# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Parimal Bharadwaj'
_publ_contact_author_email       PKB@IITK.AC.IN

_publ_section_title              
;
Diversity of binding of sulfate and nitrate
anions with laterally asymmetric aza cryptands
;
loop_
_publ_author_name
'Parimal Bharadwaj'
'Madhab C. Das'
'Sujit K. Ghosh'

# Attachment 'All.cif'

data_complex1
_database_code_depnum_ccdc_archive 'CCDC 727164'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H55 N5 O21 S4'
_chemical_formula_sum            'C33 H55 N5 O21 S4'
_chemical_formula_weight         986.06

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           Monoclinic
_symmetry_space_group_name_H-M   'P 21/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                   18.732(6)
_cell_length_b                   12.684(5)
_cell_length_c                   19.629(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.496(4)
_cell_angle_gamma                90.00
_cell_volume                     4277(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.1
_cell_measurement_theta_max      28.4

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2080
_exptl_absorpt_coefficient_mu    0.311
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9405
_exptl_absorpt_correction_T_max  0.9520
_exptl_absorpt_process_details   'SADABS 2.10 (Bruker 2003)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       /w-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            28224
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_sigmaI/netI    0.0783
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         28.35
_reflns_number_total             10598
_reflns_number_gt                6934
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART 5.628 (Bruker, 2003)'
_computing_cell_refinement       'SAINT 6.45 ( Bruker, 2003)'
_computing_data_reduction        'SAINT 6.45 (Bruker, 2003)'
_computing_structure_solution    SIR-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond 2.1e'
_computing_publication_material  ?

