# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2014


data_yk634p21n

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C66 H76 N4 O16'
_chemical_formula_weight         1181.31

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)/n

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

_cell_length_a                   12.3538(10)
_cell_length_b                   13.2468(11)
_cell_length_c                   19.3848(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.400(2)
_cell_angle_gamma                90.00
_cell_volume                     3166.7(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1671
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      18.44

_exptl_crystal_description       rod
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1256
_exptl_absorpt_coefficient_mu    0.089
_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      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17442
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_sigmaI/netI    0.1439
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         25.99
_reflns_number_total             6205
_reflns_number_gt                1957
_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)+(0.0753P)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     SHELXL
_refine_ls_extinction_coef       0.0062(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6205
_refine_ls_number_parameters     403
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1602
_refine_ls_R_factor_gt           0.0579
_refine_ls_wR_factor_ref         0.1606
_refine_ls_wR_factor_gt          0.1435
_refine_ls_goodness_of_fit_ref   0.752
_refine_ls_restrained_S_all      0.752
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2296(3) 0.7175(3) -0.0916(3) 0.147(2) Uani 1 1 d . . .
C2 C 0.2912(3) 0.8023(3) -0.1231(2) 0.0782(11) Uani 1 1 d . . .
C3 C 0.3436(3) 0.8076(3) -0.1831(2) 0.0879(12) Uani 1 1 d . . .
H3 H 0.3513 0.7554 -0.2145 0.105 Uiso 1 1 calc R . .
C4 C 0.3839(3) 0.9066(3) -0.1890(2) 0.0859(12) Uani 1 1 d . . .
H4 H 0.4231 0.9305 -0.2251 0.103 Uiso 1 1 calc R . .
C5 C 0.3565(3) 0.9613(3) -0.13363(19) 0.0659(9) Uani 1 1 d . . .
C6 C 0.3739(3) 1.0724(3) -0.11560(19) 0.0714(10) Uani 1 1 d . . .
C7 C 0.3427(3) 1.0945(2) -0.0441(2) 0.0683(10) Uani 1 1 d . . .
C8 C 0.4004(3) 1.1173(2) 0.0151(2) 0.0803(11) Uani 1 1 d . . .
H8 H 0.4751 1.1271 0.0195 0.096 Uiso 1 1 calc R . .
C9 C 0.3287(3) 1.1239(2) 0.06964(19) 0.0785(10) Uani 1 1 d . . .
H9 H 0.3479 1.1375 0.1158 0.094 Uiso 1 1 calc R . .
C10 C 0.2263(3) 1.1065(2) 0.04166(19) 0.0639(9) Uani 1 1 d . . .
C11 C 0.1191(2) 1.0909(2) 0.07317(16) 0.0634(9) Uani 1 1 d . . .
H11 H 0.0707 1.0585 0.0379 0.076 Uiso 1 1 calc R . .
C12 C 0.0617(3) 1.1851(2) 0.09659(16) 0.0598(9) Uani 1 1 d . . .
C13 C 0.1153(3) 1.2600(3) 0.13494(16) 0.0715(10) Uani 1 1 d . . .
H13 H 0.1901 1.2559 0.1434 0.086 Uiso 1 1 calc R . .
C14 C 0.0594(3) 1.3408(3) 0.16096(18) 0.0782(10) Uani 1 1 d . . .
H14 H 0.0962 1.3899 0.1874 0.094 Uiso 1 1 calc R . .
C15 C -0.0520(3) 1.3482(3) 0.14724(19) 0.0764(10) Uani 1 1 d . . .
H15 H -0.0892 1.4028 0.1645 0.092 Uiso 1 1 calc R . .
C16 C -0.1086(3) 1.2759(3) 0.1085(2) 0.0794(11) Uani 1 1 d . . .
C17 C -0.0489(3) 1.1955(3) 0.08363(17) 0.0709(10) Uani 1 1 d . . .
H17 H -0.0855 1.1465 0.0570 0.085 Uiso 1 1 calc R . .
C18 C 0.2692(4) 0.6552(5) -0.0548(4) 0.245(4) Uani 1 1 d . . .
C19 C 0.3879(5) 0.6438(5) -0.0329(5) 0.130(3) Uani 1 1 d . . .
C20 C 0.5645(3) 0.6071(3) -0.0647(2) 0.0987(13) Uani 1 1 d . . .
H20A H 0.5789 0.5519 -0.0326 0.118 Uiso 1 1 calc R . .
H20B H 0.5896 0.6691 -0.0424 0.118 Uiso 1 1 calc R . .
C21 C 0.6226(4) 0.5904(4) -0.1274(3) 0.164(2) Uani 1 1 d . . .
H21A H 0.6094 0.5228 -0.1438 0.246 Uiso 1 1 calc R . .
H21B H 0.6989 0.5998 -0.1173 0.246 Uiso 1 1 calc R . .
H21C H 0.5974 0.6376 -0.1624 0.246 Uiso 1 1 calc R . .
C22 C 0.2103(5) 0.5636(6) -0.0261(4) 0.138(3) Uani 1 1 d . . .
C23 C 0.1571(5) 0.3932(5) -0.0372(3) 0.182(3) Uani 1 1 d . . .
H23A H 0.2102 0.3480 -0.0150 0.219 Uiso 1 1 calc R . .
H23B H 0.1087 0.4146 -0.0024 0.219 Uiso 1 1 calc R . .
C24 C 0.0993(5) 0.3414(5) -0.0861(3) 0.196(3) Uani 1 1 d . . .
H24A H 0.0482 0.3858 -0.1099 0.294 Uiso 1 1 calc R . .
H24B H 0.0610 0.2876 -0.0650 0.294 Uiso 1 1 calc R . .
H24C H 0.1472 0.3138 -0.1184 0.294 Uiso 1 1 calc R . .
