19519(15) 0.21522(6) 0.0195(5) Uani 1 1 d . . .
H43A H 0.3788 0.1595 0.2404 0.023 Uiso 1 1 calc R . .
H43B H 0.3058 0.2181 0.2042 0.023 Uiso 1 1 calc R . .
C44 C 0.3941(2) 0.02966(16) 0.18810(7) 0.0280(6) Uani 1 1 d . . .
H44A H 0.3011 0.0328 0.1811 0.034 Uiso 1 1 calc R . .
H44B H 0.4072 -0.0006 0.2147 0.034 Uiso 1 1 calc R . .
C45 C 0.4596(2) -0.03437(17) 0.15818(7) 0.0304(6) Uani 1 1 d . . .
H45A H 0.4364 -0.1062 0.1619 0.037 Uiso 1 1 calc R . .
H45B H 0.5533 -0.0283 0.1632 0.037 Uiso 1 1 calc R . .
C46 C 0.4243(2) -0.00444(16) 0.11563(7) 0.0269(5) Uani 1 1 d . . .
C47 C 0.3022(2) -0.02495(19) 0.09859(8) 0.0362(6) Uani 1 1 d . . .
H47 H 0.2409 -0.0570 0.1139 0.043 Uiso 1 1 calc R . .
C48 C 0.2693(3) 0.0008(2) 0.05966(8) 0.0465(7) Uani 1 1 d . . .
H48 H 0.1863 -0.0140 0.0484 0.056 Uiso 1 1 calc R . .
C49 C 0.3593(3) 0.04879(19) 0.03691(8) 0.0424(7) Uani 1 1 d . . .
H49 H 0.3376 0.0669 0.0102 0.051 Uiso 1 1 calc R . .
C50 C 0.4774(3) 0.06886(18) 0.05351(8) 0.0387(7) Uani 1 1 d . . .
H50 H 0.5386 0.1007 0.0381 0.046 Uiso 1 1 calc R . .
C51 C 0.5110(2) 0.04383(16) 0.09265(7) 0.0305(6) Uani 1 1 d . . .
H51 H 0.5940 0.0599 0.1037 0.037 Uiso 1 1 calc R . .
C52 C 0.6046(2) 0.25138(16) 0.24317(6) 0.0216(5) Uani 1 1 d . . .
H52A H 0.6461 0.2006 0.2267 0.026 Uiso 1 1 calc R . .
H52B H 0.6632 0.3098 0.2471 0.026 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 1.344(2) . ?
O1 C3 1.462(2) . ?
O2 C1 1.228(2) . ?
O3 C15 1.415(2) . ?
O3 H3 0.8400 . ?
O4 C17 1.431(2) . ?
O4 C18 1.431(2) . ?
O5 C26 1.432(2) . ?
O5 H5 0.8400 . ?
N1 C1 1.336(3) . ?
N1 C4 1.480(2) . ?
N1 C2 1.482(2) . ?
C2 C11 1.532(3) . ?
C2 C15 1.542(3) . ?
C2 C3 1.562(3) . ?
C3 C16 1.535(3) . ?
C3 H3A 1.0000 . ?
C4 C5 1.514(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.386(3) . ?
C5 C10 1.394(3) . ?
C6 C7 1.388(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.372(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.388(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.379(3) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C14 1.547(3) . ?
C11 C12 1.552(3) . ?
C11 H11 1.0000 . ?
C12 C13 1.539(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.544(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C26 1.529(3) . ?
C16 C17 1.530(3) . ?
C16 H16 1.0000 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.505(3) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.521(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C25 1.374(4) . ?
C20 C21 1.382(4) . ?
C21 C22 1.392(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.373(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.368(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.387(4) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
O6 C27 1.345(2) . ?
O6 C29 1.465(2) . ?
O7 C27 1.226(2) . ?
O8 C41 1.425(2) . ?
O8 H8A 0.8400 . ?
O9 C44 1.420(2) . ?
O9 C43 1.432(2) . ?
O10 C52 1.429(2) . ?
O10 H10A 0.8400 . ?
N2 C27 1.349(3) . ?
N2 C30 1.470(2) . ?
N2 C28 1.491(2) . ?
C28 C37 1.535(3) . ?
C28 C41 1.538(3) . ?
C28 C29 1.564(3) . ?
C29 C42 1.534(3) . ?
C29 H29 1.0000 . ?
C30 C31 1.521(3) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C36 1.383(3) . ?
C31 C32 1.390(3) . ?
C32 C33 1.381(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.380(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.385(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.390(3) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C40 1.547(3) . ?
C37 C38 1.555(3) . ?
C37 H37 1.0000 . ?
C38 C39 1.535(3) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.547(3) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.524(3) . ?
C42 C52 1.526(3) . ?
C42 H42 1.0000 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.517(3) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C46 1.520(3) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C51 1.388(3) . ?
C46 C47 1.399(3) . ?
C47 C48 1.387(3) . ?
C47 H47 0.9500 . ?
C48 C49 1.405(4) . ?
C48 H48 0.9500 . ?
C49 C50 1.355(4) . ?
C49 H49 0.9500 . ?
C50 C51 1.392(3) . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?

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 C3 109.09(16) . . ?
C15 O3 H3 109.5 . . ?
C17 O4 C18 111.78(15) . . ?
C26 O5 H5 109.5 . . ?
C1 N1 C4 118.89(17) . . ?
C1 N1 C2 112.07(17) . . ?
C4 N1 C2 126.75(16) . . ?
O2 C1 N1 126.94(19) . . ?
O2 C1 O1 121.35(19) . . ?
N1 C1 O1 111.70(18) . . ?
N1 C2 C11 113.03(17) . . ?
N1 C2 C15 109.98(16) . . ?
C11 C2 C15 110.59(17) . . ?
N1 C2 C3 99.38(15) . . ?
C11 C2 C3 109.27(16) . . ?
C15 C2 C3 114.22(17) . . ?
O1 C3 C16 108.53(16) . . ?
O1 C3 C2 105.07(15) . . ?
C16 C3 C2 119.63(17) . . ?
O1 C3 H3A 107.7 . . ?
C16 C3 H3A 107.7 . . ?
C2 C3 H3A 107.7 . . ?
N1 C4 C5 114.68(17) . . ?
N1 C4 H4A 108.6 . . ?
C5 C4 H4A 108.6 . . ?
N1 C4 H4B 108.6 . . ?
C5 C4 H4B 108.6 . . ?
H4A C4 H4B 107.6 . . ?
C6 C5 C10 118.3(2) . . ?
C6 C5 C4 119.4(2) . . ?
C10 C5 C4 122.16(19) . . ?
C5 C6 C7 120.8(2) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 H6 119.6 . . ?
C8 C7 C6 120.4(2) . . ?
C8 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C7 C8 C9 119.4(2) . . ?
C7 C8 H8 120.3 . . ?
C9 C8 H8 120.3 . . ?
C10 C9 C8 120.3(2) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C9 C10 C5 120.8(2) . . ?
C9 C10 H10 119.6 . . ?
C5 C10 H10 119.6 . . ?
C2 C11 C14 119.37(18) . . ?
C2 C11 C12 122.31(18) . . ?
C14 C11 C12 88.53(17) . . ?
C2 C11 H11 108.3 . . ?
C14 C11 H11 108.3 . . ?
C12 C11 H11 108.3 . . ?
C13 C12 C11 88.83(17) . . ?
C13 C12 H12A 113.8 . . ?
C11 C12 H12A 113.8 . . ?
C13 C12 H12B 113.8 . . ?
C11 C12 H12B 113.8 . . ?
H12A C12 H12B 111.1 . . ?
C12 C13 C14 89.08(17) . . ?
C12 C13 H13A 113.8 . . ?
C14 C13 H13A 113.8 . . ?
C12 C13 H13B 113.8 . . ?
C14 C13 H13B 113.8 . . ?
H13A C13 H13B 111.0 . . ?
C13 C14 C11 88.82(17) . . ?
C13 C14 H14A 113.8 . . ?
C11 C14 H14A 113.8 . . ?
C13 C14 H14B 113.8 . . ?
C11 C14 H14B 113.8 . . ?
H14A C14 H14B 111.1 . . ?
O3 C15 C2 112.83(17) . . ?
O3 C15 H15A 109.0 . . ?
C2 C15 H15A 109.0 . . ?
O3 C15 H15B 109.0 . . ?
C2 C15 H15B 109.0 . . ?
H15A C15 H15B 107.8 . . ?
C26 C16 C17 110.01(17) . . ?
C26 C16 C3 109.08(17) . . ?
C17 C16 C3 112.01(17) . . ?
C26 C16 H16 108.6 . . ?
C17 C16 H16 108.6 . . ?
C3 C16 H16 108.6 . . ?
O4 C17 C16 109.17(16) . . ?
O4 C17 H17A 109.8 . . ?
C16 C17 H17A 109.8 . . ?
O4 C17 H17B 109.8 . . ?
C16 C17 H17B 109.8 . . ?
H17A C17 H17B 108.3 . . ?
O4 C18 C19 109.71(18) . . ?
O4 C18 H18A 109.7 . . ?
C19 C18 H18A 109.7 . . ?
O4 C18 H18B 109.7 . . ?
C19 C18 H18B 109.7 . . ?
H18A C18 H18B 108.2 . . ?
C18 C19 C20 112.1(2) . . ?
C18 C19 H19A 109.2 . . ?
C20 C19 H19A 109.2 . . ?
C18 C19 H19B 109.2 . . ?
C20 C19 H19B 109.2 . . ?
H19A C19 H19B 107.9 . . ?
C25 C20 C21 116.8(3) . . ?
C25 C20 C19 121.3(3) . . ?
C21 C20 C19 121.9(3) . . ?
C20 C21 C22 121.7(3) . . ?
C20 C21 H21 119.1 . . ?
C22 C21 H21 119.1 . . ?
C23 C22 C21 120.1(3) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C24 C23 C22 118.9(3) . . ?
C24 C23 H23 120.6 . . ?
C22 C23 H23 120.6 . . ?
C23 C24 C25 120.5(3) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
C20 C25 C24 121.9(3) . . ?
C20 C25 H25 119.0 . . ?
C24 C25 H25 119.0 . . ?
O5 C26 C16 109.31(17) . . ?
O5 C26 H26A 109.8 . . ?
C16 C26 H26A 109.8 . . ?
O5 C26 H26B 109.8 . . ?
C16 C26 H26B 109.8 . . ?
H26A C26 H26B 108.3 . . ?
C27 O6 C29 109.05(16) . . ?
C41 O8 H8A 109.5 . . ?
C44 O9 C43 112.70(15) . . ?
C52 O10 H10A 109.5 . . ?
C27 N2 C30 116.81(17) . . ?
C27 N2 C28 111.08(16) . . ?
C30 N2 C28 124.85(16) . . ?
O7 C27 O6 121.71(19) . . ?
O7 C27 N2 126.59(19) . . ?
O6 C27 N2 111.68(17) . . ?
N2 C28 C37 114.03(17) . . ?
N2 C28 C41 110.37(16) . . ?
C37 C28 C41 109.64(17) . . ?
N2 C28 C29 99.04(15) . . ?
C37 C28 C29 110.12(16) . . ?
C41 C28 C29 113.37(17) . . ?
O6 C29 C42 109.40(16) . . ?
O6 C29 C28 104.93(15) . . ?
C42 C29 C28 118.47(17) . . ?
O6 C29 H29 107.9 . . ?
C42 C29 H29 107.9 . . ?
C28 C29 H29 107.9 . . ?
N2 C30 C31 116.19(16) . . ?
N2 C30 H30A 108.2 . . ?
C31 C30 H30A 108.2 . . ?
N2 C30 H30B 108.2 . . ?
C31 C30 H30B 108.2 . . ?
H30A C30 H30B 107.4 . . ?
C36 C31 C32 118.3(2) . . ?
C36 C31 C30 124.41(19) . . ?
C32 C31 C30 117.26(19) . . ?
C33 C32 C31 121.3(2) . . ?
C33 C32 H32 119.4 . . ?
C31 C32 H32 119.4 . . ?