_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)+(0.0722P)²+0.4810P] 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         10598
_refine_ls_number_parameters     559
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0614
_refine_ls_wR_factor_ref         0.2051
_refine_ls_wR_factor_gt          0.1467
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.084
_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
S1 S 0.46333(7) -0.13989(9) 0.77365(6) 0.0181(3) Uani 1 1 d . . .
S2 S 0.08556(7) -0.12381(10) 0.52327(7) 0.0206(3) Uani 1 1 d . . .
S3 S 0.34426(7) 0.39656(9) 0.50949(6) 0.0162(3) Uani 1 1 d . . .
S4 S 0.12628(7) 0.58558(10) 0.39411(7) 0.0198(3) Uani 1 1 d . . .
O1 O 0.21552(18) 0.0182(3) 0.47093(17) 0.0163(7) Uani 1 1 d . . .
O2 O 0.45762(18) -0.1079(2) 0.54769(18) 0.0172(7) Uani 1 1 d . . .
O3 O 0.2543(2) -0.2853(3) 0.64662(18) 0.0211(8) Uani 1 1 d . . .
O4 O 0.19221(19) 0.6554(3) 0.40907(18) 0.0209(7) Uani 1 1 d . . .
O5 O 0.1004(2) 0.5371(3) 0.32165(19) 0.0273(8) Uani 1 1 d . . .
O6 O 0.1480(2) 0.5025(3) 0.45423(19) 0.0255(8) Uani 1 1 d . . .
H6 H 0.1834 0.4660 0.4526 0.038 Uiso 1 1 calc R . .
O7 O 0.0598(2) 0.6449(3) 0.4003(2) 0.0281(9) Uani 1 1 d . . .
O8 O 0.3727(2) 0.4967(3) 0.4937(2) 0.0292(9) Uani 1 1 d . . .
O9 O 0.2609(2) 0.3826(3) 0.45512(19) 0.0282(9) Uani 1 1 d . . .
O10 O 0.3886(2) 0.3084(3) 0.5032(2) 0.0305(9) Uani 1 1 d . . .
O11 O 0.3415(2) 0.4020(3) 0.58462(18) 0.0266(8) Uani 1 1 d . . .
O12 O 0.1458(2) -0.0648(3) 0.58127(18) 0.0210(7) Uani 1 1 d . . .
O13 O 0.0307(2) -0.1703(3) 0.5541(2) 0.0275(10) Uani 1 1 d . . .
O14 O 0.1242(2) -0.2158(3) 0.5034(2) 0.0282(9) Uani 1 1 d . . .
H14 H 0.0910 -0.2528 0.4726 0.042 Uiso 1 1 calc R . .
O15 O 0.0436(2) -0.0616(3) 0.4585(2) 0.0460(12) Uani 1 1 d . . .
O16 O 0.39962(19) -0.0870(3) 0.71444(18) 0.0198(7) Uani 1 1 d . . .
O17 O 0.4866(2) -0.2352(3) 0.74814(19) 0.0280(9) Uani 1 1 d . . .
O18 O 0.4448(2) -0.1616(3) 0.83837(19) 0.0243(8) Uani 1 1 d . . .
O19 O 0.5306(2) -0.0611(3) 0.7977(2) 0.0340(10) Uani 1 1 d . . .
H19 H 0.5685 -0.0866 0.8315 0.051 Uiso 1 1 calc R . .
OW1 O 0.0492(3) -0.0120(8) 0.6752(3) 0.036(4) Uani 1 1 d . . .
H1W1 H 0.0346(6) -0.0441(7) 0.6968(9) 0.046(8) Uiso 1 1 d . . .
H2W1 H 0.0194(8) -0.0016(7) 0.6353(5) 0.053(10) Uiso 1 1 d . . .
OW2 O 0.4637(6) 0.0186(6) 0.9144(5) 0.039(4) Uani 1 1 d . . .
H1W2 H 0.4211(9) 0.0500(6) 0.9278(11) 0.050(9) Uiso 1 1 d . . .
N1 N 0.3145(2) -0.2416(3) 0.5190(2) 0.0149(8) Uani 1 1 d . . .
H1 H 0.2705 -0.2751 0.4882 0.018 Uiso 1 1 calc R . .
N2 N 0.2555(2) 0.1449(3) 0.7004(2) 0.0153(8) Uani 1 1 d . . .
H2 H 0.2371 0.0910 0.6674 0.018 Uiso 1 1 calc R . .
N3 N 0.1288(2) 0.1548(3) 0.5443(2) 0.0160(8) Uani 1 1 d . . .
H3A H 0.0791 0.1428 0.5130 0.019 Uiso 1 1 calc R . .
H3B H 0.1521 0.0919 0.5588 0.019 Uiso 1 1 calc R . .
N4 N 0.4349(2) 0.1013(3) 0.6660(2) 0.0136(8) Uani 1 1 d . . .
H4A H 0.4687 0.1430 0.7012 0.016 Uiso 1 1 calc R . .
H4B H 0.4383 0.0362 0.6854 0.016 Uiso 1 1 calc R . .
N5 N 0.2119(2) -0.0741(3) 0.7400(2) 0.0215(9) Uani 1 1 d . . .
H5A H 0.2105 -0.0637 0.6941 0.026 Uiso 1 1 calc R . .
H5B H 0.1635 -0.0640 0.7380 0.026 Uiso 1 1 calc R . .
C1 C 0.2896(3) -0.1329(4) 0.5302(3) 0.0163(9) Uani 1 1 d . . .
H1A H 0.3352 -0.0902 0.5569 0.020 Uiso 1 1 calc R . .
H1B H 0.2589 -0.1369 0.5598 0.020 Uiso 1 1 calc R . .
C2 C 0.2414(3) -0.0809(4) 0.4553(2) 0.0175(10) Uani 1 1 d . . .
H2A H 0.2729 -0.0710 0.4268 0.021 Uiso 1 1 calc R . .
H2B H 0.1972 -0.1250 0.4268 0.021 Uiso 1 1 calc R . .
C3 C 0.1691(3) 0.0770(4) 0.4096(3) 0.0155(9) Uani 1 1 d . . .
C4 C 0.1468(3) 0.0435(4) 0.3365(3) 0.0191(10) Uani 1 1 d . . .
H4 H 0.1608 -0.0230 0.3262 0.023 Uiso 1 1 calc R . .
C5 C 0.1032(3) 0.1110(4) 0.2790(3) 0.0178(10) Uani 1 1 d . . .
H5 H 0.0884 0.0891 0.2301 0.021 Uiso 1 1 calc R . .
C6 C 0.0817(3) 0.2095(4) 0.2932(2) 0.0176(10) Uani 1 1 d . . .
H6A H 0.0529 0.2541 0.2543 0.021 Uiso 1 1 calc R . .
C7 C 0.1034(3) 0.2416(4) 0.3664(3) 0.0175(10) Uani 1 1 d . . .
H7 H 0.0892 0.3082 0.3764 0.021 Uiso 1 1 calc R . .
C8 C 0.1466(3) 0.1751(4) 0.4254(2) 0.0147(9) Uani 1 1 d . . .
C9 C 0.1694(3) 0.2139(4) 0.5033(2) 0.0174(10) Uani 1 1 d . . .
H9A H 0.1569 0.2882 0.5021 0.021 Uiso 1 1 calc R . .
H9B H 0.2252 0.2064 0.5300 0.021 Uiso 1 1 calc R . .
C10 C 0.1293(3) 0.2123(4) 0.6109(3) 0.0196(10) Uani 1 1 d . . .
H10A H 0.1040 0.1690 0.6355 0.024 Uiso 1 1 calc R . .
H10B H 0.0995 0.2767 0.5948 0.024 Uiso 1 1 calc R . .
C11 C 0.2106(3) 0.2393(4) 0.6658(3) 0.0173(10) Uani 1 1 d . . .
H11A H 0.2375 0.2778 0.6404 0.021 Uiso 1 1 calc R . .
H11B H 0.2072 0.2848 0.7041 0.021 Uiso 1 1 calc R . .
C12 C 0.3695(3) -0.2445(4) 0.4800(2) 0.0162(10) Uani 1 1 d . . .
H12A H 0.3682 -0.3147 0.4599 0.019 Uiso 1 1 calc R . .
H12B H 0.3506 -0.1959 0.4384 0.019 Uiso 1 1 calc R . .
C13 C 0.4529(3) -0.2173(3) 0.5276(3) 0.0157(9) Uani 1 1 d . . .
H13A H 0.4715 -0.2606 0.5720 0.019 Uiso 1 1 calc R . .
H13B H 0.4853 -0.2309 0.5004 0.019 Uiso 1 1 calc R . .
C14 C 0.5289(3) -0.0698(4) 0.5930(2) 0.0147(9) Uani 1 1 d . . .
C15 C 0.5979(3) -0.1270(4) 0.6114(3) 0.0169(10) Uani 1 1 d . . .
H15 H 0.5968 -0.1945 0.5925 0.020 Uiso 1 1 calc R . .
C16 C 0.6677(3) -0.0826(4) 0.6578(3) 0.0171(10) Uani 1 1 d . . .
H16 H 0.7135 -0.1207 0.6699 0.021 Uiso 1 1 calc R . .
C17 C 0.6706(3) 0.0172(4) 0.6864(3) 0.0191(10) Uani 1 1 d . . .
H17 H 0.7179 0.0456 0.7184 0.023 Uiso 1 1 calc R . .
C18 C 0.6024(3) 0.0751(4) 0.6669(3) 0.0180(10) Uani 1 1 d . . .
H18 H 0.6044 0.1431 0.6853 0.022 Uiso 1 1 calc R . .
C19 C 0.5312(3) 0.0325(3) 0.6201(2) 0.0191(9) Uani 1 1 d . . .
C20 C 0.4577(3) 0.0965(4) 0.6009(2) 0.0152(9) Uani 1 1 d . . .
H20A H 0.4661 0.1673 0.5870 0.018 Uiso 1 1 calc R . .
H20B H 0.4160 0.0647 0.5588 0.018 Uiso 1 1 calc R . .
C21 C 0.3537(3) 0.1426(4) 0.6460(2) 0.0157(9) Uani 1 1 d . . .
C22 C 0.3388(3) 0.1572(4) 0.7163(2) 0.0155(9) Uani 1 1 d . . .
H22A H 0.3686 0.1056 0.7532 0.019 Uiso 1 1 calc R . .
H22B H 0.3560 0.2269 0.7367 0.019 Uiso 1 1 calc R . .
C23 C 0.3456(3) -0.3056(4) 0.5898(2) 0.0167(10) Uani 1 1 d . . .
H23A H 0.3802 -0.3597 0.5854 0.020 Uiso 1 1 calc R . .
H23B H 0.3759 -0.2600 0.6308 0.020 Uiso 1 1 calc R . .
C24 C 0.2824(3) -0.3571(4) 0.6069(3) 0.0199(10) Uani 1 1 d . . .
H24A H 0.2400 -0.3780 0.5611 0.024 Uiso 1 1 calc R . .
H24B H 0.3026 -0.4199 0.6366 0.024 Uiso 1 1 calc R . .
C25 C 0.1910(3) -0.3188(4) 0.6596(3) 0.0186(10) Uani 1 1 d . . .
C26 C 0.1403(3) -0.3972(4) 0.6200(3) 0.0208(10) Uani 1 1 d . . .
H26 H 0.1485 -0.4321 0.5821 0.025 Uiso 1 1 calc R . .
C27 C 0.0774(3) -0.4240(4) 0.6367(3) 0.0200(10) Uani 1 1 d . . .
H27 H 0.0433 -0.4768 0.6098 0.024 Uiso 1 1 calc R . .
C28 C 0.0651(3) -0.3724(4) 0.6934(3) 0.0222(11) Uani 1 1 d . . .
H28 H 0.0227 -0.3899 0.7044 0.027 Uiso 1 1 calc R . .
C29 C 0.1166(3) -0.2945(4) 0.7336(3) 0.0195(10) Uani 1 1 d . . .
H29 H 0.1088 -0.2607 0.7721 0.023 Uiso 1 1 calc R . .
C30 C 0.1793(3) -0.2663(4) 0.7175(3) 0.0176(10) Uani 1 1 d . . .
C31 C 0.2367(3) -0.1847(4) 0.7637(3) 0.0182(10) Uani 1 1 d . . .
H31A H 0.2440 -0.1930 0.8152 0.022 Uiso 1 1 calc R . .
H31B H 0.2865 -0.1973 0.7608 0.022 Uiso 1 1 calc R . .
C32 C 0.2658(3) 0.0035(4) 0.7921(3) 0.0187(10) Uani 1 1 d . . .
H32A H 0.3182 -0.0095 0.7957 0.022 Uiso 1 1 calc R . .
H32B H 0.2657 -0.0062 0.8411 0.022 Uiso 1 1 calc R . .