C25 C 0.4948(3) 1.0992(3) -0.12235(19) 0.0962(13) Uani 1 1 d . . .
H25A H 0.5054 1.1701 -0.1144 0.144 Uiso 1 1 calc R . .
H25B H 0.5153 1.0825 -0.1680 0.144 Uiso 1 1 calc R . .
H25C H 0.5387 1.0615 -0.0889 0.144 Uiso 1 1 calc R . .
C26 C 0.3052(3) 1.1370(3) -0.16813(19) 0.0950(12) Uani 1 1 d . . .
H26A H 0.2299 1.1212 -0.1649 0.143 Uiso 1 1 calc R . .
H26B H 0.3262 1.1227 -0.2140 0.143 Uiso 1 1 calc R . .
H26C H 0.3170 1.2073 -0.1581 0.143 Uiso 1 1 calc R . .
C27 C 0.1344(2) 1.0151(2) 0.13441(16) 0.0618(9) Uani 1 1 d . . .
H27 H 0.1824 1.0453 0.1708 0.074 Uiso 1 1 calc R . .
C28 C 0.1813(3) 0.9153(3) 0.1132(2) 0.0716(10) Uani 1 1 d . . .
C29 C 0.2446(4) 0.7579(3) 0.1581(3) 0.148(2) Uani 1 1 d . . .
H29A H 0.2337 0.7409 0.1095 0.178 Uiso 1 1 calc R . .
H29B H 0.3216 0.7533 0.1707 0.178 Uiso 1 1 calc R . .
C30 C 0.1888(5) 0.6889(4) 0.1972(3) 0.172(2) Uani 1 1 d . . .
H30A H 0.1941 0.7090 0.2449 0.258 Uiso 1 1 calc R . .
H30B H 0.2201 0.6230 0.1928 0.258 Uiso 1 1 calc R . .
H30C H 0.1140 0.6872 0.1808 0.258 Uiso 1 1 calc R . .
C31 C 0.0250(3) 0.9960(3) 0.1623(2) 0.0671(10) Uani 1 1 d . . .
C32 C -0.0922(3) 1.0322(3) 0.25107(19) 0.0990(13) Uani 1 1 d . . .
H32A H -0.1489 1.0449 0.2154 0.119 Uiso 1 1 calc R . .
H32B H -0.1029 0.9655 0.2701 0.119 Uiso 1 1 calc R . .
C33 C -0.0945(4) 1.1081(3) 0.3050(2) 0.1333(18) Uani 1 1 d . . .
H33A H -0.0341 1.0982 0.3377 0.200 Uiso 1 1 calc R . .
H33B H -0.1609 1.1022 0.3280 0.200 Uiso 1 1 calc R . .
H33C H -0.0902 1.1741 0.2848 0.200 Uiso 1 1 calc R . .
N1 N 0.2997(2) 0.8963(2) -0.09342(18) 0.0689(8) Uani 1 1 d . . .
N2 N 0.2346(3) 1.0895(2) -0.02755(16) 0.0663(8) Uani 1 1 d . . .
O1 O 0.4222(3) 0.6621(3) 0.0232(2) 0.1312(15) Uani 1 1 d . . .
O2 O 0.4510(3) 0.6137(2) -0.08191(18) 0.1160(11) Uani 1 1 d . . .
O3 O 0.1649(3) 0.5716(3) 0.0253(2) 0.1543(16) Uani 1 1 d . . .
O4 O 0.2136(3) 0.4820(4) -0.0617(2) 0.1494(18) Uani 1 1 d . . .
O5 O 0.19207(19) 0.88889(18) 0.05551(14) 0.0885(8) Uani 1 1 d . . .
O6 O 0.2082(2) 0.8612(2) 0.16880(14) 0.1046(9) Uani 1 1 d . . .
O7 O -0.0454(2) 0.94770(19) 0.13068(13) 0.0853(8) Uani 1 1 d . . .
O8 O 0.01506(18) 1.03942(17) 0.22246(12) 0.0773(7) Uani 1 1 d . . .
H1N H 0.279(2) 0.911(2) -0.0465(15) 0.069(10) Uiso 1 1 d . . .
H2N H 0.173(3) 1.067(2) -0.0585(16) 0.079(11) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C18 1.178(5) . ?
C1 C2 1.506(5) . ?
C1 C16 1.513(5) 3_575 ?
C2 C3 1.367(4) . ?
C2 N1 1.374(4) . ?
C3 C4 1.408(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.354(4) . ?
C4 H4 0.9300 . ?
C5 N1 1.381(4) . ?
C5 C6 1.524(4) . ?
C6 C7 1.490(4) . ?
C6 C26 1.545(5) . ?
C6 C25 1.549(4) . ?
C7 C8 1.349(4) . ?
C7 N2 1.392(4) . ?
C8 C9 1.422(4) . ?
C8 H8 0.9300 . ?
C9 C10 1.366(4) . ?
C9 H9 0.9300 . ?
C10 N2 1.370(4) . ?
C10 C11 1.506(4) . ?
C11 C12 1.518(4) . ?
C11 C27 1.558(4) . ?
C11 H11 0.9800 . ?
C12 C17 1.381(4) . ?
C12 C13 1.384(4) . ?
C13 C14 1.386(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.390(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.381(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.398(4) . ?
C16 C1 1.513(5) 3_575 ?
C17 H17 0.9300 . ?
C18 C19 1.509(7) . ?
C18 C22 1.537(8) . ?
C19 O1 1.171(7) . ?
C19 O2 1.325(8) . ?
C20 O2 1.425(4) . ?
C20 C21 1.466(5) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 O3 1.177(7) . ?
C22 O4 1.283(8) . ?
C23 C24 1.341(6) . ?
C23 O4 1.462(6) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 C31 1.506(4) . ?
C27 C28 1.510(4) . ?