C34 C33 C32 120.1(2) . . ?
C34 C33 H33 119.9 . . ?
C32 C33 H33 119.9 . . ?
C33 C34 C35 119.3(2) . . ?
C33 C34 H34 120.4 . . ?
C35 C34 H34 120.4 . . ?
C34 C35 C36 120.4(2) . . ?
C34 C35 H35 119.8 . . ?
C36 C35 H35 119.8 . . ?
C31 C36 C35 120.6(2) . . ?
C31 C36 H36 119.7 . . ?
C35 C36 H36 119.7 . . ?
C28 C37 C40 119.99(18) . . ?
C28 C37 C38 122.47(18) . . ?
C40 C37 C38 88.54(17) . . ?
C28 C37 H37 108.0 . . ?
C40 C37 H37 108.0 . . ?
C38 C37 H37 108.0 . . ?
C39 C38 C37 88.79(17) . . ?
C39 C38 H38A 113.9 . . ?
C37 C38 H38A 113.9 . . ?
C39 C38 H38B 113.9 . . ?
C37 C38 H38B 113.9 . . ?
H38A C38 H38B 111.1 . . ?
C38 C39 C40 89.30(18) . . ?
C38 C39 H39A 113.8 . . ?
C40 C39 H39A 113.8 . . ?
C38 C39 H39B 113.8 . . ?
C40 C39 H39B 113.8 . . ?
H39A C39 H39B 111.0 . . ?
C39 C40 C37 88.66(18) . . ?
C39 C40 H40A 113.9 . . ?
C37 C40 H40A 113.9 . . ?
C39 C40 H40B 113.9 . . ?
C37 C40 H40B 113.9 . . ?
H40A C40 H40B 111.1 . . ?
O8 C41 C28 112.20(17) . . ?
O8 C41 H41A 109.2 . . ?
C28 C41 H41A 109.2 . . ?
O8 C41 H41B 109.2 . . ?
C28 C41 H41B 109.2 . . ?
H41A C41 H41B 107.9 . . ?
C43 C42 C52 109.75(17) . . ?
C43 C42 C29 111.06(17) . . ?
C52 C42 C29 110.55(16) . . ?
C43 C42 H42 108.5 . . ?
C52 C42 H42 108.5 . . ?
C29 C42 H42 108.5 . . ?
O9 C43 C42 108.45(16) . . ?
O9 C43 H43A 110.0 . . ?
C42 C43 H43A 110.0 . . ?
O9 C43 H43B 110.0 . . ?
C42 C43 H43B 110.0 . . ?
H43A C43 H43B 108.4 . . ?
O9 C44 C45 108.51(17) . . ?
O9 C44 H44A 110.0 . . ?
C45 C44 H44A 110.0 . . ?
O9 C44 H44B 110.0 . . ?
C45 C44 H44B 110.0 . . ?
H44A C44 H44B 108.4 . . ?
C44 C45 C46 113.32(19) . . ?
C44 C45 H45A 108.9 . . ?
C46 C45 H45A 108.9 . . ?
C44 C45 H45B 108.9 . . ?
C46 C45 H45B 108.9 . . ?
H45A C45 H45B 107.7 . . ?
C51 C46 C47 118.1(2) . . ?
C51 C46 C45 121.5(2) . . ?
C47 C46 C45 120.4(2) . . ?
C48 C47 C46 120.9(2) . . ?
C48 C47 H47 119.5 . . ?
C46 C47 H47 119.5 . . ?
C47 C48 C49 119.9(3) . . ?
C47 C48 H48 120.1 . . ?
C49 C48 H48 120.1 . . ?
C50 C49 C48 119.1(2) . . ?
C50 C49 H49 120.4 . . ?
C48 C49 H49 120.4 . . ?
C49 C50 C51 121.5(2) . . ?
C49 C50 H50 119.3 . . ?
C51 C50 H50 119.3 . . ?
C46 C51 C50 120.5(2) . . ?
C46 C51 H51 119.7 . . ?
C50 C51 H51 119.7 . . ?
O10 C52 C42 108.67(16) . . ?
O10 C52 H52A 110.0 . . ?
C42 C52 H52A 110.0 . . ?
O10 C52 H52B 110.0 . . ?
C42 C52 H52B 110.0 . . ?
H52A C52 H52B 108.3 . . ?

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
C4 N1 C1 O2 8.6(3) . . . . ?
C2 N1 C1 O2 172.6(2) . . . . ?
C4 N1 C1 O1 -172.21(17) . . . . ?
C2 N1 C1 O1 -8.2(2) . . . . ?
C3 O1 C1 O2 175.98(19) . . . . ?
C3 O1 C1 N1 -3.2(2) . . . . ?
C1 N1 C2 C11 130.45(18) . . . . ?
C4 N1 C2 C11 -67.1(2) . . . . ?
C1 N1 C2 C15 -105.4(2) . . . . ?
C4 N1 C2 C15 57.0(3) . . . . ?
C1 N1 C2 C3 14.8(2) . . . . ?
C4 N1 C2 C3 177.20(18) . . . . ?
C1 O1 C3 C16 141.47(17) . . . . ?
C1 O1 C3 C2 12.4(2) . . . . ?
N1 C2 C3 O1 -15.54(19) . . . . ?
C11 C2 C3 O1 -134.08(17) . . . . ?
C15 C2 C3 O1 101.47(18) . . . . ?
N1 C2 C3 C16 -137.66(18) . . . . ?
C11 C2 C3 C16 103.8(2) . . . . ?
C15 C2 C3 C16 -20.7(3) . . . . ?
C1 N1 C4 C5 -92.9(2) . . . . ?
C2 N1 C4 C5 105.7(2) . . . . ?
N1 C4 C5 C6 -137.9(2) . . . . ?
N1 C4 C5 C10 46.1(3) . . . . ?
C10 C5 C6 C7 -1.3(3) . . . . ?
C4 C5 C6 C7 -177.5(2) . . . . ?
C5 C6 C7 C8 -0.2(4) . . . . ?
C6 C7 C8 C9 1.5(4) . . . . ?
C7 C8 C9 C10 -1.4(4) . . . . ?
C8 C9 C10 C5 -0.1(4) . . . . ?
C6 C5 C10 C9 1.5(3) . . . . ?
C4 C5 C10 C9 177.5(2) . . . . ?
N1 C2 C11 C14 -41.7(3) . . . . ?
C15 C2 C11 C14 -165.53(18) . . . . ?
C3 C2 C11 C14 67.9(2) . . . . ?
N1 C2 C11 C12 67.0(2) . . . . ?
C15 C2 C11 C12 -56.8(3) . . . . ?
C3 C2 C11 C12 176.65(18) . . . . ?
C2 C11 C12 C13 -140.7(2) . . . . ?
C14 C11 C12 C13 -16.37(17) . . . . ?
C11 C12 C13 C14 16.39(17) . . . . ?
C12 C13 C14 C11 -16.44(17) . . . . ?
C2 C11 C14 C13 143.12(19) . . . . ?
C12 C11 C14 C13 16.31(17) . . . . ?
N1 C2 C15 O3 57.2(2) . . . . ?
C11 C2 C15 O3 -177.22(17) . . . . ?
C3 C2 C15 O3 -53.5(2) . . . . ?
O1 C3 C16 C26 41.7(2) . . . . ?
C2 C3 C16 C26 162.10(18) . . . . ?
O1 C3 C16 C17 163.73(16) . . . . ?
C2 C3 C16 C17 -75.9(2) . . . . ?
C18 O4 C17 C16 -163.27(17) . . . . ?
C26 C16 C17 O4 63.0(2) . . . . ?
C3 C16 C17 O4 -58.5(2) . . . . ?
C17 O4 C18 C19 -176.54(19) . . . . ?
O4 C18 C19 C20 73.7(3) . . . . ?
C18 C19 C20 C25 84.5(3) . . . . ?
C18 C19 C20 C21 -93.0(3) . . . . ?
C25 C20 C21 C22 -0.3(4) . . . . ?
C19 C20 C21 C22 177.4(3) . . . . ?
C20 C21 C22 C23 -1.7(5) . . . . ?
C21 C22 C23 C24 2.1(5) . . . . ?
C22 C23 C24 C25 -0.6(5) . . . . ?
C21 C20 C25 C24 1.9(5) . . . . ?
C19 C20 C25 C24 -175.8(3) . . . . ?
C23 C24 C25 C20 -1.5(5) . . . . ?
C17 C16 C26 O5 58.4(2) . . . . ?
C3 C16 C26 O5 -178.36(16) . . . . ?
C29 O6 C27 O7 -177.13(19) . . . . ?
C29 O6 C27 N2 1.5(2) . . . . ?
C30 N2 C27 O7 -17.2(3) . . . . ?
C28 N2 C27 O7 -169.0(2) . . . . ?
C30 N2 C27 O6 164.26(16) . . . . ?
C28 N2 C27 O6 12.5(2) . . . . ?
C27 N2 C28 C37 -136.25(18) . . . . ?
C30 N2 C28 C37 74.7(2) . . . . ?
C27 N2 C28 C41 99.8(2) . . . . ?
C30 N2 C28 C41 -49.2(3) . . . . ?
C27 N2 C28 C29 -19.3(2) . . . . ?
C30 N2 C28 C29 -168.38(18) . . . . ?
C27 O6 C29 C42 -141.82(17) . . . . ?
C27 O6 C29 C28 -13.7(2) . . . . ?
N2 C28 C29 O6 18.99(18) . . . . ?
C37 C28 C29 O6 138.83(16) . . . . ?
C41 C28 C29 O6 -97.93(18) . . . . ?
N2 C28 C29 C42 141.37(17) . . . . ?
C37 C28 C29 C42 -98.8(2) . . . . ?
C41 C28 C29 C42 24.5(2) . . . . ?
C27 N2 C30 C31 88.8(2) . . . . ?
C28 N2 C30 C31 -123.7(2) . . . . ?
N2 C30 C31 C36 3.5(3) . . . . ?
N2 C30 C31 C32 -174.77(18) . . . . ?
C36 C31 C32 C33 0.2(3) . . . . ?
C30 C31 C32 C33 178.6(2) . . . . ?
C31 C32 C33 C34 0.1(4) . . . . ?
C32 C33 C34 C35 -0.1(4) . . . . ?
C33 C34 C35 C36 -0.2(4) . . . . ?
C32 C31 C36 C35 -0.4(3) . . . . ?
C30 C31 C36 C35 -178.7(2) . . . . ?
C34 C35 C36 C31 0.4(4) . . . . ?
N2 C28 C37 C40 56.1(3) . . . . ?
C41 C28 C37 C40 -179.62(19) . . . . ?
C29 C28 C37 C40 -54.2(2) . . . . ?
N2 C28 C37 C38 -53.4(3) . . . . ?
C41 C28 C37 C38 71.0(2) . . . . ?
C29 C28 C37 C38 -163.65(18) . . . . ?
C28 C37 C38 C39 141.5(2) . . . . ?
C40 C37 C38 C39 16.32(18) . . . . ?
C37 C38 C39 C40 -16.32(18) . . . . ?
C38 C39 C40 C37 16.41(18) . . . . ?
C28 C37 C40 C39 -143.5(2) . . . . ?
C38 C37 C40 C39 -16.20(18) . . . . ?
N2 C28 C41 O8 -58.0(2) . . . . ?
C37 C28 C41 O8 175.53(16) . . . . ?
C29 C28 C41 O8 52.0(2) . . . . ?
O6 C29 C42 C43 -159.28(16) . . . . ?
C28 C29 C42 C43 80.6(2) . . . . ?
O6 C29 C42 C52 -37.2(2) . . . . ?
C28 C29 C42 C52 -157.30(17) . . . . ?
C44 O9 C43 C42 162.52(17) . . . . ?
C52 C42 C43 O9 -65.2(2) . . . . ?
C29 C42 C43 O9 57.4(2) . . . . ?
C43 O9 C44 C45 179.56(18) . . . . ?
O9 C44 C45 C46 -70.2(2) . . . . ?
C44 C45 C46 C51 108.7(2) . . . . ?