C33 C 0.2434(3) 0.1160(4) 0.7674(3) 0.0183(10) Uani 1 1 d . . .
H33A H 0.1890 0.1263 0.7580 0.022 Uiso 1 1 calc R . .
H33B H 0.2738 0.1631 0.8075 0.022 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
S1 O17 1.442(4) . ?
S1 O16 1.456(3) . ?
S1 O18 1.470(4) . ?
S1 O19 1.528(4) . ?
S2 O15 1.435(4) . ?
S2 O12 1.451(3) . ?
S2 O14 1.505(4) . ?
S2 O13 1.505(4) . ?
S3 O10 1.427(4) . ?
S3 O8 1.458(4) . ?
S3 O11 1.498(4) . ?
S3 O9 1.510(4) . ?
S4 O5 1.445(3) . ?
S4 O4 1.451(3) . ?
S4 O7 1.501(4) . ?
S4 O6 1.512(4) . ?
O1 C3 1.387(5) . ?
O1 C2 1.424(6) . ?
O2 C14 1.364(5) . ?
O2 C13 1.435(5) . ?
O3 C25 1.376(6) . ?
O3 C24 1.429(6) . ?
O6 H6 0.8200 . ?
O14 H14 0.8200 . ?
O19 H19 0.8200 . ?
OW1 H1W1 0.716(15) . ?
OW1 H2W1 0.771(11) . ?
OW2 H1W2 1.02(2) . ?
N1 C1 1.500(6) . ?
N1 C12 1.509(6) . ?
N1 C23 1.512(6) . ?
N1 H1 0.9100 . ?
N2 C11 1.465(6) . ?
N2 C33 1.468(6) . ?
N2 C22 1.472(6) . ?
N2 H2 0.9100 . ?
N3 C10 1.492(6) . ?
N3 C9 1.509(6) . ?
N3 H3A 0.9000 . ?
N3 H3B 0.9000 . ?
N4 C20 1.502(5) . ?
N4 C21 1.504(6) . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
N5 C32 1.488(6) . ?
N5 C31 1.492(6) . ?
N5 H5A 0.9000 . ?
N5 H5B 0.9000 . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C1 1.533(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C4 C3 1.391(6) . ?
C4 C5 1.392(7) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 C5 1.376(7) . ?
C6 H6A 0.9300 . ?
C7 C6 1.388(6) . ?
C7 C8 1.400(6) . ?
C7 H7 0.9300 . ?
C8 C3 1.389(6) . ?
C8 C9 1.496(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C10 1.513(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.505(6) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C15 C16 1.380(6) . ?
C15 C14 1.398(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.377(7) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C17 1.388(7) . ?
C18 H18 0.9300 . ?
C19 C18 1.392(6) . ?
C19 C14 1.397(6) . ?
C19 C20 1.511(6) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.525(6) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C23 1.504(6) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C26 C25 1.379(7) . ?
C26 C27 1.385(7) . ?
C26 H26 0.9300 . ?
C27 H27 0.9300 . ?
C28 C27 1.388(7) . ?
C28 H28 0.9300 . ?
C29 C30 1.380(7) . ?
C29 C28 1.387(7) . ?
C29 H29 0.9300 . ?
C30 C25 1.407(6) . ?
C30 C31 1.507(6) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C32 1.511(7) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O17 S1 O16 112.0(2) . . ?
O17 S1 O18 110.6(2) . . ?
O16 S1 O18 112.0(2) . . ?
O17 S1 O19 109.2(2) . . ?
O16 S1 O19 104.9(2) . . ?
O18 S1 O19 107.8(2) . . ?
O15 S2 O12 113.0(2) . . ?
O15 S2 O14 110.3(3) . . ?
O12 S2 O14 107.4(2) . . ?
O15 S2 O13 110.5(3) . . ?
O12 S2 O13 109.2(2) . . ?
O14 S2 O13 106.0(2) . . ?
O10 S3 O8 112.9(2) . . ?
O10 S3 O11 111.8(2) . . ?
O8 S3 O11 109.2(2) . . ?
O10 S3 O9 108.7(2) . . ?
O8 S3 O9 108.3(2) . . ?
O11 S3 O9 105.6(2) . . ?
O5 S4 O4 112.6(2) . . ?
O5 S4 O7 109.2(2) . . ?
O4 S4 O7 110.1(2) . . ?
O5 S4 O6 110.6(2) . . ?
O4 S4 O6 109.0(2) . . ?
O7 S4 O6 105.1(2) . . ?
S4 O6 H6 109.5 . . ?
C3 O1 C2 115.9(3) . . ?
C14 O2 C13 117.3(3) . . ?
C25 O3 C24 115.9(4) . . ?
S2 O14 H14 109.5 . . ?
S1 O19 H19 109.5 . . ?
H2W1 OW1 H1W1 114.0(9) . . ?
C1 N1 C12 114.4(3) . . ?
C1 N1 C23 112.8(3) . . ?
C12 N1 C23 111.2(4) . . ?
C1 N1 H1 105.9 . . ?
C12 N1 H1 105.9 . . ?
C23 N1 H1 105.9 . . ?
C11 N2 C33 110.7(4) . . ?
C11 N2 C22 112.1(4) . . ?
C33 N2 C22 111.4(4) . . ?
C11 N2 H2 107.5 . . ?
C33 N2 H2 107.5 . . ?
C22 N2 H2 107.5 . . ?
C10 N3 C9 113.3(4) . . ?
C10 N3 H3A 108.9 . . ?
C9 N3 H3A 108.9 . . ?
C10 N3 H3B 108.9 . . ?
C9 N3 H3B 108.9 . . ?
H3A N3 H3B 107.7 . . ?
C20 N4 C21 113.2(3) . . ?
C20 N4 H4A 108.9 . . ?
C21 N4 H4A 108.9 . . ?
C20 N4 H4B 108.9 . . ?
C21 N4 H4B 108.9 . . ?
H4A N4 H4B 107.8 . . ?
C32 N5 C31 111.5(4) . . ?
C32 N5 H5A 109.3 . . ?
C31 N5 H5A 109.3 . . ?
C32 N5 H5B 109.3 . . ?
C31 N5 H5B 109.3 . . ?
H5A N5 H5B 108.0 . . ?
N1 C1 C2 110.7(4) . . ?
N1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
O1 C2 C1 107.1(3) . . ?
O1 C2 H2A 110.3 . . ?
C1 C2 H2A 110.3 . . ?
O1 C2 H2B 110.3 . . ?
C1 C2 H2B 110.3 . . ?
H2A C2 H2B 108.5 . . ?
O1 C3 C8 115.4(4) . . ?
O1 C3 C4 123.9(4) . . ?
C8 C3 C4 120.7(4) . . ?
C3 C4 C5 119.1(5) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
C6 C5 C4 121.3(4) . . ?
C6 C5 H5 119.4 . . ?
C4 C5 H5 119.4 . . ?
C5 C6 C7 119.1(4) . . ?
C5 C6 H6A 120.4 . . ?
C7 C6 H6A 120.4 . . ?
C6 C7 C8 120.9(5) . . ?
C6 C7 H7 119.5 . . ?
C8 C7 H7 119.5 . . ?
C3 C8 C7 118.8(4) . . ?
C3 C8 C9 122.3(4) . . ?
C7 C8 C9 118.9(4) . . ?
C8 C9 N3 112.5(4) . . ?
C8 C9 H9A 109.1 . . ?
N3 C9 H9A 109.1 . . ?
C8 C9 H9B 109.1 . . ?
N3 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
N3 C10 C11 112.8(4) . . ?
N3 C10 H10A 109.0 . . ?
C11 C10 H10A 109.0 . . ?
N3 C10 H10B 109.0 . . ?
C11 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
N2 C11 C10 111.9(4) . . ?
N2 C11 H11A 109.2 . . ?
C10 C11 H11A 109.2 . . ?
N2 C11 H11B 109.2 . . ?
C10 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
C13 C12 N1 115.4(4) . . ?
C13 C12 H12A 108.4 . . ?
N1 C12 H12A 108.4 . . ?
C13 C12 H12B 108.4 . . ?
N1 C12 H12B 108.4 . . ?
H12A C12 H12B 107.5 . . ?
O2 C13 C12 109.1(4) . . ?
O2 C13 H13A 109.9 . . ?
C12 C13 H13A 109.9 . . ?
O2 C13 H13B 109.9 . . ?
C12 C13 H13B 109.9 . . ?
H13A C13 H13B 108.3 . . ?
O2 C14 C19 116.8(4) . . ?
O2 C14 C15 123.3(4) . . ?
C19 C14 C15 119.9(4) . . ?
C16 C15 C14 119.6(4) . . ?
C16 C15 H15 120.2 . . ?
C14 C15 H15 120.2 . . ?
C17 C16 C15 121.2(4) . . ?
C17 C16 H16 119.4 . . ?
C15 C16 H16 119.4 . . ?
C16 C17 C18 119.4(4) . . ?
C16 C17 H17 120.3 . . ?
C18 C17 H17 120.3 . . ?
C17 C18 C19 120.7(4) . . ?
C17 C18 H18 119.6 . . ?
C19 C18 H18 119.6 . . ?
C18 C19 C14 119.2(4) . . ?
C18 C19 C20 119.6(4) . . ?
C14 C19 C20 121.2(4) . . ?
N4 C20 C19 110.5(4) . . ?
N4 C20 H20A 109.6 . . ?
C19 C20 H20A 109.6 . . ?
N4 C20 H20B 109.6 . . ?
C19 C20 H20B 109.6 . . ?
H20A C20 H20B 108.1 . . ?
N4 C21 C22 109.7(3) . . ?
N2 C22 C21 110.8(4) . . ?
N2 C22 H22A 109.5 . . ?
C21 C22 H22A 109.5 . . ?
N2 C22 H22B 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 108.1 . . ?
C24 C23 N1 113.0(4) . . ?
C24 C23 H23A 109.0 . . ?
N1 C23 H23A 109.0 . . ?
C24 C23 H23B 109.0 . . ?
N1 C23 H23B 109.0 . . ?
H23A C23 H23B 107.8 . . ?
O3 C24 C23 109.9(4) . . ?
O3 C24 H24A 109.7 . . ?
C23 C24 H24A 109.7 . . ?
O3 C24 H24B 109.7 . . ?
C23 C24 H24B 109.7 . . ?
H24A C24 H24B 108.2 . . ?
O3 C25 C26 124.6(4) . . ?
O3 C25 C30 115.2(4) . . ?
C26 C25 C30 120.2(4) . . ?
C25 C26 C27 120.2(5) . . ?
C25 C26 H26 119.9 . . ?
C27 C26 H26 119.9 . . ?
C26 C27 C28 120.1(5) . . ?
C26 C27 H27 120.0 . . ?
C28 C27 H27 120.0 . . ?
C29 C28 C27 119.6(5) . . ?
C29 C28 H28 120.2 . . ?
C27 C28 H28 120.2 . . ?
C28 C29 H29 119.5 . . ?
C30 C29 C28 121.1(5) . . ?
C30 C29 H29 119.5 . . ?
C29 C30 C25 118.9(4) . . ?
C29 C30 C31 120.5(4) . . ?
C25 C30 C31 120.5(4) . . ?
N5 C31 C30 113.5(4) . . ?
N5 C31 H31A 108.9 . . ?
C30 C31 H31A 108.9 . . ?
N5 C31 H31B 108.9 . . ?
C30 C31 H31B 108.9 . . ?
H31A C31 H31B 107.7 . . ?
N5 C32 C33 112.3(4) . . ?
N5 C32 H32A 109.1 . . ?
C33 C32 H32A 109.1 . . ?
N5 C32 H32B 109.1 . . ?
C33 C32 H32B 109.1 . . ?
H32A C32 H32B 107.9 . . ?
N2 C33 C32 113.6(4) . . ?
N2 C33 H33A 108.8 . . ?
C32 C33 H33A 108.8 . . ?
N2 C33 H33B 108.8 . . ?
C32 C33 H33B 108.8 . . ?
H33A C33 H33B 107.7 . . ?