C27 H27 0.9800 . ?
C28 O5 1.187(4) . ?
C28 O6 1.320(4) . ?
C29 C30 1.396(5) . ?
C29 O6 1.459(4) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 O7 1.216(4) . ?
C31 O8 1.313(4) . ?
C32 C33 1.451(5) . ?
C32 O8 1.470(4) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
N1 H1N 0.98(3) . ?
N2 H2N 0.99(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C18 C1 C2 124.5(4) . . ?
C18 C1 C16 122.7(4) . 3_575 ?
C2 C1 C16 112.7(3) . 3_575 ?
C3 C2 N1 106.3(3) . . ?
C3 C2 C1 131.4(5) . . ?
N1 C2 C1 122.3(4) . . ?
C2 C3 C4 107.7(3) . . ?
C2 C3 H3 126.1 . . ?
C4 C3 H3 126.1 . . ?
C5 C4 C3 109.2(3) . . ?
C5 C4 H4 125.4 . . ?
C3 C4 H4 125.4 . . ?
C4 C5 N1 105.8(3) . . ?
C4 C5 C6 131.3(3) . . ?
N1 C5 C6 122.8(3) . . ?
C7 C6 C5 111.3(3) . . ?
C7 C6 C26 110.0(3) . . ?
C5 C6 C26 108.6(3) . . ?
C7 C6 C25 109.7(3) . . ?
C5 C6 C25 109.0(3) . . ?
C26 C6 C25 108.2(3) . . ?
C8 C7 N2 106.3(3) . . ?
C8 C7 C6 133.0(3) . . ?
N2 C7 C6 120.6(4) . . ?
C7 C8 C9 108.9(3) . . ?
C7 C8 H8 125.5 . . ?
C9 C8 H8 125.5 . . ?
C10 C9 C8 107.3(3) . . ?
C10 C9 H9 126.3 . . ?
C8 C9 H9 126.3 . . ?
C9 C10 N2 107.2(3) . . ?
C9 C10 C11 132.7(3) . . ?
N2 C10 C11 119.6(3) . . ?
C10 C11 C12 116.5(3) . . ?
C10 C11 C27 109.1(3) . . ?
C12 C11 C27 109.9(2) . . ?
C10 C11 H11 107.0 . . ?
C12 C11 H11 107.0 . . ?
C27 C11 H11 107.0 . . ?
C17 C12 C13 117.6(3) . . ?
C17 C12 C11 120.1(3) . . ?
C13 C12 C11 122.2(3) . . ?
C12 C13 C14 121.1(3) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 H13 119.5 . . ?
C13 C14 C15 119.6(3) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C16 C15 C14 121.3(3) . . ?
C16 C15 H15 119.4 . . ?
C14 C15 H15 119.4 . . ?
C15 C16 C17 117.1(3) . . ?
C15 C16 C1 122.7(4) . 3_575 ?
C17 C16 C1 120.2(4) . 3_575 ?
C12 C17 C16 123.4(3) . . ?
C12 C17 H17 118.3 . . ?
C16 C17 H17 118.3 . . ?
C1 C18 C19 127.1(4) . . ?
C1 C18 C22 125.7(4) . . ?
C19 C18 C22 107.0(4) . . ?
O1 C19 O2 122.1(6) . . ?
O1 C19 C18 122.2(9) . . ?
O2 C19 C18 115.6(7) . . ?
O2 C20 C21 109.7(4) . . ?
O2 C20 H20A 109.7 . . ?
C21 C20 H20A 109.7 . . ?
O2 C20 H20B 109.7 . . ?
C21 C20 H20B 109.7 . . ?
H20A C20 H20B 108.2 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O3 C22 O4 124.2(7) . . ?
O3 C22 C18 119.7(9) . . ?
O4 C22 C18 116.1(8) . . ?
C24 C23 O4 115.3(5) . . ?
C24 C23 H23A 108.4 . . ?
O4 C23 H23A 108.4 . . ?
C24 C23 H23B 108.4 . . ?
O4 C23 H23B 108.4 . . ?
H23A C23 H23B 107.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C6 C25 H25A 109.5 . . ?
C6 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C6 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C6 C26 H26A 109.5 . . ?
C6 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C6 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C31 C27 C28 108.5(3) . . ?
C31 C27 C11 108.1(3) . . ?
C28 C27 C11 112.9(3) . . ?
C31 C27 H27 109.1 . . ?
C28 C27 H27 109.1 . . ?
C11 C27 H27 109.1 . . ?
O5 C28 O6 124.9(4) . . ?
O5 C28 C27 125.5(4) . . ?
O6 C28 C27 109.6(3) . . ?
C30 C29 O6 111.8(4) . . ?
C30 C29 H29A 109.3 . . ?
O6 C29 H29A 109.3 . . ?
C30 C29 H29B 109.3 . . ?
O6 C29 H29B 109.3 . . ?
H29A C29 H29B 107.9 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O7 C31 O8 125.2(3) . . ?
O7 C31 C27 122.5(3) . . ?
O8 C31 C27 112.3(3) . . ?
C33 C32 O8 106.5(3) . . ?
C33 C32 H32A 110.4 . . ?
O8 C32 H32A 110.4 . . ?
C33 C32 H32B 110.4 . . ?
O8 C32 H32B 110.4 . . ?
H32A C32 H32B 108.6 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C2 N1 C5 111.0(3) . . ?
C2 N1 H1N 123.4(16) . . ?
C5 N1 H1N 124.9(17) . . ?
C10 N2 C7 110.2(3) . . ?
C10 N2 H2N 123.0(16) . . ?
C7 N2 H2N 126.2(16) . . ?
C19 O2 C20 117.6(4) . . ?
C22 O4 C23 118.2(5) . . ?
C28 O6 C29 117.3(3) . . ?