C44 C45 C46 C47 -71.2(3) . . . . ?
C51 C46 C47 C48 1.0(3) . . . . ?
C45 C46 C47 C48 -179.2(2) . . . . ?
C46 C47 C48 C49 -0.4(4) . . . . ?
C47 C48 C49 C50 0.2(4) . . . . ?
C48 C49 C50 C51 -0.6(4) . . . . ?
C47 C46 C51 C50 -1.3(3) . . . . ?
C45 C46 C51 C50 178.8(2) . . . . ?
C49 C50 C51 C46 1.2(4) . . . . ?
C43 C42 C52 O10 -61.4(2) . . . . ?
C29 C42 C52 O10 175.74(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
O3 H3 O5 0.84 1.94 2.772(2) 173.7 2_545
O5 H5 O7 0.84 1.90 2.735(2) 172.2 1_455
O8 H8A O10 0.84 1.93 2.765(2) 173.2 2_655
O10 H10A O2 0.84 1.85 2.683(2) 169.8 1_655

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        26.38
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.135

####################################################################### 
# 
# 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_s3081
_database_code_depnum_ccdc_archive 'CCDC 1424601'
_audit_update_record             
;
2015-09-15 deposited with the CCDC.
2016-01-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H28 N2 O3'
_chemical_formula_weight         392.48

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           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                   11.874(3)
_cell_length_b                   18.239(4)
_cell_length_c                   9.829(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.881(4)
_cell_angle_gamma                90.00
_cell_volume                     2120.8(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    962
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      22.33

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             840
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12048
_diffrn_reflns_av_R_equivalents  0.0726
_diffrn_reflns_av_sigmaI/netI    0.0979
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.72
_diffrn_reflns_theta_max         26.50
_reflns_number_total             4328
_reflns_number_gt                2650
_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)+(0.0335P)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         4328
_refine_ls_number_parameters     266
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0534
_refine_ls_wR_factor_ref         0.1032
_refine_ls_wR_factor_gt          0.0905
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_restrained_S_all      0.928
_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 0.37556(11) 0.09497(7) -0.06182(13) 0.0262(4) Uani 1 1 d . . .
O2 O 0.51105(11) 0.16443(7) -0.14217(14) 0.0309(4) Uani 1 1 d . . .
O3 O 0.08214(11) -0.00050(8) 0.19545(15) 0.0338(4) Uani 1 1 d . . .
N1 N 0.49690(12) 0.15148(8) 0.08976(16) 0.0210(4) Uani 1 1 d . . .
N2 N 0.29785(15) 0.23565(9) 0.10665(18) 0.0268(4) Uani 1 1 d . . .
H2N H 0.3621(17) 0.2605(11) 0.098(2) 0.039(7) Uiso 1 1 d . . .
C1 C 0.40983(15) 0.12369(10) 0.1750(2) 0.0214(5) Uani 1 1 d . . .
C2 C 0.35062(16) 0.06856(11) 0.07127(18) 0.0223(5) Uani 1 1 d . . .
H2 H 0.3884 0.0199 0.0863 0.027 Uiso 1 1 calc R . .
C3 C 0.46622(17) 0.13995(11) -0.0454(2) 0.0244(5) Uani 1 1 d . . .
C4 C 0.45523(16) 0.08165(10) 0.30221(19) 0.0220(5) Uani 1 1 d . . .
H4 H 0.3905 0.0570 0.3423 0.026 Uiso 1 1 calc R . .
C5 C 0.52859(16) 0.12072(11) 0.4185(2) 0.0261(5) Uani 1 1 d . . .
H5A H 0.5596 0.1684 0.3912 0.031 Uiso 1 1 calc R . .
H5B H 0.4910 0.1255 0.5042 0.031 Uiso 1 1 calc R . .
C6 C 0.61428(17) 0.05721(11) 0.4202(2) 0.0302(5) Uani 1 1 d . . .
H6A H 0.6135 0.0252 0.5014 0.036 Uiso 1 1 calc R . .
H6B H 0.6922 0.0732 0.4065 0.036 Uiso 1 1 calc R . .
C7 C 0.55026(16) 0.02483(11) 0.2908(2) 0.0250(5) Uani 1 1 d . . .
H7A H 0.5255 -0.0265 0.3019 0.030 Uiso 1 1 calc R . .
H7B H 0.5909 0.0304 0.2076 0.030 Uiso 1 1 calc R . .
C8 C 0.33397(16) 0.18574(10) 0.21783(19) 0.0236(5) Uani 1 1 d . . .
H8A H 0.2662 0.1642 0.2545 0.028 Uiso 1 1 calc R . .
H8B H 0.3752 0.2140 0.2922 0.028 Uiso 1 1 calc R . .
C9 C 0.21328(17) 0.28785(11) 0.1487(2) 0.0304(5) Uani 1 1 d . . .
H9A H 0.2449 0.3153 0.2300 0.036 Uiso 1 1 calc R . .
H9B H 0.1459 0.2608 0.1738 0.036 Uiso 1 1 calc R . .
C10 C 0.17962(17) 0.34021(12) 0.0365(2) 0.0311(5) Uani 1 1 d . . .
H10 H 0.1444 0.3209 -0.0462 0.037 Uiso 1 1 calc R . .
C11 C 0.19535(18) 0.41110(13) 0.0443(2) 0.0420(6) Uani 1 1 d . . .
H11A H 0.2304 0.4322 0.1256 0.050 Uiso 1 1 calc R . .
H11B H 0.1718 0.4415 -0.0313 0.050 Uiso 1 1 calc R . .
C12 C 0.22593(16) 0.05715(11) 0.07526(19) 0.0246(5) Uani 1 1 d . . .
C13 C 0.19371(16) -0.00012(11) 0.1684(2) 0.0238(5) Uani 1 1 d . . .
C14 C 0.24774(17) -0.05648(11) 0.2333(2) 0.0268(5) Uani 1 1 d . . .
H14 H 0.3254 -0.0686 0.2310 0.032 Uiso 1 1 calc R . .
C15 C 0.16704(17) -0.09475(12) 0.3061(2) 0.0319(5) Uani 1 1 d . . .
H15 H 0.1801 -0.1370 0.3617 0.038 Uiso 1 1 calc R . .
C16 C 0.06950(19) -0.05908(12) 0.2802(2) 0.0361(6) Uani 1 1 d . . .
H16 H 0.0005 -0.0725 0.3158 0.043 Uiso 1 1 calc R . .
C17 C 0.15000(17) 0.09614(12) -0.0008(2) 0.0349(6) Uani 1 1 d . . .
H17A H 0.0716 0.0872 0.0043 0.042 Uiso 1 1 calc R . .
H17B H 0.1740 0.1330 -0.0602 0.042 Uiso 1 1 calc R . .
C18 C 0.57614(16) 0.21100(10) 0.1289(2) 0.0248(5) Uani 1 1 d . . .
H18A H 0.5448 0.2403 0.2016 0.030 Uiso 1 1 calc R . .
H18B H 0.5813 0.2435 0.0491 0.030 Uiso 1 1 calc R . .
C19 C 0.69386(16) 0.18683(11) 0.1792(2) 0.0238(5) Uani 1 1 d . . .
C20 C 0.75304(17) 0.22334(11) 0.2868(2) 0.0302(5) Uani 1 1 d . . .
H20 H 0.7183 0.2629 0.3302 0.036 Uiso 1 1 calc R . .
C21 C 0.86190(18) 0.20267(13) 0.3315(2) 0.0391(6) Uani 1 1 d . . .
H21 H 0.9019 0.2284 0.4045 0.047 Uiso 1 1 calc R . .
C22 C 0.91309(19) 0.14433(13) 0.2698(3) 0.0438(6) Uani 1 1 d . . .
H22 H 0.9873 0.1293 0.3015 0.053 Uiso 1 1 calc R . .
C23 C 0.85491(17) 0.10839(12) 0.1620(2) 0.0372(6) Uani 1 1 d . . .
H23 H 0.8897 0.0689 0.1185 0.045 Uiso 1 1 calc R . .
C24 C 0.74657(16) 0.12953(11) 0.1171(2) 0.0286(5) Uani 1 1 d . . .
H24 H 0.7075 0.1045 0.0425 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
O1 C3 1.352(2) . ?
O1 C2 1.448(2) . ?
O2 C3 1.214(2) . ?
O3 C16 1.371(2) . ?
O3 C13 1.373(2) . ?
N1 C3 1.364(2) . ?
N1 C18 1.466(2) . ?
N1 C1 1.475(2) . ?
N2 C8 1.458(2) . ?
N2 C9 1.468(2) . ?
N2 H2N 0.90(2) . ?
C1 C4 1.526(3) . ?
C1 C8 1.528(2) . ?
C1 C2 1.556(3) . ?
C2 C12 1.499(3) . ?
C2 H2 1.0000 . ?
C4 C7 1.543(3) . ?
C4 C5 1.550(2) . ?
C4 H4 1.0000 . ?
C5 C6 1.541(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.542(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.487(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.308(3) . ?
C10 H10 0.9500 . ?
C11 H11A 0.9500 . ?
C11 H11B 0.9500 . ?
C12 C17 1.327(3) . ?
C12 C13 1.461(3) . ?
C13 C14 1.344(3) . ?
C14 C15 1.426(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.334(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 H17A 0.9500 . ?
C17 H17B 0.9500 . ?
C18 C19 1.508(3) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C24 1.386(3) . ?
C19 C20 1.389(3) . ?
C20 C21 1.382(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.390(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.380(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.379(3) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?

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 O1 C2 108.43(14) . . ?
C16 O3 C13 106.20(16) . . ?
C3 N1 C18 118.83(16) . . ?
C3 N1 C1 111.00(15) . . ?
C18 N1 C1 124.78(15) . . ?
C8 N2 C9 111.01(16) . . ?
C8 N2 H2N 100.9(13) . . ?
C9 N2 H2N 107.9(14) . . ?
N1 C1 C4 114.99(15) . . ?
N1 C1 C8 111.12(15) . . ?
C4 C1 C8 108.77(16) . . ?
N1 C1 C2 98.60(15) . . ?
C4 C1 C2 108.70(15) . . ?
C8 C1 C2 114.52(15) . . ?
O1 C2 C12 110.38(15) . . ?
O1 C2 C1 105.13(15) . . ?
C12 C2 C1 117.70(16) . . ?
O1 C2 H2 107.7 . . ?
C12 C2 H2 107.7 . . ?
C1 C2 H2 107.7 . . ?
O2 C3 O1 121.85(18) . . ?
O2 C3 N1 127.45(19) . . ?
O1 C3 N1 110.70(17) . . ?
C1 C4 C7 119.19(16) . . ?
C1 C4 C5 120.69(16) . . ?
C7 C4 C5 89.64(14) . . ?
C1 C4 H4 108.6 . . ?
C7 C4 H4 108.6 . . ?
C5 C4 H4 108.6 . . ?
C6 C5 C4 89.52(14) . . ?
C6 C5 H5A 113.7 . . ?
C4 C5 H5A 113.7 . . ?
C6 C5 H5B 113.7 . . ?
C4 C5 H5B 113.7 . . ?
H5A C5 H5B 111.0 . . ?
C5 C6 C7 90.01(14) . . ?
C5 C6 H6A 113.6 . . ?
C7 C6 H6A 113.6 . . ?
C5 C6 H6B 113.6 . . ?
C7 C6 H6B 113.6 . . ?
H6A C6 H6B 110.9 . . ?
C6 C7 C4 89.73(15) . . ?
C6 C7 H7A 113.7 . . ?
C4 C7 H7A 113.7 . . ?
C6 C7 H7B 113.7 . . ?
C4 C7 H7B 113.7 . . ?
H7A C7 H7B 110.9 . . ?
N2 C8 C1 113.48(16) . . ?
N2 C8 H8A 108.9 . . ?
C1 C8 H8A 108.9 . . ?
N2 C8 H8B 108.9 . . ?
C1 C8 H8B 108.9 . . ?
H8A C8 H8B 107.7 . . ?
N2 C9 C10 110.79(17) . . ?