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
C12 N1 C1 C2 65.0(5) . . . . ?
C23 N1 C1 C2 -166.6(4) . . . . ?
O1 C2 C1 N1 175.9(3) . . . . ?
C3 O1 C2 C1 -178.8(4) . . . . ?
C2 O1 C3 C8 -177.8(4) . . . . ?
C2 O1 C3 C4 1.0(6) . . . . ?
C7 C8 C3 O1 176.4(4) . . . . ?
C9 C8 C3 O1 -1.2(6) . . . . ?
C7 C8 C3 C4 -2.4(7) . . . . ?
C9 C8 C3 C4 180.0(4) . . . . ?
C5 C4 C3 O1 -176.9(4) . . . . ?
C5 C4 C3 C8 1.8(7) . . . . ?
C8 C7 C6 C5 -0.2(7) . . . . ?
C7 C6 C5 C4 -0.5(7) . . . . ?
C3 C4 C5 C6 -0.3(7) . . . . ?
C6 C7 C8 C3 1.6(7) . . . . ?
C6 C7 C8 C9 179.3(4) . . . . ?
C3 C8 C9 N3 -70.0(5) . . . . ?
C7 C8 C9 N3 112.4(5) . . . . ?
C10 N3 C9 C8 -161.1(4) . . . . ?
C9 N3 C10 C11 -56.7(5) . . . . ?
N2 C11 C10 N3 -66.9(5) . . . . ?
C33 N2 C11 C10 -88.6(4) . . . . ?
C22 N2 C11 C10 146.4(4) . . . . ?
C1 N1 C12 C13 77.9(5) . . . . ?
C23 N1 C12 C13 -51.3(5) . . . . ?
C14 O2 C13 C12 178.0(3) . . . . ?
N1 C12 C13 O2 -67.7(5) . . . . ?
C13 O2 C14 C19 -171.8(4) . . . . ?
C13 O2 C14 C15 9.5(6) . . . . ?
C18 C19 C14 O2 179.7(4) . . . . ?
C20 C19 C14 O2 0.9(6) . . . . ?
C18 C19 C14 C15 -1.6(6) . . . . ?
C20 C19 C14 C15 179.7(4) . . . . ?
C16 C15 C14 O2 -179.9(4) . . . . ?
C16 C15 C14 C19 1.4(7) . . . . ?
C14 C15 C16 C17 0.1(7) . . . . ?
C15 C16 C17 C18 -1.4(7) . . . . ?
C19 C18 C17 C16 1.3(7) . . . . ?
C14 C19 C18 C17 0.2(7) . . . . ?
C20 C19 C18 C17 179.0(4) . . . . ?
C21 N4 C20 C19 -167.2(4) . . . . ?
C18 C19 C20 N4 -73.9(5) . . . . ?
C14 C19 C20 N4 104.9(5) . . . . ?
C20 N4 C21 C22 -173.3(4) . . . . ?
C11 N2 C22 C21 -78.3(5) . . . . ?
C33 N2 C22 C21 156.9(4) . . . . ?
N4 C21 C22 N2 -151.6(4) . . . . ?
O3 C24 C23 N1 -85.7(5) . . . . ?
C1 N1 C23 C24 83.0(5) . . . . ?
C12 N1 C23 C24 -147.0(4) . . . . ?
C25 O3 C24 C23 174.0(4) . . . . ?
C24 O3 C25 C26 -20.4(7) . . . . ?
C24 O3 C25 C30 160.2(4) . . . . ?
C27 C26 C25 O3 -178.9(5) . . . . ?
C27 C26 C25 C30 0.5(7) . . . . ?
C29 C30 C25 O3 179.4(4) . . . . ?
C31 C30 C25 O3 -3.8(7) . . . . ?
C29 C30 C25 C26 -0.1(7) . . . . ?
C31 C30 C25 C26 176.7(4) . . . . ?
C25 C26 C27 C28 -0.2(7) . . . . ?
C29 C28 C27 C26 -0.5(7) . . . . ?
C30 C29 C28 C27 1.0(7) . . . . ?
C28 C29 C30 C25 -0.6(7) . . . . ?
C28 C29 C30 C31 -177.4(4) . . . . ?
C32 N5 C31 C30 173.8(4) . . . . ?
C29 C30 C31 N5 -84.5(6) . . . . ?
C25 C30 C31 N5 98.7(5) . . . . ?
C31 N5 C32 C33 177.8(4) . . . . ?
N2 C33 C32 N5 -69.4(5) . . . . ?
C11 N2 C33 C32 161.5(4) . . . . ?
C22 N2 C33 C32 -73.0(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        28.35
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.127