C31 O8 C32 116.2(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
C18 C1 C2 C3 87.9(9) . . . . ?
C16 C1 C2 C3 -95.7(5) 3_575 . . . ?
C18 C1 C2 N1 -95.1(8) . . . . ?
C16 C1 C2 N1 81.3(5) 3_575 . . . ?
N1 C2 C3 C4 0.1(4) . . . . ?
C1 C2 C3 C4 177.5(4) . . . . ?
C2 C3 C4 C5 -0.2(4) . . . . ?
C3 C4 C5 N1 0.3(4) . . . . ?
C3 C4 C5 C6 -176.4(3) . . . . ?
C4 C5 C6 C7 -172.2(4) . . . . ?
N1 C5 C6 C7 11.6(5) . . . . ?
C4 C5 C6 C26 66.6(4) . . . . ?
N1 C5 C6 C26 -109.6(3) . . . . ?
C4 C5 C6 C25 -51.1(5) . . . . ?
N1 C5 C6 C25 132.8(3) . . . . ?
C5 C6 C7 C8 109.1(4) . . . . ?
C26 C6 C7 C8 -130.4(4) . . . . ?
C25 C6 C7 C8 -11.5(5) . . . . ?
C5 C6 C7 N2 -67.9(4) . . . . ?
C26 C6 C7 N2 52.6(4) . . . . ?
C25 C6 C7 N2 171.4(3) . . . . ?
N2 C7 C8 C9 1.6(4) . . . . ?
C6 C7 C8 C9 -175.8(3) . . . . ?
C7 C8 C9 C10 -1.1(4) . . . . ?
C8 C9 C10 N2 0.2(4) . . . . ?
C8 C9 C10 C11 171.4(3) . . . . ?
C9 C10 C11 C12 79.3(5) . . . . ?
N2 C10 C11 C12 -110.4(3) . . . . ?
C9 C10 C11 C27 -45.8(5) . . . . ?
N2 C10 C11 C27 124.5(3) . . . . ?
C10 C11 C12 C17 137.8(3) . . . . ?
C27 C11 C12 C17 -97.5(3) . . . . ?
C10 C11 C12 C13 -46.4(4) . . . . ?
C27 C11 C12 C13 78.3(3) . . . . ?
C17 C12 C13 C14 1.8(5) . . . . ?
C11 C12 C13 C14 -174.2(3) . . . . ?
C12 C13 C14 C15 -1.3(5) . . . . ?
C13 C14 C15 C16 0.4(5) . . . . ?
C14 C15 C16 C17 -0.1(5) . . . . ?
C14 C15 C16 C1 -179.0(4) . . . 3_575 ?
C13 C12 C17 C16 -1.5(5) . . . . ?
C11 C12 C17 C16 174.6(3) . . . . ?
C15 C16 C17 C12 0.7(5) . . . . ?
C1 C16 C17 C12 179.5(3) 3_575 . . . ?
C2 C1 C18 C19 -2.0(14) . . . . ?
C16 C1 C18 C19 -178.0(8) 3_575 . . . ?
C2 C1 C18 C22 -175.2(7) . . . . ?
C16 C1 C18 C22 8.7(14) 3_575 . . . ?
C1 C18 C19 O1 108.2(10) . . . . ?
C22 C18 C19 O1 -77.5(9) . . . . ?
C1 C18 C19 O2 -70.4(11) . . . . ?
C22 C18 C19 O2 103.9(7) . . . . ?
C1 C18 C22 O3 -86.6(11) . . . . ?
C19 C18 C22 O3 99.0(8) . . . . ?
C1 C18 C22 O4 92.7(11) . . . . ?
C19 C18 C22 O4 -81.7(8) . . . . ?
C10 C11 C27 C31 -176.7(3) . . . . ?
C12 C11 C27 C31 54.5(3) . . . . ?
C10 C11 C27 C28 -56.7(3) . . . . ?
C12 C11 C27 C28 174.5(3) . . . . ?
C31 C27 C28 O5 109.4(4) . . . . ?
C11 C27 C28 O5 -10.3(5) . . . . ?
C31 C27 C28 O6 -70.2(4) . . . . ?
C11 C27 C28 O6 170.1(3) . . . . ?
C28 C27 C31 O7 -51.9(4) . . . . ?
C11 C27 C31 O7 70.8(4) . . . . ?
C28 C27 C31 O8 129.9(3) . . . . ?
C11 C27 C31 O8 -107.4(3) . . . . ?
C3 C2 N1 C5 0.1(4) . . . . ?
C1 C2 N1 C5 -177.7(3) . . . . ?
C4 C5 N1 C2 -0.2(4) . . . . ?
C6 C5 N1 C2 176.8(3) . . . . ?
C9 C10 N2 C7 0.8(4) . . . . ?
C11 C10 N2 C7 -171.8(3) . . . . ?
C8 C7 N2 C10 -1.5(4) . . . . ?
C6 C7 N2 C10 176.2(3) . . . . ?
O1 C19 O2 C20 -2.0(8) . . . . ?
C18 C19 O2 C20 176.6(4) . . . . ?
C21 C20 O2 C19 -170.0(4) . . . . ?
O3 C22 O4 C23 0.4(10) . . . . ?
C18 C22 O4 C23 -178.9(4) . . . . ?
C24 C23 O4 C22 136.2(7) . . . . ?
O5 C28 O6 C29 -5.8(5) . . . . ?
C27 C28 O6 C29 173.8(3) . . . . ?
C30 C29 O6 C28 -129.1(5) . . . . ?
O7 C31 O8 C32 -3.2(5) . . . . ?
C27 C31 O8 C32 175.0(3) . . . . ?