N2 C9 H9A 109.5 . . ?
C10 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
C10 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
C11 C10 C9 124.3(2) . . ?
C11 C10 H10 117.9 . . ?
C9 C10 H10 117.9 . . ?
C10 C11 H11A 120.0 . . ?
C10 C11 H11B 120.0 . . ?
H11A C11 H11B 120.0 . . ?
C17 C12 C13 122.28(18) . . ?
C17 C12 C2 122.42(18) . . ?
C13 C12 C2 115.31(17) . . ?
C14 C13 O3 109.50(17) . . ?
C14 C13 C12 134.78(18) . . ?
O3 C13 C12 115.67(17) . . ?
C13 C14 C15 107.37(18) . . ?
C13 C14 H14 126.3 . . ?
C15 C14 H14 126.3 . . ?
C16 C15 C14 105.97(19) . . ?
C16 C15 H15 127.0 . . ?
C14 C15 H15 127.0 . . ?
C15 C16 O3 110.96(19) . . ?
C15 C16 H16 124.5 . . ?
O3 C16 H16 124.5 . . ?
C12 C17 H17A 120.0 . . ?
C12 C17 H17B 120.0 . . ?
H17A C17 H17B 120.0 . . ?
N1 C18 C19 115.20(16) . . ?
N1 C18 H18A 108.5 . . ?
C19 C18 H18A 108.5 . . ?
N1 C18 H18B 108.5 . . ?
C19 C18 H18B 108.5 . . ?
H18A C18 H18B 107.5 . . ?
C24 C19 C20 118.60(18) . . ?
C24 C19 C18 121.11(18) . . ?
C20 C19 C18 120.26(18) . . ?
C21 C20 C19 120.7(2) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
C20 C21 C22 120.2(2) . . ?
C20 C21 H21 119.9 . . ?
C22 C21 H21 119.9 . . ?
C23 C22 C21 119.3(2) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
C24 C23 C22 120.4(2) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C23 C24 C19 120.9(2) . . ?
C23 C24 H24 119.6 . . ?
C19 C24 H24 119.6 . . ?

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
C3 N1 C1 C4 136.73(17) . . . . ?
C18 N1 C1 C4 -69.7(2) . . . . ?
C3 N1 C1 C8 -99.18(18) . . . . ?
C18 N1 C1 C8 54.4(2) . . . . ?
C3 N1 C1 C2 21.38(18) . . . . ?
C18 N1 C1 C2 174.95(15) . . . . ?
C3 O1 C2 C12 147.39(16) . . . . ?
C3 O1 C2 C1 19.51(18) . . . . ?
N1 C1 C2 O1 -23.75(17) . . . . ?
C4 C1 C2 O1 -143.90(15) . . . . ?
C8 C1 C2 O1 94.25(17) . . . . ?
N1 C1 C2 C12 -147.07(16) . . . . ?
C4 C1 C2 C12 92.8(2) . . . . ?
C8 C1 C2 C12 -29.1(2) . . . . ?
C2 O1 C3 O2 173.29(17) . . . . ?
C2 O1 C3 N1 -6.1(2) . . . . ?
C18 N1 C3 O2 14.2(3) . . . . ?
C1 N1 C3 O2 169.58(19) . . . . ?
C18 N1 C3 O1 -166.40(15) . . . . ?
C1 N1 C3 O1 -11.1(2) . . . . ?
N1 C1 C4 C7 -44.1(2) . . . . ?
C8 C1 C4 C7 -169.39(16) . . . . ?
C2 C1 C4 C7 65.3(2) . . . . ?
N1 C1 C4 C5 64.8(2) . . . . ?
C8 C1 C4 C5 -60.5(2) . . . . ?
C2 C1 C4 C5 174.18(16) . . . . ?
C1 C4 C5 C6 -132.23(17) . . . . ?
C7 C4 C5 C6 -7.94(15) . . . . ?
C4 C5 C6 C7 7.95(14) . . . . ?
C5 C6 C7 C4 -7.98(14) . . . . ?
C1 C4 C7 C6 133.47(17) . . . . ?
C5 C4 C7 C6 7.94(14) . . . . ?
C9 N2 C8 C1 172.25(16) . . . . ?
N1 C1 C8 N2 44.7(2) . . . . ?
C4 C1 C8 N2 172.27(16) . . . . ?
C2 C1 C8 N2 -65.9(2) . . . . ?
C8 N2 C9 C10 178.08(17) . . . . ?
N2 C9 C10 C11 -117.8(2) . . . . ?
O1 C2 C12 C17 -29.0(3) . . . . ?
C1 C2 C12 C17 91.6(2) . . . . ?
O1 C2 C12 C13 150.76(16) . . . . ?
C1 C2 C12 C13 -88.6(2) . . . . ?
C16 O3 C13 C14 0.3(2) . . . . ?
C16 O3 C13 C12 178.16(17) . . . . ?
C17 C12 C13 C14 163.3(2) . . . . ?
C2 C12 C13 C14 -16.5(3) . . . . ?
C17 C12 C13 O3 -13.8(3) . . . . ?
C2 C12 C13 O3 166.39(16) . . . . ?
O3 C13 C14 C15 -0.3(2) . . . . ?
C12 C13 C14 C15 -177.5(2) . . . . ?
C13 C14 C15 C16 0.1(2) . . . . ?
C14 C15 C16 O3 0.1(2) . . . . ?
C13 O3 C16 C15 -0.3(2) . . . . ?
C3 N1 C18 C19 -107.01(19) . . . . ?
C1 N1 C18 C19 101.3(2) . . . . ?
N1 C18 C19 C24 40.4(3) . . . . ?
N1 C18 C19 C20 -141.53(18) . . . . ?
C24 C19 C20 C21 -0.4(3) . . . . ?
C18 C19 C20 C21 -178.49(19) . . . . ?
C19 C20 C21 C22 -0.7(3) . . . . ?
C20 C21 C22 C23 1.3(4) . . . . ?
C21 C22 C23 C24 -0.8(4) . . . . ?
C22 C23 C24 C19 -0.3(3) . . . . ?
C20 C19 C24 C23 0.8(3) . . . . ?
C18 C19 C24 C23 178.97(18) . . . . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.043
####################################################################### 
# 
# 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_s3255m
_database_code_depnum_ccdc_archive 'CCDC 1424602'
_audit_update_record             
;
2015-09-15 deposited with the CCDC.
2016-01-08 downloaded from the CCDC.
;
#------------------  SECTION 2. COMPOUND(S) DETAILS -------------------------# 

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H30 N3 O7 S'
_chemical_formula_weight         576.63

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'
S S 0.1246 0.1234 '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                   13.818(2)
_cell_length_b                   14.714(2)
_cell_length_c                   14.863(3)
_cell_angle_alpha                76.010(4)
_cell_angle_beta                 82.840(4)
_cell_angle_gamma                70.291(3)
_cell_volume                     2757.3(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    779
_cell_measurement_theta_min      2.159
_cell_measurement_theta_max      16.107

_exptl_crystal_description       plate
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1212
_exptl_absorpt_coefficient_mu    0.171
_exptl_absorpt_correction_type   none
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20144
_diffrn_reflns_av_R_equivalents  0.1125
_diffrn_reflns_av_sigmaI/netI    0.2881
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.41
_diffrn_reflns_theta_max         25.03
_reflns_number_total             9704
_reflns_number_gt                3309
_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)+(0.0686P)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         9704
_refine_ls_number_parameters     738
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.2054
_refine_ls_R_factor_gt           0.0668
_refine_ls_wR_factor_ref         0.2176
_refine_ls_wR_factor_gt          0.1249
_refine_ls_goodness_of_fit_ref   0.820
_refine_ls_restrained_S_all      0.820
_refine_ls_shift/su_max          0.034
_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 0.7702(3) 0.2435(3) 0.2072(2) 0.0267(12) Uani 1 1 d . . .
H1 H 0.8017 0.1706 0.2123 0.032 Uiso 1 1 calc R . .
C2 C 0.8532(3) 0.2881(3) 0.2144(3) 0.0236(11) Uani 1 1 d . . .
H2 H 0.8820 0.2564 0.2770 0.028 Uiso 1 1 calc R . .
C3 C 0.8104(3) 0.3989(3) 0.2109(3) 0.0288(12) Uani 1 1 d . . .
H3A H 0.8593 0.4195 0.2383 0.035 Uiso 1 1 calc R . .
H3B H 0.8020 0.4355 0.1455 0.035 Uiso 1 1 calc R . .
C4 C 0.6870(3) 0.3411(3) 0.3317(3) 0.0275(12) Uani 1 1 d . . .
H4A H 0.6213 0.3663 0.3667 0.033 Uiso 1 1 calc R . .
H4B H 0.7424 0.3101 0.3764 0.033 Uiso 1 1 calc R . .
C5 C 0.6797(3) 0.2645(3) 0.2818(2) 0.0231(11) Uani 1 1 d . . .
C6 C 0.6180(3) 0.3231(3) 0.1309(3) 0.0299(12) Uani 1 1 d . . .
C7 C 0.9414(3) 0.2645(3) 0.1450(3) 0.0262(11) Uani 1 1 d . . .
C8 C 1.0206(3) 0.2847(3) 0.0072(3) 0.0425(14) Uani 1 1 d . . .
H8 H 1.0365 0.3103 -0.0558 0.051 Uiso 1 1 calc R . .
C9 C 1.0795(3) 0.2055(3) 0.0614(3) 0.0422(14) Uani 1 1 d . . .
H9 H 1.1448 0.1643 0.0435 0.051 Uiso 1 1 calc R . .
C10 C 1.0296(3) 0.1916(3) 0.1509(3) 0.0268(12) Uani 1 1 d . . .
H10 H 1.0545 0.1408 0.2037 0.032 Uiso 1 1 calc R . .
C17 C 0.6753(3) 0.1710(3) 0.3530(3) 0.0284(12) Uani 1 1 d . . .
H17 H 0.6200 0.1901 0.4015 0.034 Uiso 1 1 calc R . .
C18 C 0.7757(3) 0.1030(3) 0.4014(3) 0.0370(14) Uani 1 1 d . . .
H18A H 0.8393 0.1079 0.3647 0.044 Uiso 1 1 calc R . .
H18B H 0.7778 0.1094 0.4658 0.044 Uiso 1 1 calc R . .
C19 C 0.7457(3) 0.0132(3) 0.3945(3) 0.0399(15) Uani 1 1 d . . .
H19A H 0.7146 -0.0166 0.4529 0.048 Uiso 1 1 calc R . .
H19B H 0.8018 -0.0378 0.3691 0.048 Uiso 1 1 calc R . .
C20 C 0.6654(3) 0.0828(3) 0.3222(3) 0.0363(14) Uani 1 1 d . . .
H20A H 0.6893 0.0802 0.2570 0.044 Uiso 1 1 calc R . .
H20B H 0.5962 0.0752 0.3354 0.044 Uiso 1 1 calc R . .
C21 C 0.4826(3) 0.3468(3) 0.2547(3) 0.0295(13) Uani 1 1 d . . .
H21A H 0.4515 0.4107 0.2120 0.035 Uiso 1 1 calc R . .
H21B H 0.4821 0.3608 0.3167 0.035 Uiso 1 1 calc R . .
C22 C 0.4148(3) 0.2837(3) 0.2617(3) 0.0256(12) Uani 1 1 d . . .
C23 C 0.3404(3) 0.2825(3) 0.3340(3) 0.0374(14) Uani 1 1 d . . .
H23 H 0.3370 0.3176 0.3809 0.045 Uiso 1 1 calc R . .
C24 C 0.2725(3) 0.2322(3) 0.3394(3) 0.0442(15) Uani 1 1 d . . .
H24 H 0.2215 0.2340 0.3887 0.053 Uiso 1 1 calc R . .
C25 C 0.2774(3) 0.1792(3) 0.2740(3) 0.0411(15) Uani 1 1 d . . .
H25 H 0.2298 0.1444 0.2779 0.049 Uiso 1 1 calc R . .