data_complex2
_database_code_depnum_ccdc_archive 'CCDC 727165'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H53 N9 O17'
_chemical_formula_sum            'C33 H53 N9 O17'
_chemical_formula_weight         847.84

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   'P 21/n'

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

_cell_length_a                   10.947(4)
_cell_length_b                   25.408(6)
_cell_length_c                   15.235(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.129(2)
_cell_angle_gamma                90.00
_cell_volume                     4071(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.1
_cell_measurement_theta_max      28.3

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1800
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9812
_exptl_absorpt_correction_T_max  0.9845
_exptl_absorpt_process_details   'SADABS 2.10 (Bruker 2003)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       /w-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26981
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0563
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.10
_diffrn_reflns_theta_max         28.31
_reflns_number_total             10042
_reflns_number_gt                7156
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART 5.628 (Bruker, 2003)'
_computing_cell_refinement       'SAINT 6.45 ( Bruker, 2003)'
_computing_data_reduction        'SAINT 6.45 (Bruker, 2003)'
_computing_structure_solution    SIR-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond 2.1e'
_computing_publication_material  ?

_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)+(0.0920P)²+0.5151P] 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         10042
_refine_ls_number_parameters     548
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0617
_refine_ls_wR_factor_ref         0.2042
_refine_ls_wR_factor_gt          0.1589
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.062
_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 -0.22217(19) 0.24170(8) 0.31926(14) 0.0216(4) Uani 1 1 d . . .
O2 O 0.1689(2) 0.22734(8) 0.19518(14) 0.0234(5) Uani 1 1 d . . .
O3 O 0.2213(2) 0.11119(8) 0.43576(15) 0.0298(5) Uani 1 1 d . . .
O4 O -0.0206(3) 0.06585(11) 0.49317(18) 0.0448(7) Uani 1 1 d . . .
O5 O -0.1759(2) 0.09905(10) 0.53545(16) 0.0342(6) Uani 1 1 d . . .
O6 O -0.1388(2) 0.12596(10) 0.41006(16) 0.0332(6) Uani 1 1 d . . .
O7 O -0.3948(3) -0.02082(15) -0.0900(3) 0.0357(10) Uani 1 1 d . . .
O8 O -0.2661(3) -0.00025(11) -0.1665(2) 0.0362(8) Uani 1 1 d . . .
O9 O -0.3479(3) -0.07733(13) -0.1855(3) 0.0424(11) Uani 1 1 d . . .
O10 O -0.1762(2) 0.13253(9) -0.11294(15) 0.0277(5) Uani 1 1 d . . .
O11 O -0.0142(2) 0.09444(9) -0.14260(15) 0.0302(5) Uani 1 1 d . . .
O12 O -0.1896(2) 0.10446(9) -0.24994(14) 0.0311(5) Uani 1 1 d . . .
O13 O -0.2322(2) 0.21847(10) 0.05345(14) 0.0301(5) Uani 1 1 d . . .
O14 O -0.10350(19) 0.19029(8) 0.17991(13) 0.0197(4) Uani 1 1 d . . .
O15 O -0.1314(2) 0.27419(8) 0.15637(15) 0.0239(5) Uani 1 1 d . . .
OW1 O -0.4171(3) 0.09255(14) -0.1130(2) 0.0409(7) Uani 1 1 d D . .
H1W1 H -0.404(10) 0.0611(11) -0.112(7) 0.039(5) Uiso 1 1 d D . .
H2W1 H -0.346(5) 0.1039(18) -0.119(3) 0.044(13) Uiso 1 1 d . . .
OW2 O -0.4774(3) -0.12235(13) -0.02159(18) 0.0400(7) Uani 1 1 d . . .
H1W2 H -0.5244(7) -0.1228(6) 0.0151(8) 0.037(8) Uiso 1 1 d D . .
H2W2 H -0.418(9) -0.099(6) -0.002(11) 0.033(9) Uiso 1 1 d D . .
N1 N -0.1205(2) 0.06252(10) 0.15737(16) 0.0212(5) Uani 1 1 d . . .
N2 N 0.0527(2) 0.23259(9) 0.34392(16) 0.0181(5) Uani 1 1 d . . .
H1N2 H -0.008(3) 0.2282(13) 0.293(2) 0.018(8) Uiso 1 1 d . . .
N3 N -0.3287(2) 0.13064(9) 0.18117(17) 0.0195(5) Uani 1 1 d . . .
H3C H -0.3773 0.1334 0.1231 0.023 Uiso 1 1 calc R . .
H3D H -0.2518 0.1443 0.1842 0.023 Uiso 1 1 calc R . .
N4 N 0.0063(2) 0.13136(9) 0.05424(17) 0.0202(5) Uani 1 1 d . . .
H4A H -0.0219 0.1449 0.0997 0.024 Uiso 1 1 calc R . .
H4B H -0.0569 0.1339 0.0020 0.024 Uiso 1 1 calc R . .
N5 N 0.0923(3) 0.00553(11) 0.37978(18) 0.0297(6) Uani 1 1 d . . .
H5A H 0.0809 -0.0232 0.4112 0.036 Uiso 1 1 calc R . .
H5B H 0.0700 0.0337 0.4077 0.036 Uiso 1 1 calc R . .
N6 N -0.1138(3) 0.09729(10) 0.47882(17) 0.0245(6) Uani 1 1 d . . .
N7 N -0.3350(3) -0.03248(14) -0.1470(3) 0.0370(9) Uani 1 1 d . . .
N8 N -0.1263(3) 0.10992(10) -0.17050(17) 0.0238(5) Uani 1 1 d . . .
N9 N -0.1572(2) 0.22881(10) 0.12834(16) 0.0181(5) Uani 1 1 d . . .
C1 C -0.2482(3) 0.04282(12) 0.1509(2) 0.0235(6) Uani 1 1 d . . .
C2 C -0.3147(3) 0.07384(12) 0.2083(2) 0.0228(6) Uani 1 1 d . . .
H2A H -0.3982 0.0588 0.2019 0.027 Uiso 1 1 calc R . .
H2B H -0.2665 0.0712 0.2721 0.027 Uiso 1 1 calc R . .
C3 C -0.3886(3) 0.16131(12) 0.2429(2) 0.0217(6) Uani 1 1 d . . .
H3A H -0.3325 0.1602 0.3046 0.026 Uiso 1 1 calc R . .
H3B H -0.4677 0.1443 0.2436 0.026 Uiso 1 1 calc R . .
C4 C -0.4157(3) 0.21807(12) 0.2151(2) 0.0197(6) Uani 1 1 d . . .
C5 C -0.5270(3) 0.23231(13) 0.1504(2) 0.0257(7) Uani 1 1 d . . .
H5 H -0.5824 0.2061 0.1205 0.031 Uiso 1 1 calc R . .
C6 C -0.5578(3) 0.28470(13) 0.1291(2) 0.0271(7) Uani 1 1 d . . .
H6 H -0.6319 0.2934 0.0844 0.033 Uiso 1 1 calc R . .
C7 C -0.4773(3) 0.32379(13) 0.1751(2) 0.0260(7) Uani 1 1 d . . .
H7 H -0.4984 0.3590 0.1624 0.031 Uiso 1 1 calc R . .
C8 C -0.3652(3) 0.31075(12) 0.2398(2) 0.0252(6) Uani 1 1 d . . .
H8 H -0.3116 0.3372 0.2709 0.030 Uiso 1 1 calc R . .
C9 C -0.3326(3) 0.25836(12) 0.25847(19) 0.0198(6) Uani 1 1 d . . .
C10 C -0.1336(3) 0.28036(12) 0.3686(2) 0.0230(6) Uani 1 1 d . . .
H10A H -0.1664 0.2977 0.4141 0.028 Uiso 1 1 calc R . .
H10B H -0.1171 0.3067 0.3273 0.028 Uiso 1 1 calc R . .
C11 C -0.0148(3) 0.25018(12) 0.41324(19) 0.0218(6) Uani 1 1 d . . .
H11A H -0.0365 0.2196 0.4439 0.026 Uiso 1 1 calc R . .
H11B H 0.0418 0.2722 0.4589 0.026 Uiso 1 1 calc R . .
C12 C -0.0709(3) 0.04276(12) 0.0839(2) 0.0237(6) Uani 1 1 d . . .
H12A H -0.1381 0.0436 0.0268 0.028 Uiso 1 1 calc R . .
H12B H -0.0444 0.0065 0.0965 0.028 Uiso 1 1 calc R . .
C13 C 0.0401(3) 0.07488(12) 0.0738(2) 0.0245(6) Uani 1 1 d . . .