C33 C32 O8 C31 -163.4(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.035
_database_code_depnum_ccdc_archive 'CCDC 957472'

data_yk623sadp21c

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C64 H78 N6 O16'
_chemical_formula_weight         1187.32

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                   10.0275(9)
_cell_length_b                   28.009(3)
_cell_length_c                   11.9161(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.138(2)
_cell_angle_gamma                90.00
_cell_volume                     3142.2(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1430
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      20.02

_exptl_crystal_description       rod
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1264
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.995
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_process_details   '(SADABS; Bruker, 1997)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17540
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_sigmaI/netI    0.0961
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         26.00
_reflns_number_total             6163
_reflns_number_gt                3221
_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)+(0.0652P)²+0.8201P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0039(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6163
_refine_ls_number_parameters     403
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1321
_refine_ls_R_factor_gt           0.0645
_refine_ls_wR_factor_ref         0.1781
_refine_ls_wR_factor_gt          0.1495
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6861(3) -0.15216(10) 0.2859(3) 0.0439(7) Uani 1 1 d . . .
C2 C 0.5973(3) -0.15967(12) 0.1721(3) 0.0580(9) Uani 1 1 d . . .
H2 H 0.5976 -0.1861 0.1250 0.070 Uiso 1 1 calc R . .
C3 C 0.5049(3) -0.12052(12) 0.1380(3) 0.0579(9) Uani 1 1 d . . .
H3 H 0.4336 -0.1166 0.0641 0.070 Uiso 1 1 calc R . .
C4 C 0.5369(3) -0.08911(10) 0.2311(3) 0.0433(7) Uani 1 1 d . . .
C5 C 0.4698(3) -0.04199(10) 0.2444(2) 0.0406(7) Uani 1 1 d . . .
C6 C 0.5659(3) -0.00011(10) 0.2439(2) 0.0387(7) Uani 1 1 d . . .
C7 C 0.5508(3) 0.03519(11) 0.1622(3) 0.0463(8) Uani 1 1 d . . .
H7 H 0.4732 0.0395 0.0925 0.056 Uiso 1 1 calc R . .
C8 C 0.6734(3) 0.06433(11) 0.2016(3) 0.0492(8) Uani 1 1 d . . .
H8 H 0.6904 0.0911 0.1624 0.059 Uiso 1 1 calc R . .
C9 C 0.7621(3) 0.04639(10) 0.3067(2) 0.0383(7) Uani 1 1 d . . .
C10 C 0.9100(3) 0.06042(10) 0.3819(2) 0.0370(7) Uani 1 1 d . . .
H10 H 0.9547 0.0328 0.4308 0.044 Uiso 1 1 calc R . .
C11 C 0.9174(3) 0.10228(10) 0.4666(2) 0.0392(7) Uani 1 1 d . . .
C12 C 0.8031(3) 0.11538(12) 0.4991(3) 0.0553(9) Uani 1 1 d . . .
H12 H 0.7172 0.0992 0.4684 0.066 Uiso 1 1 calc R . .
C13 C 0.8180(3) 0.15254(13) 0.5773(3) 0.0661(10) Uani 1 1 d . . .
H13 H 0.7421 0.1619 0.6002 0.079 Uiso 1 1 calc R . .
C14 C 0.9469(3) 0.17606(12) 0.6218(3) 0.0550(9) Uani 1 1 d . . .
H14 H 0.9591 0.2013 0.6750 0.066 Uiso 1 1 calc R . .
C15 C 1.0567(3) 0.16139(10) 0.5858(2) 0.0383(7) Uani 1 1 d . . .
C16 C 1.2026(3) 0.18434(10) 0.6331(3) 0.0433(7) Uani 1 1 d . . .
H16 H 1.1950 0.2121 0.6806 0.052 Uiso 1 1 calc R . .
C17 C 0.3305(3) -0.03637(11) 0.1389(3) 0.0543(9) Uani 1 1 d . . .
H17A H 0.3503 -0.0355 0.0656 0.081 Uiso 1 1 calc R . .
H17B H 0.2847 -0.0072 0.1476 0.081 Uiso 1 1 calc R . .
H17C H 0.2692 -0.0629 0.1373 0.081 Uiso 1 1 calc R . .
C18 C 0.4337(3) -0.04244(11) 0.3598(3) 0.0502(8) Uani 1 1 d . . .
H18A H 0.3779 -0.0702 0.3607 0.075 Uiso 1 1 calc R . .
H18B H 0.3807 -0.0143 0.3631 0.075 Uiso 1 1 calc R . .
H18C H 0.5199 -0.0431 0.4278 0.075 Uiso 1 1 calc R . .
C19 C 0.9953(3) 0.07199(10) 0.2994(2) 0.0408(7) Uani 1 1 d . . .
H19 H 0.9624 0.1028 0.2610 0.049 Uiso 1 1 calc R . .
C20 C 0.9733(3) 0.03457(14) 0.2011(3) 0.0554(9) Uani 1 1 d . . .
C21 C 0.9682(4) -0.04936(16) 0.1622(4) 0.0889(14) Uani 1 1 d . . .
H21A H 0.9969 -0.0400 0.0955 0.107 Uiso 1 1 calc R . .
H21B H 1.0275 -0.0759 0.2026 0.107 Uiso 1 1 calc R . .
C22 C 0.8227(4) -0.06430(16) 0.1182(4) 0.0938(14) Uani 1 1 d . . .
H22A H 0.7952 -0.0748 0.1837 0.141 Uiso 1 1 calc R . .
H22B H 0.8116 -0.0901 0.0625 0.141 Uiso 1 1 calc R . .
H22C H 0.7637 -0.0380 0.0787 0.141 Uiso 1 1 calc R . .
C23 C 1.1539(3) 0.07488(10) 0.3613(3) 0.0387(7) Uani 1 1 d . . .
C24 C 1.3639(3) 0.10683(12) 0.3401(3) 0.0584(9) Uani 1 1 d . . .