C26 C 0.3517(3) 0.1763(3) 0.2021(3) 0.0393(14) Uani 1 1 d . . .
H26 H 0.3561 0.1388 0.1571 0.047 Uiso 1 1 calc R . .
C27 C 0.4204(3) 0.2297(3) 0.1964(3) 0.0375(14) Uani 1 1 d . . .
H27 H 0.4713 0.2284 0.1470 0.045 Uiso 1 1 calc R . .
C28 C 0.7160(3) 0.1019(3) 0.9126(3) 0.0288(13) Uani 1 1 d . . .
H28 H 0.6738 0.0607 0.9490 0.035 Uiso 1 1 calc R . .
C29 C 0.7568(3) 0.1437(3) 0.9787(2) 0.0242(12) Uani 1 1 d . . .
H29 H 0.6958 0.1849 1.0108 0.029 Uiso 1 1 calc R . .
C30 C 0.8174(3) 0.2112(3) 0.9272(3) 0.0289(12) Uani 1 1 d . C .
H30A H 0.8298 0.2479 0.9699 0.035 Uiso 1 1 calc R . .
H30B H 0.8849 0.1712 0.9044 0.035 Uiso 1 1 calc R . .
C31 C 0.6536(3) 0.2854(3) 0.8406(3) 0.0310(13) Uani 1 1 d . C .
H31A H 0.6245 0.3341 0.7841 0.037 Uiso 1 1 calc R . .
H31B H 0.6112 0.3071 0.8951 0.037 Uiso 1 1 calc R . .
C32 C 0.6500(3) 0.1835(3) 0.8363(2) 0.0235(11) Uani 1 1 d . . .
C33 C 0.7915(3) 0.0723(3) 0.7700(3) 0.0302(12) Uani 1 1 d . . .
C34 C 0.8194(3) 0.0645(3) 1.0524(2) 0.0275(12) Uani 1 1 d . . .
C35 C 0.8431(4) -0.0665(3) 1.1668(3) 0.0608(19) Uani 1 1 d . . .
H35 H 0.8326 -0.1218 1.2103 0.073 Uiso 1 1 calc R . .
C36 C 0.9254(3) -0.0399(4) 1.1600(3) 0.0586(18) Uani 1 1 d . . .
H36 H 0.9835 -0.0712 1.1973 0.070 Uiso 1 1 calc R . .
C37 C 0.9113(3) 0.0465(3) 1.0845(3) 0.0406(14) Uani 1 1 d . . .
H37 H 0.9580 0.0827 1.0625 0.049 Uiso 1 1 calc R . .
C38 C 0.78202(15) 0.46027(15) 0.8502(2) 0.0241(12) Uani 1 1 d D . .
C40 C 0.8269(3) 0.58720(17) 0.89573(18) 0.0280(12) Uani 1 1 d D . .
H40 H 0.8696 0.6278 0.8870 0.034 Uiso 1 1 calc R A 3
C41 C 0.7526(3) 0.5893(3) 0.9677(3) 0.0293(13) Uani 1 1 d . C .
H41 H 0.7444 0.6315 1.0093 0.035 Uiso 1 1 calc R . .
C42 C 0.6913(3) 0.5313(3) 0.9793(3) 0.0281(13) Uani 1 1 d . . .
H42 H 0.6373 0.5368 1.0260 0.034 Uiso 1 1 calc R C .
C43 C 0.7076(3) 0.4640(3) 0.9228(3) 0.0288(12) Uani 1 1 d . C .
H43 H 0.6678 0.4205 0.9339 0.035 Uiso 1 1 calc R . .
C44 C 0.5381(3) 0.1873(3) 0.8430(3) 0.0257(12) Uani 1 1 d . . .
H44 H 0.4997 0.2441 0.7947 0.031 Uiso 1 1 calc R . .
C45 C 0.5065(3) 0.0952(3) 0.8428(3) 0.0338(13) Uani 1 1 d . . .
H45A H 0.5589 0.0313 0.8670 0.041 Uiso 1 1 calc R . .
H45B H 0.4825 0.0959 0.7825 0.041 Uiso 1 1 calc R . .
C46 C 0.4180(3) 0.1303(3) 0.9150(3) 0.0473(15) Uani 1 1 d . . .
H46A H 0.3511 0.1700 0.8872 0.057 Uiso 1 1 calc R . .
H46B H 0.4102 0.0767 0.9674 0.057 Uiso 1 1 calc R . .
C47 C 0.4782(3) 0.1928(3) 0.9378(3) 0.0344(13) Uani 1 1 d . . .
H47A H 0.5218 0.1595 0.9919 0.041 Uiso 1 1 calc R . .
H47B H 0.4349 0.2605 0.9431 0.041 Uiso 1 1 calc R . .
C48 C 0.6803(3) 0.2052(3) 0.6572(2) 0.0252(12) Uani 1 1 d . . .
H48A H 0.7432 0.1918 0.6160 0.030 Uiso 1 1 calc R . .
H48B H 0.6538 0.2772 0.6547 0.030 Uiso 1 1 calc R . .
C49 C 0.5999(3) 0.1744(3) 0.6222(3) 0.0281(12) Uani 1 1 d . . .
C50 C 0.5060(3) 0.2429(3) 0.5952(3) 0.0324(13) Uani 1 1 d . . .
H50 H 0.4926 0.3106 0.5957 0.039 Uiso 1 1 calc R . .
C51 C 0.4306(3) 0.2128(3) 0.5672(3) 0.0434(15) Uani 1 1 d . . .
H51 H 0.3662 0.2599 0.5485 0.052 Uiso 1 1 calc R . .
C52 C 0.4496(3) 0.1157(3) 0.5669(3) 0.0398(13) Uani 1 1 d . . .
H52 H 0.3977 0.0950 0.5497 0.048 Uiso 1 1 calc R . .
C53 C 0.5442(3) 0.0472(3) 0.5916(3) 0.0369(14) Uani 1 1 d . . .
H53 H 0.5579 -0.0200 0.5897 0.044 Uiso 1 1 calc R . .
C54 C 0.6188(3) 0.0766(3) 0.6189(3) 0.0281(12) Uani 1 1 d . . .
H54 H 0.6838 0.0293 0.6357 0.034 Uiso 1 1 calc R . .
C55 C 0.9641(3) 0.3147(3) 0.4429(3) 0.0401(14) Uani 1 1 d . . .
H55 H 0.9500 0.3815 0.4104 0.048 Uiso 1 1 calc R . .
C56 C 1.0147(3) 0.2386(3) 0.3982(3) 0.0513(15) Uani 1 1 d . . .
H56 H 1.0369 0.2534 0.3348 0.062 Uiso 1 1 calc R . .
C57 C 1.0333(3) 0.1420(3) 0.4438(3) 0.0604(16) Uani 1 1 d . . .
H57 H 1.0678 0.0901 0.4123 0.073 Uiso 1 1 calc R . .
C58 C 1.0020(3) 0.1212(3) 0.5348(3) 0.0537(16) Uani 1 1 d . . .
H58 H 1.0142 0.0543 0.5664 0.064 Uiso 1 1 calc R . .
C59 C 0.9528(3) 0.1955(3) 0.5816(3) 0.0451(15) Uani 1 1 d . . .
H59 H 0.9319 0.1799 0.6452 0.054 Uiso 1 1 calc R . .
C60 C 0.9339(3) 0.2927(3) 0.5358(3) 0.0398(15) Uani 1 1 d . . .
H60 H 0.9004 0.3443 0.5678 0.048 Uiso 1 1 calc R . .
N1 N 0.7089(2) 0.4228(2) 0.2636(2) 0.0290(10) Uani 1 1 d . B .
N2 N 0.5907(2) 0.3058(2) 0.2227(2) 0.0216(9) Uani 1 1 d . . .
N4 N 0.7595(2) 0.2820(2) 0.8477(2) 0.0268(10) Uani 1 1 d . . .
N5 N 0.7067(2) 0.1526(2) 0.7525(2) 0.0249(10) Uani 1 1 d . . .
O1 O 0.72353(19) 0.28923(18) 0.11769(17) 0.0273(8) Uani 1 1 d . . .
O2 O 0.9312(2) 0.3242(2) 0.05818(19) 0.0410(10) Uani 1 1 d . . .
O3 O 0.5569(2) 0.54508(19) 0.32109(19) 0.0423(9) Uani 1 1 d . B .
O4 O 0.6664(2) 0.59856(18) 0.18491(18) 0.0385(9) Uani 1 1 d . B .
O7 O 0.56218(19) 0.36009(19) 0.06519(18) 0.0330(9) Uani 1 1 d . . .
O8 O 0.8010(2) 0.04112(18) 0.86385(17) 0.0326(9) Uani 1 1 d . . .
O9 O 0.7726(2) -0.0024(2) 1.1012(2) 0.0508(11) Uani 1 1 d . . .
O10 O 0.91540(19) 0.31979(18) 0.77961(17) 0.0321(8) Uani 1 1 d . . .
O11 O 0.7479(2) 0.40733(19) 0.70335(17) 0.0356(9) Uani 1 1 d . . .
O14 O 0.8503(2) 0.02956(19) 0.71600(18) 0.0363(9) Uani 1 1 d . . .
S1 S 0.65585(8) 0.53621(8) 0.27461(8) 0.0342(3) Uani 1 1 d . . .
S2 S 0.80554(8) 0.36511(7) 0.78544(7) 0.0282(3) Uani 1 1 d . C .
C11 C 0.7327(2) 0.5559(2) 0.3555(2) 0.0181(12) Uani 0.6164(16) 1 d PG B 1
C12 C 0.7265(3) 0.5343(3) 0.4520(2) 0.0244(17) Uani 0.6164(16) 1 d PGDU B 1
C13 C 0.7904(3) 0.5585(3) 0.5009(2) 0.0347(19) Uani 0.6164(16) 1 d PG B 1
H13 H 0.7861 0.5437 0.5668 0.042 Uiso 0.6164(16) 1 calc PR B 1
C14 C 0.8605(3) 0.6043(4) 0.4533(3) 0.0313(15) Uani 0.6164(16) 1 d PG B 1
H14 H 0.9041 0.6208 0.4868 0.038 Uiso 0.6164(16) 1 calc PR B 1
C15 C 0.8667(3) 0.6259(3) 0.3569(3) 0.0260(16) Uani 0.6164(16) 1 d PGU B 1
H15 H 0.9146 0.6573 0.3244 0.031 Uiso 0.6164(16) 1 calc PR B 1
C16 C 0.8028(2) 0.6017(2) 0.3079(2) 0.0192(15) Uani 0.6164(16) 1 d PG B 1
H16 H 0.8070 0.6165 0.2420 0.023 Uiso 0.6164(16) 1 calc PR B 1
N3 N 0.6494(4) 0.4952(3) 0.5019(3) 0.0331(14) Uani 0.6164(16) 1 d PD B 1
O5 O 0.5821(4) 0.5480(3) 0.5467(3) 0.0445(14) Uani 0.6164(16) 1 d PD B 1
O6 O 0.6580(3) 0.4095(3) 0.5032(3) 0.0377(12) Uani 0.6164(16) 1 d PD B 1
C11S C 0.7417(4) 0.5670(4) 0.3380(3) 0.0181(12) Uani 0.3836(16) 1 d PG B 2
C12S C 0.8179(5) 0.6117(4) 0.3118(4) 0.0244(17) Uani 0.3836(16) 1 d PGDU B 2
C13S C 0.8754(5) 0.6184(6) 0.3789(5) 0.0347(19) Uani 0.3836(16) 1 d PG B 2
H13S H 0.9274 0.6489 0.3610 0.042 Uiso 0.3836(16) 1 calc PR B 2
C14S C 0.8568(6) 0.5803(6) 0.4721(5) 0.0313(15) Uani 0.3836(16) 1 d PG B 2
H14S H 0.8961 0.5849 0.5179 0.038 Uiso 0.3836(16) 1 calc PR B 2
C15S C 0.7806(6) 0.5356(6) 0.4982(3) 0.0260(16) Uani 0.3836(16) 1 d PGU B 2
H15S H 0.7679 0.5096 0.5619 0.031 Uiso 0.3836(16) 1 calc PR B 2
C16S C 0.7231(5) 0.5289(4) 0.4312(3) 0.0192(15) Uani 0.3836(16) 1 d PG B 2
H16S H 0.6711 0.4984 0.4490 0.023 Uiso 0.3836(16) 1 calc PR B 2
N3S N 0.8324(6) 0.6515(4) 0.2168(5) 0.0331(14) Uani 0.3836(16) 1 d PD B 2
O5S O 0.7979(6) 0.7414(5) 0.1904(5) 0.0445(14) Uani 0.3836(16) 1 d PD B 2
O6S O 0.8876(5) 0.5942(5) 0.1699(4) 0.0377(12) Uani 0.3836(16) 1 d PD B 2
C39 C 0.83695(12) 0.52495(10) 0.83764(11) 0.0227(11) Uani 0.581(4) 1 d PGD C 3
N6 N 0.90625(14) 0.54212(16) 0.75198(12) 0.0284(11) Uani 0.581(4) 1 d PG C 3
O12 O 0.89846(19) 0.5135(2) 0.68349(12) 0.0205(11) Uani 0.581(4) 1 d PG C 3
O13 O 0.9707(2) 0.5789(3) 0.76257(17) 0.0630(14) Uani 0.581(4) 1 d PG C 3
C39S C 0.84018(12) 0.51983(10) 0.84294(11) 0.0227(11) Uani 0.419(4) 1 d PGD C 4
N6S N 0.92444(13) 0.51817(16) 0.76670(12) 0.0284(11) Uani 0.419(4) 1 d PG C 4
O12S O 1.00935(14) 0.5144(3) 0.78573(17) 0.0205(11) Uani 0.419(4) 1 d PG C 4
O13S O 0.89575(18) 0.5277(2) 0.68890(12) 0.0630(14) Uani 0.419(4) 1 d PG C 4


_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 1.459(4) . ?