H13A H 0.1091 0.0724 0.1296 0.029 Uiso 1 1 calc R . .
H13B H 0.0699 0.0604 0.0245 0.029 Uiso 1 1 calc R . .
C14 C 0.1189(3) 0.16237(13) 0.0456(2) 0.0260(7) Uani 1 1 d . . .
H14A H 0.1427 0.1500 -0.0076 0.031 Uiso 1 1 calc R . .
H14B H 0.1899 0.1557 0.0988 0.031 Uiso 1 1 calc R . .
C15 C 0.0960(3) 0.22067(12) 0.0369(2) 0.0231(6) Uani 1 1 d . . .
C16 C 0.0481(3) 0.24349(15) -0.0494(2) 0.0300(7) Uani 1 1 d . . .
H16 H 0.0254 0.2222 -0.1011 0.036 Uiso 1 1 calc R . .
C17 C 0.0343(3) 0.29758(15) -0.0583(2) 0.0323(8) Uani 1 1 d . . .
H17 H 0.0019 0.3125 -0.1159 0.039 Uiso 1 1 calc R . .
C18 C 0.0686(3) 0.32932(13) 0.0178(2) 0.0288(7) Uani 1 1 d . . .
H18 H 0.0608 0.3657 0.0112 0.035 Uiso 1 1 calc R . .
C19 C 0.1145(3) 0.30774(13) 0.1040(2) 0.0249(6) Uani 1 1 d . . .
H19 H 0.1373 0.3293 0.1552 0.030 Uiso 1 1 calc R . .
C20 C 0.1262(3) 0.25359(12) 0.1132(2) 0.0208(6) Uani 1 1 d . . .
C21 C 0.2330(3) 0.25539(13) 0.27626(19) 0.0237(6) Uani 1 1 d . . .
H21A H 0.2754 0.2857 0.2594 0.028 Uiso 1 1 calc R . .
H21B H 0.2978 0.2328 0.3143 0.028 Uiso 1 1 calc R . .
C22 C 0.1456(3) 0.27400(11) 0.3316(2) 0.0210(6) Uani 1 1 d . . .
H22A H 0.1969 0.2852 0.3914 0.025 Uiso 1 1 calc R . .
H22B H 0.0982 0.3044 0.3016 0.025 Uiso 1 1 calc R . .
C23 C -0.0302(3) 0.05769(11) 0.2483(2) 0.0214(6) Uani 1 1 d . . .
H23A H -0.0645 0.0768 0.2912 0.026 Uiso 1 1 calc R . .
H23B H 0.0481 0.0751 0.2469 0.026 Uiso 1 1 calc R . .
C24 C 0.0029(4) 0.00195(13) 0.2855(2) 0.0339(8) Uani 1 1 d . . .
H24A H -0.0738 -0.0165 0.2875 0.041 Uiso 1 1 calc R . .
H24B H 0.0426 -0.0175 0.2460 0.041 Uiso 1 1 calc R . .
C25 C 0.2313(3) 0.00991(13) 0.3869(2) 0.0277(7) Uani 1 1 d . . .
H25A H 0.2439 0.0348 0.3421 0.033 Uiso 1 1 calc R . .
H25B H 0.2637 -0.0240 0.3746 0.033 Uiso 1 1 calc R . .
C26 C 0.3023(3) 0.02806(12) 0.4816(2) 0.0236(6) Uani 1 1 d . . .
C27 C 0.3759(3) -0.00565(13) 0.5467(2) 0.0298(7) Uani 1 1 d . . .
H27 H 0.3834 -0.0408 0.5318 0.036 Uiso 1 1 calc R . .
C28 C 0.4390(3) 0.01224(13) 0.6339(2) 0.0322(8) Uani 1 1 d . . .
H28 H 0.4894 -0.0106 0.6767 0.039 Uiso 1 1 calc R . .
C29 C 0.4258(4) 0.06426(14) 0.6563(2) 0.0338(8) Uani 1 1 d . . .
H29 H 0.4668 0.0762 0.7148 0.041 Uiso 1 1 calc R . .
C30 C 0.3522(3) 0.09921(13) 0.5926(2) 0.0308(7) Uani 1 1 d . . .
H30 H 0.3435 0.1342 0.6080 0.037 Uiso 1 1 calc R . .
C31 C 0.2923(3) 0.08059(12) 0.5059(2) 0.0244(6) Uani 1 1 d . . .
H1A H -0.2424 0.0063 0.1702 0.028 Uiso 1 1 calc R . .
H1B H -0.2988 0.0441 0.0876 0.028 Uiso 1 1 calc R . .
C32 C 0.1961(3) 0.16517(11) 0.45151(19) 0.0217(6) Uani 1 1 d . . .
H32A H 0.2721 0.1867 0.4627 0.026 Uiso 1 1 calc R . .
H32B H 0.1583 0.1691 0.5017 0.026 Uiso 1 1 calc R . .
C33 C 0.1018(3) 0.17754(11) 0.35963(19) 0.0199(6) Uani 1 1 d . . .
H33A H 0.1419 0.1690 0.3121 0.024 Uiso 1 1 calc R . .
H33B H 0.0294 0.1542 0.3519 0.024 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 C9 1.370(3) . ?
O1 C10 1.437(4) . ?
O2 C20 1.379(3) . ?
O2 C21 1.430(3) . ?
O3 C31 1.375(4) . ?
O3 C32 1.432(3) . ?
O5 N6 1.239(4) . ?
O6 N6 1.242(3) . ?
O8 N7 1.206(5) . ?
O10 N8 1.290(3) . ?
O11 N8 1.246(3) . ?
O12 N8 1.224(3) . ?
O14 N9 1.290(3) . ?
O15 N9 1.235(3) . ?
OW1 H1W1 0.81(2) . ?
OW1 H2W1 0.86(5) . ?
OW2 H1W2 0.859(10) . ?
OW2 H2W2 0.87(10) . ?
N1 C12 1.462(4) . ?
N1 C1 1.463(4) . ?
N1 C23 1.466(4) . ?
N2 C33 1.494(4) . ?
N2 C22 1.510(4) . ?
N2 C11 1.515(4) . ?
N2 H1N2 0.88(4) . ?
N3 C2 1.497(4) . ?
N3 C3 1.505(4) . ?
N3 H3C 0.9000 . ?
N3 H3D 0.9000 . ?
N4 C13 1.491(4) . ?
N4 C14 1.499(4) . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
N5 C24 1.499(4) . ?
N5 C25 1.499(5) . ?
N5 H5A 0.9000 . ?
N5 H5B 0.9000 . ?
N6 O4 1.266(4) . ?
N7 O7 1.260(5) . ?
N7 O9 1.271(5) . ?
N9 O13 1.235(3) . ?
C1 C2 1.506(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.385(4) . ?
C4 C9 1.406(4) . ?
C4 C3 1.509(4) . ?
C5 H5 0.9300 . ?
C6 C5 1.389(5) . ?
C6 H6 0.9300 . ?
C7 C6 1.382(5) . ?
C7 H7 0.9300 . ?
C8 C7 1.384(4) . ?
C8 C9 1.387(4) . ?
C8 H8 0.9300 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C10 1.500(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C12 1.507(5) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.502(4) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C16 C17 1.385(5) . ?
C16 C15 1.399(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.377(5) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C18 1.382(4) . ?
C19 C20 1.385(4) . ?
C19 H19 0.9300 . ?
C20 C15 1.395(4) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C21 1.517(4) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.531(4) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C27 1.386(4) . ?
C26 C31 1.398(4) . ?
C26 C25 1.508(4) . ?
C27 C28 1.393(5) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 C28 1.382(5) . ?
C29 H29 0.9300 . ?
C30 C29 1.394(5) . ?
C30 H30 0.9300 . ?
C31 C30 1.384(4) . ?
C32 C33 1.524(4) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C9 O1 C10 118.9(2) . . ?
C20 O2 C21 120.2(2) . . ?
C31 O3 C32 120.3(2) . . ?
H2W1 OW1 H1W1 100(8) . . ?
H1W2 OW2 H2W2 108(9) . . ?
C12 N1 C1 112.5(2) . . ?
C12 N1 C23 113.5(2) . . ?
C1 N1 C23 114.6(2) . . ?
C33 N2 C22 116.6(2) . . ?
C33 N2 C11 112.8(2) . . ?
C22 N2 C11 110.9(2) . . ?
C33 N2 H1N2 100(2) . . ?
C22 N2 H1N2 110(2) . . ?
C11 N2 H1N2 105(2) . . ?
C2 N3 C3 110.8(2) . . ?
C2 N3 H3C 109.5 . . ?
C3 N3 H3C 109.5 . . ?
C2 N3 H3D 109.5 . . ?
C3 N3 H3D 109.5 . . ?
H3C N3 H3D 108.1 . . ?
C13 N4 C14 111.0(2) . . ?
C13 N4 H4A 109.4 . . ?
C14 N4 H4A 109.4 . . ?
C13 N4 H4B 109.4 . . ?
C14 N4 H4B 109.4 . . ?
H4A N4 H4B 108.0 . . ?
C24 N5 C25 117.0(3) . . ?
C24 N5 H5A 108.1 . . ?
C25 N5 H5A 108.1 . . ?
C24 N5 H5B 108.1 . . ?
C25 N5 H5B 108.1 . . ?
H5A N5 H5B 107.3 . . ?
O5 N6 O6 122.1(3) . . ?
O5 N6 O4 118.3(3) . . ?
O6 N6 O4 119.6(3) . . ?
O8 N7 O7 119.4(4) . . ?
O8 N7 O9 119.5(4) . . ?
O7 N7 O9 121.1(4) . . ?
O12 N8 O11 122.4(3) . . ?
O12 N8 O10 119.5(3) . . ?
O11 N8 O10 118.2(2) . . ?
O13 N9 O15 123.2(2) . . ?
O13 N9 O14 118.4(2) . . ?
O15 N9 O14 118.4(2) . . ?
N1 C1 C2 112.9(2) . . ?
N1 C1 H1A 109.0 . . ?
C2 C1 H1A 109.0 . . ?
N1 C1 H1B 109.0 . . ?