H24A H 1.4009 0.0756 0.3314 0.070 Uiso 1 1 calc R . .
H24B H 1.4061 0.1168 0.4228 0.070 Uiso 1 1 calc R . .
C25 C 1.3966(4) 0.14164(16) 0.2602(4) 0.0923(14) Uani 1 1 d . . .
H25A H 1.3547 0.1312 0.1788 0.138 Uiso 1 1 calc R . .
H25B H 1.4977 0.1440 0.2805 0.138 Uiso 1 1 calc R . .
H25C H 1.3588 0.1723 0.2693 0.138 Uiso 1 1 calc R . .
C26 C 1.2436(3) 0.20339(11) 0.5270(3) 0.0476(8) Uani 1 1 d . . .
H26 H 1.2272 0.1772 0.4693 0.057 Uiso 1 1 calc R . .
C27 C 1.1529(4) 0.24405(14) 0.4627(4) 0.0657(10) Uani 1 1 d . . .
C28 C 1.0176(6) 0.31177(18) 0.4764(6) 0.137(2) Uani 1 1 d . . .
H28A H 1.0774 0.3384 0.4718 0.165 Uiso 1 1 calc R . .
H28B H 0.9564 0.3040 0.3959 0.165 Uiso 1 1 calc R . .
C29 C 0.9354(8) 0.3247(2) 0.5443(6) 0.192(4) Uani 1 1 d . . .
H29A H 0.8680 0.2999 0.5405 0.287 Uiso 1 1 calc R . .
H29B H 0.8857 0.3538 0.5135 0.287 Uiso 1 1 calc R . .
H29C H 0.9955 0.3294 0.6258 0.287 Uiso 1 1 calc R . .
C30 C 1.3988(4) 0.21602(13) 0.5635(3) 0.0638(10) Uani 1 1 d . . .
C31 C 1.5869(8) 0.2767(2) 0.6456(7) 0.157(3) Uani 1 1 d . . .
H31A H 1.6297 0.2639 0.5904 0.188 Uiso 1 1 calc R . .
H31B H 1.5907 0.3113 0.6464 0.188 Uiso 1 1 calc R . .
C32 C 1.6387(8) 0.2573(2) 0.7549(7) 0.163(3) Uani 1 1 d . . .
H32A H 1.5818 0.2671 0.8012 0.245 Uiso 1 1 calc R . .
H32B H 1.7349 0.2677 0.7937 0.245 Uiso 1 1 calc R . .
H32C H 1.6367 0.2231 0.7482 0.245 Uiso 1 1 calc R . .
N1 N 0.6482(2) -0.10900(9) 0.3215(2) 0.0413(6) Uani 1 1 d . . .
N2 N 0.6947(2) 0.00708(9) 0.3326(2) 0.0386(6) Uani 1 1 d . . .
N3 N 1.0427(2) 0.12515(8) 0.50883(19) 0.0391(6) Uani 1 1 d . . .
O1 O 0.9505(3) 0.04495(11) 0.0986(2) 0.0860(9) Uani 1 1 d . . .
O2 O 0.9895(2) -0.00898(9) 0.2456(2) 0.0664(7) Uani 1 1 d . . .
O3 O 1.2232(2) 0.05044(7) 0.44466(17) 0.0450(5) Uani 1 1 d . . .
O4 O 1.2096(2) 0.10518(7) 0.30510(18) 0.0522(6) Uani 1 1 d . . .
O5 O 1.1251(5) 0.25088(14) 0.3583(3) 0.1438(15) Uani 1 1 d . . .
O6 O 1.1058(3) 0.27090(10) 0.5292(3) 0.0913(9) Uani 1 1 d . . .
O7 O 1.4862(3) 0.19183(10) 0.5433(3) 0.0963(10) Uani 1 1 d . . .
O8 O 1.4297(3) 0.25578(10) 0.6244(3) 0.1132(13) Uani 1 1 d . . .
H2N H 0.727(3) -0.0095(11) 0.397(3) 0.056(10) Uiso 1 1 d . . .
H1N H 0.695(3) -0.0956(11) 0.393(3) 0.059(10) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.358(4) . ?
C1 N1 1.377(4) . ?
C1 C16 1.500(4) 3_756 ?
C2 C3 1.402(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.365(4) . ?
C3 H3 0.9300 . ?
C4 N1 1.374(3) . ?
C4 C5 1.514(4) . ?
C5 C6 1.520(4) . ?
C5 C17 1.532(4) . ?
C5 C18 1.538(4) . ?
C6 C7 1.359(4) . ?
C6 N2 1.373(3) . ?
C7 C8 1.415(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.358(4) . ?
C8 H8 0.9300 . ?
C9 N2 1.381(4) . ?
C9 C10 1.497(4) . ?
C10 C11 1.532(4) . ?
C10 C19 1.544(4) . ?
C10 H10 0.9800 . ?
C11 N3 1.344(3) . ?
C11 C12 1.380(4) . ?
C12 C13 1.370(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.384(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.375(4) . ?
C14 H14 0.9300 . ?
C15 N3 1.342(3) . ?
C15 C16 1.518(4) . ?
C16 C1 1.500(4) 3_756 ?
C16 C26 1.552(4) . ?
C16 H16 0.9800 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 C23 1.508(4) . ?
C19 C20 1.530(4) . ?
C19 H19 0.9800 . ?
C20 O1 1.198(4) . ?
C20 O2 1.318(4) . ?
C21 C22 1.433(5) . ?
C21 O2 1.472(4) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 O3 1.209(3) . ?
C23 O4 1.318(3) . ?
C24 O4 1.458(3) . ?
C24 C25 1.476(5) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 C27 1.494(5) . ?
C26 C30 1.507(4) . ?
C26 H26 0.9800 . ?
C27 O5 1.194(5) . ?
C27 O6 1.293(4) . ?