C1 C2 1.525(6) . ?
C1 C5 1.563(5) . ?
C1 H1 1.0000 . ?
C2 C7 1.498(5) . ?
C2 C3 1.526(5) . ?
C2 H2 1.0000 . ?
C3 N1 1.494(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N1 1.464(5) . ?
C4 C5 1.526(6) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.469(4) . ?
C5 C17 1.535(5) . ?
C6 O7 1.222(4) . ?
C6 N2 1.356(5) . ?
C6 O1 1.377(4) . ?
C7 C10 1.321(5) . ?
C7 O2 1.368(4) . ?
C8 C9 1.318(5) . ?
C8 O2 1.390(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.422(6) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C17 C20 1.527(6) . ?
C17 C18 1.551(5) . ?
C17 H17 1.0000 . ?
C18 C19 1.540(6) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.560(5) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 N2 1.475(4) . ?
C21 C22 1.505(6) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C27 1.375(6) . ?
C22 C23 1.393(5) . ?
C23 C24 1.362(7) . ?
C23 H23 0.9500 . ?
C24 C25 1.368(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.384(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.406(6) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 O8 1.447(4) . ?
C28 C29 1.525(6) . ?
C28 C32 1.556(5) . ?
C28 H28 1.0000 . ?
C29 C34 1.498(5) . ?
C29 C30 1.518(5) . ?
C29 H29 1.0000 . ?
C30 N4 1.483(4) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 N4 1.463(5) . ?
C31 C32 1.534(6) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 N5 1.472(5) . ?
C32 C44 1.520(5) . ?
C33 O14 1.199(4) . ?
C33 N5 1.352(4) . ?
C33 O8 1.367(4) . ?
C34 C37 1.331(6) . ?
C34 O9 1.372(5) . ?
C35 C36 1.307(7) . ?
C35 O9 1.400(5) . ?
C35 H35 0.9500 . ?
C36 C37 1.452(6) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 C39S 1.354(2) . ?
C38 C39 1.372(2) . ?
C38 C43 1.393(5) . ?
C38 S2 1.805(3) . ?
C40 C39S 1.360(3) . ?
C40 C39 1.368(3) . ?
C40 C41 1.386(5) . ?
C40 H40 0.9500 . ?
C41 C42 1.362(6) . ?
C41 H41 0.9500 . ?
C42 C43 1.393(6) . ?
C42 H42 0.9500 . ?
C43 H43 0.9500 . ?
C44 C47 1.547(5) . ?
C44 C45 1.558(6) . ?
C44 H44 1.0000 . ?
C45 C46 1.559(5) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.546(7) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 N5 1.464(4) . ?
C48 C49 1.520(6) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 C50 1.383(5) . ?
C49 C54 1.385(5) . ?
C50 C51 1.402(6) . ?
C50 H50 0.9500 . ?
C51 C52 1.364(6) . ?
C51 H51 0.9500 . ?
C52 C53 1.382(5) . ?
C52 H52 0.9500 . ?
C53 C54 1.380(6) . ?
C53 H53 0.9500 . ?
C54 H54 0.9500 . ?
C55 C56 1.379(6) . ?
C55 C60 1.383(6) . ?
C55 H55 0.9500 . ?
C56 C57 1.370(6) . ?
C56 H56 0.9500 . ?
C57 C58 1.361(6) . ?
C57 H57 0.9500 . ?
C58 C59 1.374(6) . ?
C58 H58 0.9500 . ?
C59 C60 1.378(6) . ?
C59 H59 0.9500 . ?
C60 H60 0.9500 . ?
N1 S1 1.621(3) . ?
N4 S2 1.608(3) . ?
O3 S1 1.433(3) . ?
O4 S1 1.446(3) . ?
O10 S2 1.438(3) . ?
O11 S2 1.432(3) . ?
S1 C11S 1.830(6) . ?
S1 C11 1.830(3) . ?
C11 C12 1.3900 . ?
C11 C16 1.3900 . ?
C12 C13 1.3900 . ?
C12 N3 1.424(6) . ?
C13 C14 1.3900 . ?
C13 H13 0.9500 . ?
C14 C15 1.3900 . ?
C14 H14 0.9500 . ?
C15 C16 1.3900 . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
N3 O6 1.222(6) . ?
N3 O5 1.233(6) . ?
C11S C12S 1.3900 . ?
C11S C16S 1.3900 . ?
C12S C13S 1.3900 . ?
C12S N3S 1.409(8) . ?
C13S C14S 1.3900 . ?
C13S H13S 0.9500 . ?
C14S C15S 1.3900 . ?
C14S H14S 0.9500 . ?
C15S C16S 1.3900 . ?
C15S H15S 0.9500 . ?
C16S H16S 0.9500 . ?
N3S O6S 1.223(8) . ?
N3S O5S 1.226(7) . ?
C39 N6 1.5184 . ?
N6 O12 1.2210 . ?
N6 O13 1.2297 . ?
C39S N6S 1.5183 . ?
N6S O12S 1.2210 . ?
N6S O13S 1.2297 . ?

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 108.7(3) . . ?
O1 C1 C5 105.6(3) . . ?
C2 C1 C5 113.3(3) . . ?
O1 C1 H1 109.7 . . ?
C2 C1 H1 109.7 . . ?
C5 C1 H1 109.7 . . ?
C7 C2 C1 113.0(3) . . ?
C7 C2 C3 111.2(3) . . ?
C1 C2 C3 112.9(3) . . ?
C7 C2 H2 106.4 . . ?
C1 C2 H2 106.4 . . ?
C3 C2 H2 106.4 . . ?
N1 C3 C2 109.9(3) . . ?
N1 C3 H3A 109.7 . . ?
C2 C3 H3A 109.7 . . ?
N1 C3 H3B 109.7 . . ?
C2 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
N1 C4 C5 109.4(3) . . ?
N1 C4 H4A 109.8 . . ?
C5 C4 H4A 109.8 . . ?
N1 C4 H4B 109.8 . . ?
C5 C4 H4B 109.8 . . ?
H4A C4 H4B 108.2 . . ?
N2 C5 C4 110.7(3) . . ?
N2 C5 C17 111.9(3) . . ?
C4 C5 C17 109.8(3) . . ?
N2 C5 C1 100.9(3) . . ?
C4 C5 C1 110.5(3) . . ?
C17 C5 C1 112.9(3) . . ?
O7 C6 N2 128.4(4) . . ?
O7 C6 O1 121.3(3) . . ?
N2 C6 O1 110.3(3) . . ?
C10 C7 O2 111.4(3) . . ?
C10 C7 C2 131.1(3) . . ?
O2 C7 C2 117.4(3) . . ?
C9 C8 O2 108.3(4) . . ?
C9 C8 H8 125.8 . . ?
O2 C8 H8 125.8 . . ?
C8 C9 C10 109.1(3) . . ?
C8 C9 H9 125.4 . . ?
C10 C9 H9 125.4 . . ?
C7 C10 C9 105.2(3) . . ?
C7 C10 H10 127.4 . . ?
C9 C10 H10 127.4 . . ?
C20 C17 C5 121.0(3) . . ?
C20 C17 C18 89.7(3) . . ?
C5 C17 C18 117.9(3) . . ?
C20 C17 H17 108.9 . . ?
C5 C17 H17 108.9 . . ?
C18 C17 H17 108.9 . . ?
C19 C18 C17 88.5(3) . . ?
C19 C18 H18A 113.9 . . ?
C17 C18 H18A 113.9 . . ?
C19 C18 H18B 113.9 . . ?
C17 C18 H18B 113.9 . . ?
H18A C18 H18B 111.1 . . ?
C18 C19 C20 88.9(3) . . ?
C18 C19 H19A 113.8 . . ?
C20 C19 H19A 113.8 . . ?
C18 C19 H19B 113.8 . . ?
C20 C19 H19B 113.8 . . ?
H19A C19 H19B 111.1 . . ?
C17 C20 C19 88.6(3) . . ?
C17 C20 H20A 113.9 . . ?
C19 C20 H20A 113.9 . . ?
C17 C20 H20B 113.9 . . ?
C19 C20 H20B 113.9 . . ?
H20A C20 H20B 111.1 . . ?
N2 C21 C22 116.8(3) . . ?
N2 C21 H21A 108.1 . . ?
C22 C21 H21A 108.1 . . ?
N2 C21 H21B 108.1 . . ?
C22 C21 H21B 108.1 . . ?
H21A C21 H21B 107.3 . . ?
C27 C22 C23 118.1(4) . . ?
C27 C22 C21 122.2(4) . . ?
C23 C22 C21 119.6(4) . . ?
C24 C23 C22 121.7(4) . . ?
C24 C23 H23 119.2 . . ?
C22 C23 H23 119.2 . . ?
C23 C24 C25 120.3(4) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C24 C25 C26 120.1(5) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C25 C26 C27 119.2(4) . . ?
C25 C26 H26 120.4 . . ?
C27 C26 H26 120.4 . . ?
C22 C27 C26 120.7(4) . . ?
C22 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?
O8 C28 C29 110.0(3) . . ?
O8 C28 C32 106.0(3) . . ?
C29 C28 C32 112.9(3) . . ?
O8 C28 H28 109.3 . . ?
C29 C28 H28 109.3 . . ?
C32 C28 H28 109.3 . . ?
C34 C29 C30 110.6(3) . . ?
C34 C29 C28 112.5(3) . . ?
C30 C29 C28 111.9(3) . . ?
C34 C29 H29 107.2 . . ?
C30 C29 H29 107.2 . . ?
C28 C29 H29 107.2 . . ?
N4 C30 C29 110.1(3) . . ?
N4 C30 H30A 109.6 . . ?
C29 C30 H30A 109.6 . . ?
N4 C30 H30B 109.6 . . ?
C29 C30 H30B 109.6 . . ?
H30A C30 H30B 108.2 . . ?
N4 C31 C32 110.7(3) . . ?
N4 C31 H31A 109.5 . . ?
C32 C31 H31A 109.5 . . ?
N4 C31 H31B 109.5 . . ?
C32 C31 H31B 109.5 . . ?
H31A C31 H31B 108.1 . . ?
N5 C32 C44 113.3(3) . . ?
N5 C32 C31 110.6(3) . . ?