C2 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
N3 C2 C1 111.9(2) . . ?
N3 C2 H2A 109.2 . . ?
C1 C2 H2A 109.2 . . ?
N3 C2 H2B 109.2 . . ?
C1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
N3 C3 C4 113.9(2) . . ?
N3 C3 H3A 108.8 . . ?
C4 C3 H3A 108.8 . . ?
N3 C3 H3B 108.8 . . ?
C4 C3 H3B 108.8 . . ?
H3A C3 H3B 107.7 . . ?
C5 C4 C9 118.1(3) . . ?
C5 C4 C3 121.0(3) . . ?
C9 C4 C3 120.9(3) . . ?
C4 C5 C6 121.7(3) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C7 C6 C5 119.4(3) . . ?
C7 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
C6 C7 C8 120.2(3) . . ?
C6 C7 H7 119.9 . . ?
C8 C7 H7 119.9 . . ?
C7 C8 C9 120.1(3) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
O1 C9 C8 124.3(3) . . ?
O1 C9 C4 115.3(3) . . ?
C8 C9 C4 120.4(3) . . ?
O1 C10 C11 105.2(2) . . ?
O1 C10 H10A 110.7 . . ?
C11 C10 H10A 110.7 . . ?
O1 C10 H10B 110.7 . . ?
C11 C10 H10B 110.7 . . ?
H10A C10 H10B 108.8 . . ?
C10 C11 N2 111.3(2) . . ?
C10 C11 H11A 109.4 . . ?
N2 C11 H11A 109.4 . . ?
C10 C11 H11B 109.4 . . ?
N2 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
N1 C12 C13 111.9(2) . . ?
N1 C12 H12A 109.2 . . ?
C13 C12 H12A 109.2 . . ?
N1 C12 H12B 109.2 . . ?
C13 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
N4 C13 C12 112.3(2) . . ?
N4 C13 H13A 109.2 . . ?
C12 C13 H13A 109.2 . . ?
N4 C13 H13B 109.2 . . ?
C12 C13 H13B 109.2 . . ?
H13A C13 H13B 107.9 . . ?
N4 C14 C15 113.9(2) . . ?
N4 C14 H14A 108.8 . . ?
C15 C14 H14A 108.8 . . ?
N4 C14 H14B 108.8 . . ?
C15 C14 H14B 108.8 . . ?
H14A C14 H14B 107.7 . . ?
C20 C15 C16 118.3(3) . . ?
C20 C15 C14 121.5(3) . . ?
C16 C15 C14 120.1(3) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 C15 120.4(3) . . ?
C17 C16 H16 119.8 . . ?
C18 C17 C16 120.1(3) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C17 C18 C19 120.7(3) . . ?
C17 C18 H18 119.7 . . ?
C19 C18 H18 119.7 . . ?
C18 C19 C20 119.3(3) . . ?
C18 C19 H19 120.4 . . ?
C20 C19 H19 120.4 . . ?
O2 C20 C19 124.8(3) . . ?
O2 C20 C15 114.0(3) . . ?
C19 C20 C15 121.2(3) . . ?
O2 C21 C22 113.7(2) . . ?
O2 C21 H21A 108.8 . . ?
C22 C21 H21A 108.8 . . ?
O2 C21 H21B 108.8 . . ?
C22 C21 H21B 108.8 . . ?
H21A C21 H21B 107.7 . . ?
N2 C22 C21 113.7(2) . . ?
N2 C22 H22A 108.8 . . ?
C21 C22 H22A 108.8 . . ?
N2 C22 H22B 108.8 . . ?
C21 C22 H22B 108.8 . . ?
H22A C22 H22B 107.7 . . ?
N1 C23 C24 117.1(2) . . ?
N1 C23 H23A 108.0 . . ?
C24 C23 H23A 108.0 . . ?
N1 C23 H23B 108.0 . . ?
C24 C23 H23B 108.0 . . ?
H23A C23 H23B 107.3 . . ?
N5 C24 C23 108.9(3) . . ?
N5 C24 H24A 109.9 . . ?
C23 C24 H24A 109.9 . . ?
N5 C24 H24B 109.9 . . ?
C23 C24 H24B 109.9 . . ?
H24A C24 H24B 108.3 . . ?
N5 C25 C26 109.6(3) . . ?
N5 C25 H25A 109.7 . . ?
C26 C25 H25A 109.7 . . ?
N5 C25 H25B 109.7 . . ?
C26 C25 H25B 109.7 . . ?
H25A C25 H25B 108.2 . . ?
C27 C26 C31 118.2(3) . . ?
C27 C26 C25 122.5(3) . . ?
C31 C26 C25 119.2(3) . . ?
C26 C27 C28 121.1(3) . . ?
C26 C27 H27 119.5 . . ?
C28 C27 H27 119.5 . . ?
C29 C28 C27 119.3(3) . . ?
C29 C28 H28 120.4 . . ?
C27 C28 H28 120.4 . . ?
C28 C29 C30 121.2(3) . . ?
C28 C29 H29 119.4 . . ?
C30 C29 H29 119.4 . . ?
C31 C30 C29 118.4(3) . . ?
C31 C30 H30 120.8 . . ?
C29 C30 H30 120.8 . . ?
O3 C31 C30 124.3(3) . . ?
O3 C31 C26 113.8(3) . . ?
C30 C31 C26 121.9(3) . . ?
O3 C32 C33 99.0(2) . . ?
O3 C32 H32A 112.0 . . ?
C33 C32 H32A 112.0 . . ?
O3 C32 H32B 112.0 . . ?
C33 C32 H32B 112.0 . . ?
H32A C32 H32B 109.7 . . ?
N2 C33 C32 117.5(2) . . ?
N2 C33 H33A 107.9 . . ?
C32 C33 H33A 107.9 . . ?
N2 C33 H33B 107.9 . . ?
C32 C33 H33B 107.9 . . ?
H33A C33 H33B 107.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C12 N1 C1 C2 -163.8(2) . . . . ?
C23 N1 C1 C2 64.6(3) . . . . ?
C3 N3 C2 C1 -176.8(2) . . . . ?
N1 C1 C2 N3 59.6(3) . . . . ?
C2 N3 C3 C4 -175.3(2) . . . . ?
C5 C4 C3 N3 85.1(3) . . . . ?
C9 C4 C3 N3 -99.3(3) . . . . ?
C9 C4 C5 C6 -0.8(4) . . . . ?
C3 C4 C5 C6 175.0(3) . . . . ?
C7 C6 C5 C4 -1.7(5) . . . . ?
C8 C7 C6 C5 1.8(5) . . . . ?
C9 C8 C7 C6 0.5(5) . . . . ?
C10 O1 C9 C8 0.8(4) . . . . ?
C10 O1 C9 C4 -178.2(2) . . . . ?
C7 C8 C9 O1 177.9(3) . . . . ?
C7 C8 C9 C4 -3.0(4) . . . . ?
C5 C4 C9 O1 -177.8(3) . . . . ?
C3 C4 C9 O1 6.5(4) . . . . ?
C5 C4 C9 C8 3.1(4) . . . . ?
C3 C4 C9 C8 -172.7(3) . . . . ?
C9 O1 C10 C11 -168.9(2) . . . . ?
N2 C11 C10 O1 72.4(3) . . . . ?
C33 N2 C11 C10 -138.0(3) . . . . ?
C22 N2 C11 C10 89.1(3) . . . . ?
C1 N1 C12 C13 162.8(2) . . . . ?
C23 N1 C12 C13 -65.1(3) . . . . ?
N4 C13 C12 N1 -58.9(3) . . . . ?
C14 N4 C13 C12 179.4(2) . . . . ?
C13 N4 C14 C15 -173.2(2) . . . . ?
O2 C20 C15 C16 178.1(3) . . . . ?
C19 C20 C15 C16 -2.8(4) . . . . ?
O2 C20 C15 C14 -4.4(4) . . . . ?
C19 C20 C15 C14 174.7(3) . . . . ?
C17 C16 C15 C20 1.6(5) . . . . ?
C17 C16 C15 C14 -175.9(3) . . . . ?
N4 C14 C15 C20 92.9(3) . . . . ?
N4 C14 C15 C16 -89.6(3) . . . . ?
C15 C16 C17 C18 0.4(5) . . . . ?
C16 C17 C18 C19 -1.4(5) . . . . ?
C20 C19 C18 C17 0.2(5) . . . . ?
C21 O2 C20 C19 -14.9(4) . . . . ?
C21 O2 C20 C15 164.2(3) . . . . ?
C18 C19 C20 O2 -179.1(3) . . . . ?
C18 C19 C20 C15 1.9(4) . . . . ?
C20 O2 C21 C22 93.1(3) . . . . ?
N2 C22 C21 O2 45.5(3) . . . . ?
C33 N2 C22 C21 38.9(3) . . . . ?
C11 N2 C22 C21 169.8(2) . . . . ?
C12 N1 C23 C24 -67.3(4) . . . . ?
C1 N1 C23 C24 63.8(4) . . . . ?
C25 N5 C24 C23 -86.1(3) . . . . ?
N1 C23 C24 N5 -178.1(3) . . . . ?
C24 N5 C25 C26 164.3(3) . . . . ?
C27 C26 C25 N5 104.8(3) . . . . ?
C31 C26 C25 N5 -74.0(4) . . . . ?
C31 C26 C27 C28 -0.3(5) . . . . ?
C25 C26 C27 C28 -179.1(3) . . . . ?
C30 C29 C28 C27 -1.0(6) . . . . ?
C26 C27 C28 C29 1.2(5) . . . . ?
C31 C30 C29 C28 -0.1(6) . . . . ?
O3 C31 C30 C29 -177.3(3) . . . . ?
C26 C31 C30 C29 1.0(5) . . . . ?
C32 O3 C31 C30 -5.3(5) . . . . ?
C32 O3 C31 C26 176.4(3) . . . . ?
C27 C26 C31 O3 177.7(3) . . . . ?
C25 C26 C31 O3 -3.5(4) . . . . ?
C27 C26 C31 C30 -0.8(5) . . . . ?
C25 C26 C31 C30 178.1(3) . . . . ?
C31 O3 C32 C33 -172.2(3) . . . . ?
C22 N2 C33 C32 71.1(3) . . . . ?
C11 N2 C33 C32 -59.0(3) . . . . ?
O3 C32 C33 N2 -177.5(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        28.31
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.090