C28 C29 1.387(8) . ?
C28 O6 1.451(5) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 O7 1.196(4) . ?
C30 O8 1.307(4) . ?
C31 C32 1.340(8) . ?
C31 O8 1.618(7) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
N1 H1N 0.90(3) . ?
N2 H2N 0.86(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 N1 106.7(3) . . ?
C2 C1 C16 129.6(3) . 3_756 ?
N1 C1 C16 123.5(2) . 3_756 ?
C1 C2 C3 108.0(3) . . ?
C1 C2 H2 126.0 . . ?
C3 C2 H2 126.0 . . ?
C4 C3 C2 108.8(3) . . ?
C4 C3 H3 125.6 . . ?
C2 C3 H3 125.6 . . ?
C3 C4 N1 106.0(3) . . ?
C3 C4 C5 131.2(3) . . ?
N1 C4 C5 122.8(2) . . ?
C4 C5 C6 111.5(2) . . ?
C4 C5 C17 108.4(2) . . ?
C6 C5 C17 108.5(2) . . ?
C4 C5 C18 109.7(2) . . ?
C6 C5 C18 110.8(2) . . ?
C17 C5 C18 107.8(2) . . ?
C7 C6 N2 106.7(2) . . ?
C7 C6 C5 130.6(2) . . ?
N2 C6 C5 122.7(2) . . ?
C6 C7 C8 108.2(3) . . ?
C6 C7 H7 125.9 . . ?
C8 C7 H7 125.9 . . ?
C9 C8 C7 108.1(3) . . ?
C9 C8 H8 125.9 . . ?
C7 C8 H8 125.9 . . ?
C8 C9 N2 106.6(2) . . ?
C8 C9 C10 130.8(3) . . ?
N2 C9 C10 122.4(2) . . ?
C9 C10 C11 114.1(2) . . ?
C9 C10 C19 109.0(2) . . ?
C11 C10 C19 110.3(2) . . ?
C9 C10 H10 107.7 . . ?
C11 C10 H10 107.7 . . ?
C19 C10 H10 107.7 . . ?
N3 C11 C12 121.9(3) . . ?
N3 C11 C10 116.0(2) . . ?
C12 C11 C10 122.1(3) . . ?
C13 C12 C11 119.1(3) . . ?
C13 C12 H12 120.4 . . ?
C11 C12 H12 120.4 . . ?
C12 C13 C14 119.4(3) . . ?
C12 C13 H13 120.3 . . ?
C14 C13 H13 120.3 . . ?
C15 C14 C13 118.8(3) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
N3 C15 C14 122.2(3) . . ?
N3 C15 C16 115.8(2) . . ?
C14 C15 C16 122.1(3) . . ?
C1 C16 C15 113.2(2) 3_756 . ?
C1 C16 C26 112.6(2) 3_756 . ?
C15 C16 C26 109.6(2) . . ?
C1 C16 H16 107.1 3_756 . ?
C15 C16 H16 107.1 . . ?
C26 C16 H16 107.1 . . ?
C5 C17 H17A 109.5 . . ?
C5 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C5 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C5 C18 H18A 109.5 . . ?
C5 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C5 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C23 C19 C20 105.2(2) . . ?
C23 C19 C10 115.0(2) . . ?
C20 C19 C10 112.2(2) . . ?
C23 C19 H19 108.1 . . ?
C20 C19 H19 108.1 . . ?
C10 C19 H19 108.1 . . ?
O1 C20 O2 126.1(3) . . ?
O1 C20 C19 122.7(4) . . ?
O2 C20 C19 111.1(3) . . ?
C22 C21 O2 111.4(3) . . ?
C22 C21 H21A 109.4 . . ?
O2 C21 H21A 109.4 . . ?
C22 C21 H21B 109.4 . . ?
O2 C21 H21B 109.4 . . ?
H21A C21 H21B 108.0 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O3 C23 O4 123.9(3) . . ?
O3 C23 C19 125.7(3) . . ?
O4 C23 C19 110.2(2) . . ?
O4 C24 C25 106.6(3) . . ?
O4 C24 H24A 110.4 . . ?
C25 C24 H24A 110.4 . . ?
O4 C24 H24B 110.4 . . ?
C25 C24 H24B 110.4 . . ?
H24A C24 H24B 108.6 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 C30 110.8(3) . . ?
C27 C26 C16 113.2(3) . . ?
C30 C26 C16 112.4(3) . . ?
C27 C26 H26 106.6 . . ?
C30 C26 H26 106.6 . . ?
C16 C26 H26 106.6 . . ?
O5 C27 O6 122.8(4) . . ?
O5 C27 C26 122.6(4) . . ?
O6 C27 C26 114.6(3) . . ?
C29 C28 O6 110.4(5) . . ?
C29 C28 H28A 109.6 . . ?
O6 C28 H28A 109.6 . . ?
C29 C28 H28B 109.6 . . ?
O6 C28 H28B 109.6 . . ?
H28A C28 H28B 108.1 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O7 C30 O8 123.0(3) . . ?
O7 C30 C26 124.3(3) . . ?
O8 C30 C26 112.6(3) . . ?
C32 C31 O8 92.1(6) . . ?
C32 C31 H31A 113.3 . . ?
O8 C31 H31A 113.3 . . ?
C32 C31 H31B 113.3 . . ?
O8 C31 H31B 113.3 . . ?
H31A C31 H31B 110.6 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C4 N1 C1 110.5(2) . . ?
C4 N1 H1N 126(2) . . ?
C1 N1 H1N 123(2) . . ?
C6 N2 C9 110.4(2) . . ?
C6 N2 H2N 125(2) . . ?
C9 N2 H2N 124(2) . . ?
C15 N3 C11 118.7(2) . . ?
C20 O2 C21 118.0(3) . . ?
C23 O4 C24 117.9(2) . . ?