C44 C32 C31 108.6(3) . . ?
N5 C32 C28 100.1(3) . . ?
C44 C32 C28 113.5(3) . . ?
C31 C32 C28 110.5(3) . . ?
O14 C33 N5 128.6(4) . . ?
O14 C33 O8 122.1(3) . . ?
N5 C33 O8 109.2(3) . . ?
C37 C34 O9 111.2(3) . . ?
C37 C34 C29 133.5(4) . . ?
O9 C34 C29 115.2(3) . . ?
C36 C35 O9 110.7(4) . . ?
C36 C35 H35 124.6 . . ?
O9 C35 H35 124.6 . . ?
C35 C36 C37 107.1(4) . . ?
C35 C36 H36 126.5 . . ?
C37 C36 H36 126.5 . . ?
C34 C37 C36 105.9(4) . . ?
C34 C37 H37 127.1 . . ?
C36 C37 H37 127.1 . . ?
C39S C38 C39 4.1 . . ?
C39S C38 C43 116.2(3) . . ?
C39 C38 C43 117.2(3) . . ?
C39S C38 S2 125.4(2) . . ?
C39 C38 S2 124.9(2) . . ?
C43 C38 S2 117.7(2) . . ?
C39S C40 C39 4.1 . . ?
C39S C40 C41 116.8(3) . . ?
C39 C40 C41 118.0(3) . . ?
C39S C40 H40 122.0 . . ?
C39 C40 H40 121.0 . . ?
C41 C40 H40 121.0 . . ?
C42 C41 C40 120.6(4) . . ?
C42 C41 H41 119.7 . . ?
C40 C41 H41 119.7 . . ?
C41 C42 C43 120.1(4) . . ?
C41 C42 H42 119.9 . . ?
C43 C42 H42 119.9 . . ?
C42 C43 C38 120.2(4) . . ?
C42 C43 H43 119.9 . . ?
C38 C43 H43 119.9 . . ?
C32 C44 C47 118.0(3) . . ?
C32 C44 C45 122.1(3) . . ?
C47 C44 C45 88.2(3) . . ?
C32 C44 H44 108.9 . . ?
C47 C44 H44 108.9 . . ?
C45 C44 H44 108.9 . . ?
C44 C45 C46 87.7(3) . . ?
C44 C45 H45A 114.0 . . ?
C46 C45 H45A 114.0 . . ?
C44 C45 H45B 114.0 . . ?
C46 C45 H45B 114.0 . . ?
H45A C45 H45B 111.2 . . ?
C47 C46 C45 88.2(3) . . ?
C47 C46 H46A 113.9 . . ?
C45 C46 H46A 113.9 . . ?
C47 C46 H46B 113.9 . . ?
C45 C46 H46B 113.9 . . ?
H46A C46 H46B 111.1 . . ?
C46 C47 C44 88.5(3) . . ?
C46 C47 H47A 113.9 . . ?
C44 C47 H47A 113.9 . . ?
C46 C47 H47B 113.9 . . ?
C44 C47 H47B 113.9 . . ?
H47A C47 H47B 111.1 . . ?
N5 C48 C49 112.0(3) . . ?
N5 C48 H48A 109.2 . . ?
C49 C48 H48A 109.2 . . ?
N5 C48 H48B 109.2 . . ?
C49 C48 H48B 109.2 . . ?
H48A C48 H48B 107.9 . . ?
C50 C49 C54 119.0(4) . . ?
C50 C49 C48 120.6(4) . . ?
C54 C49 C48 120.3(3) . . ?
C49 C50 C51 120.1(4) . . ?
C49 C50 H50 120.0 . . ?
C51 C50 H50 120.0 . . ?
C52 C51 C50 120.0(4) . . ?
C52 C51 H51 120.0 . . ?
C50 C51 H51 120.0 . . ?
C51 C52 C53 120.2(4) . . ?
C51 C52 H52 119.9 . . ?
C53 C52 H52 119.9 . . ?
C54 C53 C52 120.0(4) . . ?
C54 C53 H53 120.0 . . ?
C52 C53 H53 120.0 . . ?
C53 C54 C49 120.6(4) . . ?
C53 C54 H54 119.7 . . ?
C49 C54 H54 119.7 . . ?
C56 C55 C60 119.2(4) . . ?
C56 C55 H55 120.4 . . ?
C60 C55 H55 120.4 . . ?
C57 C56 C55 120.9(4) . . ?
C57 C56 H56 119.5 . . ?
C55 C56 H56 119.5 . . ?
C58 C57 C56 119.3(4) . . ?
C58 C57 H57 120.3 . . ?
C56 C57 H57 120.3 . . ?
C57 C58 C59 121.0(4) . . ?
C57 C58 H58 119.5 . . ?
C59 C58 H58 119.5 . . ?
C58 C59 C60 119.7(4) . . ?
C58 C59 H59 120.1 . . ?
C60 C59 H59 120.1 . . ?
C59 C60 C55 119.7(4) . . ?
C59 C60 H60 120.1 . . ?
C55 C60 H60 120.1 . . ?
C4 N1 C3 116.7(3) . . ?
C4 N1 S1 121.2(2) . . ?
C3 N1 S1 116.9(3) . . ?
C6 N2 C5 112.8(3) . . ?
C6 N2 C21 120.2(3) . . ?
C5 N2 C21 125.6(3) . . ?
C31 N4 C30 117.5(3) . . ?
C31 N4 S2 122.0(2) . . ?
C30 N4 S2 119.3(3) . . ?
C33 N5 C48 121.2(3) . . ?
C33 N5 C32 114.0(3) . . ?
C48 N5 C32 124.8(3) . . ?
C6 O1 C1 109.5(3) . . ?
C7 O2 C8 105.9(3) . . ?
C33 O8 C28 110.6(3) . . ?
C34 O9 C35 105.1(4) . . ?
O3 S1 O4 121.00(16) . . ?
O3 S1 N1 108.18(18) . . ?
O4 S1 N1 106.97(16) . . ?
O3 S1 C11S 113.0(2) . . ?
O4 S1 C11S 98.5(2) . . ?
N1 S1 C11S 108.3(2) . . ?
O3 S1 C11 105.43(16) . . ?
O4 S1 C11 108.04(17) . . ?
N1 S1 C11 106.39(15) . . ?
C11S S1 C11 9.68(19) . . ?
O11 S2 O10 120.92(16) . . ?
O11 S2 N4 107.24(18) . . ?
O10 S2 N4 106.45(15) . . ?
O11 S2 C38 108.12(15) . . ?
O10 S2 C38 106.09(15) . . ?
N4 S2 C38 107.37(15) . . ?
C12 C11 C16 120.0 . . ?
C12 C11 S1 129.05(15) . . ?
C16 C11 S1 110.92(15) . . ?
C11 C12 C13 120.0 . . ?
C11 C12 N3 120.9(3) . . ?
C13 C12 N3 118.9(3) . . ?
C12 C13 C14 120.0 . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C15 C14 C13 120.0 . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C16 120.0 . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C15 C16 C11 120.0 . . ?
C15 C16 H16 120.0 . . ?
C11 C16 H16 120.0 . . ?
O6 N3 O5 124.1(5) . . ?
O6 N3 C12 118.2(4) . . ?
O5 N3 C12 117.5(4) . . ?
C12S C11S C16S 120.0 . . ?
C12S C11S S1 134.4(3) . . ?
C16S C11S S1 105.5(3) . . ?
C13S C12S C11S 120.0 . . ?
C13S C12S N3S 121.9(5) . . ?
C11S C12S N3S 118.1(5) . . ?
C12S C13S C14S 120.0 . . ?
C12S C13S H13S 120.0 . . ?
C14S C13S H13S 120.0 . . ?
C15S C14S C13S 120.0 . . ?
C15S C14S H14S 120.0 . . ?
C13S C14S H14S 120.0 . . ?
C14S C15S C16S 120.0 . . ?
C14S C15S H15S 120.0 . . ?
C16S C15S H15S 120.0 . . ?
C15S C16S C11S 120.0 . . ?
C15S C16S H16S 120.0 . . ?
C11S C16S H16S 120.0 . . ?
O6S N3S O5S 125.3(7) . . ?
O6S N3S C12S 116.7(6) . . ?
O5S N3S C12S 117.5(6) . . ?
C40 C39 C38 123.6(2) . . ?
C40 C39 N6 113.27(17) . . ?
C38 C39 N6 122.81(17) . . ?
O12 N6 O13 126.6 . . ?
O12 N6 C39 119.2 . . ?
O13 N6 C39 114.0 . . ?
C38 C39S C40 125.7(2) . . ?
C38 C39S N6S 119.25(17) . . ?
C40 C39S N6S 114.98(18) . . ?
O12S N6S O13S 126.6 . . ?
O12S N6S C39S 119.2 . . ?
O13S N6S C39S 114.0 . . ?

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 C7 -65.0(4) . . . . ?
C5 C1 C2 C7 177.9(3) . . . . ?
O1 C1 C2 C3 62.2(4) . . . . ?
C5 C1 C2 C3 -54.8(4) . . . . ?
C7 C2 C3 N1 166.8(3) . . . . ?
C1 C2 C3 N1 38.5(4) . . . . ?
N1 C4 C5 N2 -65.7(4) . . . . ?
N1 C4 C5 C17 170.3(3) . . . . ?
N1 C4 C5 C1 45.2(4) . . . . ?
O1 C1 C5 N2 8.9(4) . . . . ?
C2 C1 C5 N2 127.8(3) . . . . ?
O1 C1 C5 C4 -108.2(3) . . . . ?
C2 C1 C5 C4 10.7(4) . . . . ?
O1 C1 C5 C17 128.5(3) . . . . ?
C2 C1 C5 C17 -112.6(4) . . . . ?
C1 C2 C7 C10 -92.3(5) . . . . ?
C3 C2 C7 C10 139.5(5) . . . . ?
C1 C2 C7 O2 84.7(4) . . . . ?
C3 C2 C7 O2 -43.5(5) . . . . ?
O2 C8 C9 C10 -0.6(6) . . . . ?
O2 C7 C10 C9 -0.1(5) . . . . ?
C2 C7 C10 C9 177.0(4) . . . . ?
C8 C9 C10 C7 0.4(5) . . . . ?
N2 C5 C17 C20 55.4(4) . . . . ?
C4 C5 C17 C20 178.7(3) . . . . ?
C1 C5 C17 C20 -57.6(5) . . . . ?
N2 C5 C17 C18 163.5(3) . . . . ?
C4 C5 C17 C18 -73.3(4) . . . . ?
C1 C5 C17 C18 50.5(5) . . . . ?
C20 C17 C18 C19 -15.8(3) . . . . ?
C5 C17 C18 C19 -141.2(4) . . . . ?
C17 C18 C19 C20 15.5(3) . . . . ?
C5 C17 C20 C19 138.4(3) . . . . ?
C18 C17 C20 C19 15.6(3) . . . . ?
C18 C19 C20 C17 -15.7(3) . . . . ?
N2 C21 C22 C27 -39.9(5) . . . . ?
N2 C21 C22 C23 142.9(3) . . . . ?
C27 C22 C23 C24 -2.1(5) . . . . ?
C21 C22 C23 C24 175.2(3) . . . . ?
C22 C23 C24 C25 1.5(6) . . . . ?
C23 C24 C25 C26 0.1(6) . . . . ?
C24 C25 C26 C27 -1.1(6) . . . . ?
C23 C22 C27 C26 1.1(5) . . . . ?
C21 C22 C27 C26 -176.1(3) . . . . ?
C25 C26 C27 C22 0.4(6) . . . . ?
O8 C28 C29 C34 -62.4(4) . . . . ?
C32 C28 C29 C34 179.4(3) . . . . ?
O8 C28 C29 C30 62.9(4) . . . . ?
C32 C28 C29 C30 -55.3(4) . . . . ?
C34 C29 C30 N4 173.5(3) . . . . ?
C28 C29 C30 N4 47.3(4) . . . . ?
N4 C31 C32 N5 -63.0(4) . . . . ?
N4 C31 C32 C44 172.0(3) . . . . ?