C27 O6 C28 119.3(4) . . ?
C30 O8 C31 115.3(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
N1 C1 C2 C3 0.3(4) . . . . ?
C16 C1 C2 C3 175.3(3) 3_756 . . . ?
C1 C2 C3 C4 -0.2(4) . . . . ?
C2 C3 C4 N1 0.0(4) . . . . ?
C2 C3 C4 C5 -178.4(3) . . . . ?
C3 C4 C5 C6 -108.7(4) . . . . ?
N1 C4 C5 C6 73.1(4) . . . . ?
C3 C4 C5 C17 10.7(5) . . . . ?
N1 C4 C5 C17 -167.5(3) . . . . ?
C3 C4 C5 C18 128.2(4) . . . . ?
N1 C4 C5 C18 -50.0(4) . . . . ?
C4 C5 C6 C7 112.0(3) . . . . ?
C17 C5 C6 C7 -7.3(4) . . . . ?
C18 C5 C6 C7 -125.5(3) . . . . ?
C4 C5 C6 N2 -65.6(3) . . . . ?
C17 C5 C6 N2 175.1(3) . . . . ?
C18 C5 C6 N2 56.8(3) . . . . ?
N2 C6 C7 C8 0.4(3) . . . . ?
C5 C6 C7 C8 -177.5(3) . . . . ?
C6 C7 C8 C9 0.1(4) . . . . ?
C7 C8 C9 N2 -0.6(3) . . . . ?
C7 C8 C9 C10 174.3(3) . . . . ?
C8 C9 C10 C11 83.7(4) . . . . ?
N2 C9 C10 C11 -102.0(3) . . . . ?
C8 C9 C10 C19 -40.1(4) . . . . ?
N2 C9 C10 C19 134.2(3) . . . . ?
C9 C10 C11 N3 -161.0(2) . . . . ?
C19 C10 C11 N3 -37.9(3) . . . . ?
C9 C10 C11 C12 19.9(4) . . . . ?
C19 C10 C11 C12 143.0(3) . . . . ?
N3 C11 C12 C13 -0.5(5) . . . . ?
C10 C11 C12 C13 178.6(3) . . . . ?
C11 C12 C13 C14 0.0(5) . . . . ?
C12 C13 C14 C15 0.1(5) . . . . ?
C13 C14 C15 N3 0.2(5) . . . . ?
C13 C14 C15 C16 -178.2(3) . . . . ?
N3 C15 C16 C1 -68.3(3) . . . 3_756 ?
C14 C15 C16 C1 110.1(3) . . . 3_756 ?
N3 C15 C16 C26 58.2(3) . . . . ?
C14 C15 C16 C26 -123.3(3) . . . . ?
C9 C10 C19 C23 -165.6(2) . . . . ?
C11 C10 C19 C23 68.3(3) . . . . ?
C9 C10 C19 C20 -45.5(3) . . . . ?
C11 C10 C19 C20 -171.6(2) . . . . ?
C23 C19 C20 O1 -100.2(3) . . . . ?
C10 C19 C20 O1 134.2(3) . . . . ?
C23 C19 C20 O2 76.9(3) . . . . ?
C10 C19 C20 O2 -48.8(3) . . . . ?
C20 C19 C23 O3 -88.5(3) . . . . ?
C10 C19 C23 O3 35.5(4) . . . . ?
C20 C19 C23 O4 86.0(3) . . . . ?
C10 C19 C23 O4 -150.1(2) . . . . ?
C1 C16 C26 C27 -166.2(3) 3_756 . . . ?
C15 C16 C26 C27 67.0(3) . . . . ?
C1 C16 C26 C30 -39.6(3) 3_756 . . . ?
C15 C16 C26 C30 -166.4(3) . . . . ?
C30 C26 C27 O5 84.1(5) . . . . ?
C16 C26 C27 O5 -148.5(4) . . . . ?
C30 C26 C27 O6 -96.6(4) . . . . ?
C16 C26 C27 O6 30.9(4) . . . . ?
C27 C26 C30 O7 -129.2(4) . . . . ?
C16 C26 C30 O7 103.0(4) . . . . ?
C27 C26 C30 O8 53.3(4) . . . . ?
C16 C26 C30 O8 -74.5(4) . . . . ?
C3 C4 N1 C1 0.2(3) . . . . ?
C5 C4 N1 C1 178.7(3) . . . . ?
C2 C1 N1 C4 -0.3(4) . . . . ?
C16 C1 N1 C4 -175.7(3) 3_756 . . . ?
C7 C6 N2 C9 -0.8(3) . . . . ?
C5 C6 N2 C9 177.3(2) . . . . ?
C8 C9 N2 C6 0.9(3) . . . . ?
C10 C9 N2 C6 -174.5(2) . . . . ?
C14 C15 N3 C11 -0.6(4) . . . . ?
C16 C15 N3 C11 177.9(2) . . . . ?
C12 C11 N3 C15 0.7(4) . . . . ?
C10 C11 N3 C15 -178.4(2) . . . . ?
O1 C20 O2 C21 -4.6(5) . . . . ?
C19 C20 O2 C21 178.5(3) . . . . ?
C22 C21 O2 C20 -88.8(4) . . . . ?
O3 C23 O4 C24 4.5(4) . . . . ?
C19 C23 O4 C24 -170.1(2) . . . . ?
C25 C24 O4 C23 177.4(3) . . . . ?
O5 C27 O6 C28 -1.3(6) . . . . ?
C26 C27 O6 C28 179.4(4) . . . . ?
C29 C28 O6 C27 157.2(6) . . . . ?
O7 C30 O8 C31 13.3(7) . . . . ?
C26 C30 O8 C31 -169.2(4) . . . . ?
C32 C31 O8 C30 -97.4(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.045
_database_code_depnum_ccdc_archive 'CCDC 957473'