N4 C31 C32 C28 46.9(4) . . . . ?
O8 C28 C32 N5 2.8(4) . . . . ?
C29 C28 C32 N5 123.3(3) . . . . ?
O8 C28 C32 C44 123.9(3) . . . . ?
C29 C28 C32 C44 -115.6(4) . . . . ?
O8 C28 C32 C31 -113.8(3) . . . . ?
C29 C28 C32 C31 6.7(4) . . . . ?
C30 C29 C34 C37 5.3(6) . . . . ?
C28 C29 C34 C37 131.2(5) . . . . ?
C30 C29 C34 O9 -178.1(3) . . . . ?
C28 C29 C34 O9 -52.1(4) . . . . ?
O9 C35 C36 C37 -0.9(5) . . . . ?
O9 C34 C37 C36 0.5(5) . . . . ?
C29 C34 C37 C36 177.2(4) . . . . ?
C35 C36 C37 C34 0.3(5) . . . . ?
C39S C40 C41 C42 -4.9(5) . . . . ?
C39 C40 C41 C42 -0.4(5) . . . . ?
C40 C41 C42 C43 4.6(5) . . . . ?
C41 C42 C43 C38 -4.4(5) . . . . ?
C39S C38 C43 C42 4.4(4) . . . . ?
C39 C38 C43 C42 0.0(4) . . . . ?
S2 C38 C43 C42 175.5(3) . . . . ?
N5 C32 C44 C47 164.9(3) . . . . ?
C31 C32 C44 C47 -71.7(4) . . . . ?
C28 C32 C44 C47 51.6(4) . . . . ?
N5 C32 C44 C45 57.9(4) . . . . ?
C31 C32 C44 C45 -178.8(3) . . . . ?
C28 C32 C44 C45 -55.5(5) . . . . ?
C32 C44 C45 C46 142.5(3) . . . . ?
C47 C44 C45 C46 20.1(3) . . . . ?
C44 C45 C46 C47 -20.1(3) . . . . ?
C45 C46 C47 C44 20.3(3) . . . . ?
C32 C44 C47 C46 -146.2(3) . . . . ?
C45 C44 C47 C46 -20.3(3) . . . . ?
N5 C48 C49 C50 119.6(4) . . . . ?
N5 C48 C49 C54 -58.8(4) . . . . ?
C54 C49 C50 C51 1.5(6) . . . . ?
C48 C49 C50 C51 -176.9(3) . . . . ?
C49 C50 C51 C52 0.2(6) . . . . ?
C50 C51 C52 C53 -1.8(6) . . . . ?
C51 C52 C53 C54 1.7(6) . . . . ?
C52 C53 C54 C49 0.1(6) . . . . ?
C50 C49 C54 C53 -1.7(6) . . . . ?
C48 C49 C54 C53 176.8(3) . . . . ?
C60 C55 C56 C57 1.5(7) . . . . ?
C55 C56 C57 C58 -0.5(7) . . . . ?
C56 C57 C58 C59 -0.6(7) . . . . ?
C57 C58 C59 C60 0.6(7) . . . . ?
C58 C59 C60 C55 0.4(7) . . . . ?
C56 C55 C60 C59 -1.4(7) . . . . ?
C5 C4 N1 C3 -65.0(4) . . . . ?
C5 C4 N1 S1 141.4(3) . . . . ?
C2 C3 N1 C4 20.4(5) . . . . ?
C2 C3 N1 S1 175.2(3) . . . . ?
O7 C6 N2 C5 -177.1(4) . . . . ?
O1 C6 N2 C5 4.9(5) . . . . ?
O7 C6 N2 C21 -9.8(7) . . . . ?
O1 C6 N2 C21 172.3(3) . . . . ?
C4 C5 N2 C6 108.4(4) . . . . ?
C17 C5 N2 C6 -128.9(3) . . . . ?
C1 C5 N2 C6 -8.6(4) . . . . ?
C4 C5 N2 C21 -58.1(5) . . . . ?
C17 C5 N2 C21 64.6(5) . . . . ?
C1 C5 N2 C21 -175.1(3) . . . . ?
C22 C21 N2 C6 89.6(4) . . . . ?
C22 C21 N2 C5 -104.8(4) . . . . ?
C32 C31 N4 C30 -57.8(4) . . . . ?
C32 C31 N4 S2 134.4(3) . . . . ?
C29 C30 N4 C31 8.7(4) . . . . ?
C29 C30 N4 S2 176.9(2) . . . . ?
O14 C33 N5 C48 -5.7(7) . . . . ?
O8 C33 N5 C48 176.7(3) . . . . ?
O14 C33 N5 C32 177.9(4) . . . . ?
O8 C33 N5 C32 0.2(5) . . . . ?
C49 C48 N5 C33 98.2(4) . . . . ?
C49 C48 N5 C32 -85.7(4) . . . . ?
C44 C32 N5 C33 -123.2(4) . . . . ?
C31 C32 N5 C33 114.6(4) . . . . ?
C28 C32 N5 C33 -2.0(4) . . . . ?
C44 C32 N5 C48 60.5(5) . . . . ?
C31 C32 N5 C48 -61.7(5) . . . . ?
C28 C32 N5 C48 -178.2(4) . . . . ?
O7 C6 O1 C1 -176.5(4) . . . . ?
N2 C6 O1 C1 1.6(4) . . . . ?
C2 C1 O1 C6 -128.8(3) . . . . ?
C5 C1 O1 C6 -6.9(4) . . . . ?
C10 C7 O2 C8 -0.2(5) . . . . ?
C2 C7 O2 C8 -177.8(4) . . . . ?
C9 C8 O2 C7 0.5(5) . . . . ?
O14 C33 O8 C28 -176.0(4) . . . . ?
N5 C33 O8 C28 1.9(5) . . . . ?
C29 C28 O8 C33 -125.4(3) . . . . ?
C32 C28 O8 C33 -3.0(4) . . . . ?
C37 C34 O9 C35 -1.0(4) . . . . ?
C29 C34 O9 C35 -178.4(3) . . . . ?
C36 C35 O9 C34 1.2(5) . . . . ?
C4 N1 S1 O3 -30.4(3) . . . . ?
C3 N1 S1 O3 176.0(3) . . . . ?
C4 N1 S1 O4 -162.3(3) . . . . ?
C3 N1 S1 O4 44.2(3) . . . . ?
C4 N1 S1 C11S 92.4(3) . . . . ?
C3 N1 S1 C11S -61.2(3) . . . . ?
C4 N1 S1 C11 82.4(3) . . . . ?
C3 N1 S1 C11 -71.1(3) . . . . ?
C31 N4 S2 O11 -25.2(3) . . . . ?
C30 N4 S2 O11 167.2(3) . . . . ?
C31 N4 S2 O10 -155.9(3) . . . . ?
C30 N4 S2 O10 36.4(3) . . . . ?
C31 N4 S2 C38 90.8(3) . . . . ?
C30 N4 S2 C38 -76.9(3) . . . . ?
C39S C38 S2 O11 -92.6(2) . . . . ?
C39 C38 S2 O11 -87.7(2) . . . . ?
C43 C38 S2 O11 97.2(3) . . . . ?
C39S C38 S2 O10 38.5(3) . . . . ?
C39 C38 S2 O10 43.4(3) . . . . ?
C43 C38 S2 O10 -131.7(2) . . . . ?
C39S C38 S2 N4 152.0(2) . . . . ?
C39 C38 S2 N4 156.9(2) . . . . ?
C43 C38 S2 N4 -18.2(3) . . . . ?
O3 S1 C11 C12 30.6(2) . . . . ?
O4 S1 C11 C12 161.24(19) . . . . ?
N1 S1 C11 C12 -84.2(2) . . . . ?
C11S S1 C11 C12 172.7(11) . . . . ?
O3 S1 C11 C16 -147.37(16) . . . . ?
O4 S1 C11 C16 -16.68(17) . . . . ?
N1 S1 C11 C16 97.88(17) . . . . ?
C11S S1 C11 C16 -5.2(11) . . . . ?
C16 C11 C12 C13 0.0 . . . . ?
S1 C11 C12 C13 -177.76(18) . . . . ?
C16 C11 C12 N3 174.6(3) . . . . ?
S1 C11 C12 N3 -3.2(3) . . . . ?
C11 C12 C13 C14 0.0 . . . . ?
N3 C12 C13 C14 -174.7(3) . . . . ?
C12 C13 C14 C15 0.0 . . . . ?
C13 C14 C15 C16 0.0 . . . . ?
C14 C15 C16 C11 0.0 . . . . ?
C12 C11 C16 C15 0.0 . . . . ?
S1 C11 C16 C15 178.14(15) . . . . ?
C11 C12 N3 O6 72.4(5) . . . . ?
C13 C12 N3 O6 -113.0(4) . . . . ?
C11 C12 N3 O5 -112.6(5) . . . . ?
C13 C12 N3 O5 62.0(5) . . . . ?
O3 S1 C11S C12S -145.5(3) . . . . ?
O4 S1 C11S C12S -16.5(4) . . . . ?
N1 S1 C11S C12S 94.6(4) . . . . ?
C11 S1 C11S C12S 174.5(13) . . . . ?
O3 S1 C11S C16S 38.5(3) . . . . ?
O4 S1 C11S C16S 167.5(2) . . . . ?
N1 S1 C11S C16S -81.4(2) . . . . ?
C11 S1 C11S C16S -1.4(10) . . . . ?
C16S C11S C12S C13S 0.0 . . . . ?
S1 C11S C12S C13S -175.5(4) . . . . ?
C16S C11S C12S N3S -178.4(5) . . . . ?
S1 C11S C12S N3S 6.0(6) . . . . ?
C11S C12S C13S C14S 0.0 . . . . ?
N3S C12S C13S C14S 178.4(5) . . . . ?
C12S C13S C14S C15S 0.0 . . . . ?
C13S C14S C15S C16S 0.0 . . . . ?
C14S C15S C16S C11S 0.0 . . . . ?
C12S C11S C16S C15S 0.0 . . . . ?
S1 C11S C16S C15S 176.7(3) . . . . ?
C13S C12S N3S O6S 97.3(8) . . . . ?
C11S C12S N3S O6S -84.3(9) . . . . ?
C13S C12S N3S O5S -75.4(9) . . . . ?
C11S C12S N3S O5S 103.0(9) . . . . ?
C39S C40 C39 C38 70.0(2) . . . . ?
C41 C40 C39 C38 -4.2(4) . . . . ?
C39S C40 C39 N6 -116.25(8) . . . . ?
C41 C40 C39 N6 169.5(2) . . . . ?
C39S C38 C39 C40 -73.2(2) . . . . ?
C43 C38 C39 C40 4.4(3) . . . . ?
S2 C38 C39 C40 -170.7(2) . . . . ?
C39S C38 C39 N6 113.70(10) . . . . ?
C43 C38 C39 N6 -168.8(2) . . . . ?
S2 C38 C39 N6 16.2(3) . . . . ?
C40 C39 N6 O12 -158.88(18) . . . . ?
C38 C39 N6 O12 14.89(18) . . . . ?
C40 C39 N6 O13 25.89(18) . . . . ?
C38 C39 N6 O13 -160.35(18) . . . . ?
C39 C38 C39S C40 99.3(2) . . . . ?
C43 C38 C39S C40 -5.1(3) . . . . ?
S2 C38 C39S C40 -175.4(2) . . . . ?
C39 C38 C39S N6S -76.87(9) . . . . ?
C43 C38 C39S N6S 178.7(2) . . . . ?
S2 C38 C39S N6S 8.4(3) . . . . ?
C39 C40 C39S C38 -102.4(2) . . . . ?
C41 C40 C39S C38 5.4(4) . . . . ?
C39 C40 C39S N6S 73.89(9) . . . . ?
C41 C40 C39S N6S -178.3(2) . . . . ?
C38 C39S N6S O12S -134.07(18) . . . . ?
C40 C39S N6S O12S 49.36(17) . . . . ?
C38 C39S N6S O13S 50.68(18) . . . . ?
C40 C39S N6S O13S -125.88(17) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.099