data_complex3
_database_code_depnum_ccdc_archive 'CCDC 727166'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H57 N9 O17'
_chemical_formula_sum            'C33 H57 N9 O17'
_chemical_formula_weight         851.88

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   'P 21/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                   16.091(4)
_cell_length_b                   25.497(6)
_cell_length_c                   19.744(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.330(5)
_cell_angle_gamma                90.00
_cell_volume                     8087(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      28.4

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3632
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9788
_exptl_absorpt_correction_T_max  0.9821
_exptl_absorpt_process_details   'SADABS 2.10 (Bruker 2003)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       /w-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            53515
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_sigmaI/netI    0.0646
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.04
_diffrn_reflns_theta_max         28.36
_reflns_number_total             20086
_reflns_number_gt                12154
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART 5.628 (Bruker, 2003)'
_computing_cell_refinement       'SAINT 6.45 ( Bruker, 2003)'
_computing_data_reduction        'SAINT 6.45 (Bruker, 2003)'
_computing_structure_solution    SIR-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond 2.1e'
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         20086
_refine_ls_number_parameters     1051
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1139
_refine_ls_R_factor_gt           0.0767
_refine_ls_wR_factor_ref         0.2333
_refine_ls_wR_factor_gt          0.1643
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.108
_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 0.3997(2) 0.34097(13) -0.2178(2) 0.0265(8) Uani 1 1 d . . .
O2 O 0.3362(2) 0.33561(14) -0.0159(2) 0.0303(9) Uani 1 1 d . . .
O3 O 0.5739(2) 0.34452(15) -0.0619(2) 0.0302(9) Uani 1 1 d . . .
O4 O 0.9181(3) 0.15820(14) 0.0410(2) 0.0309(9) Uani 1 1 d . . .
O5 O 0.8517(2) 0.17808(14) 0.2355(2) 0.0279(9) Uani 1 1 d . . .
O6 O 1.0903(3) 0.18629(16) 0.1888(2) 0.0333(9) Uani 1 1 d . . .
O7 O 0.3793(2) 0.18343(14) -0.1313(2) 0.0256(8) Uani 1 1 d . . .
O8 O 0.5116(2) 0.18995(14) -0.14612(19) 0.0247(8) Uani 1 1 d . . .
O9 O 0.4688(2) 0.18535(14) -0.04461(19) 0.0252(8) Uani 1 1 d . . .
O10 O 0.8565(2) 0.32167(14) 0.1040(2) 0.0261(8) Uani 1 1 d . . .
O11 O 0.9882(2) 0.32668(15) 0.0883(2) 0.0265(8) Uani 1 1 d . . .
O12 O 0.9450(2) 0.33806(15) 0.1891(2) 0.0272(9) Uani 1 1 d . . .
O13 O 1.0101(2) 0.39070(16) -0.1266(2) 0.0322(9) Uani 1 1 d . . .
O14 O 1.0885(2) 0.41034(15) -0.0375(2) 0.0310(9) Uani 1 1 d . . .
O15 O 1.1408(2) 0.40688(15) -0.1360(2) 0.0302(9) Uani 1 1 d . . .
O16 O 0.2967(3) -0.00975(17) -0.4556(2) 0.0425(11) Uani 1 1 d . . .
O17 O 0.2535(4) -0.0264(2) -0.3552(3) 0.0675(17) Uani 1 1 d . . .
O18 O 0.2949(3) 0.05050(17) -0.3800(3) 0.0481(13) Uani 1 1 d . . .
O19 O 0.5037(3) 0.05752(18) -0.3648(3) 0.0428(12) Uani 1 1 d . . .
O20 O 0.6329(2) 0.04846(15) -0.3884(2) 0.0356(9) Uani 1 1 d . . .
O21 O 0.5976(2) 0.10663(14) -0.3151(2) 0.0256(8) Uani 1 1 d . . .
O22 O 0.6650(3) 0.00783(19) -0.2081(2) 0.0452(12) Uani 1 1 d . . .
O23 O 0.7616(3) -0.0483(2) -0.2083(3) 0.0457(16) Uani 1 1 d . . .
O24 O 0.7185(4) -0.0208(3) -0.1128(3) 0.0507(19) Uani 1 1 d . . .
O25 O 0.9655(5) 0.0277(4) -0.1952(3) 0.052(3) Uani 1 1 d . . .
O26 O 0.9945(4) 0.0349(3) -0.0882(3) 0.051(3) Uani 1 1 d . . .
O27 O 0.8810(10) 0.0569(5) -0.1298(11) 0.039(10) Uani 1 1 d . . .
O28 O 0.3750(5) -0.0782(3) -0.1799(4) 0.093(2) Uani 1 1 d . . .
O29 O 0.4375(5) -0.0934(3) -0.0869(4) 0.046 Uani 1 1 d . . .
O30 O 0.3066(4) -0.0860(2) -0.0894(3) 0.046(2) Uani 1 1 d . . .
OW1 O 1.1753(4) 0.0758(3) -0.0732(4) 0.043(3) Uani 1 1 d . . .
OW2 O 1.1299(5) 0.0323(4) 0.0435(4) 0.041(4) Uani 1 1 d . . .
OW3 O 1.1232(10) 0.0704(7) -0.2091(8) 0.067(7) Uani 1 1 d . . .
OW4 O 1.2453(10) -0.0016(5) -0.2230(5) 0.043(10) Uani 1 1 d . . .
N1 N 0.4662(3) 0.06989(17) -0.1126(2) 0.0245(10) Uani 1 1 d . . .
H1 H 0.4648 0.1056 -0.1113 0.029 Uiso 1 1 calc R . .
N2 N 0.4266(3) 0.40548(17) -0.0982(2) 0.0280(10) Uani 1 1 d . . .
N3 N 0.3197(3) 0.12177(16) -0.0246(2) 0.0226(9) Uani 1 1 d . . .
H3D H 0.3418 0.1431 -0.0551 0.027 Uiso 1 1 calc R . .
H3C H 0.2699 0.1108 -0.0424 0.027 Uiso 1 1 calc R . .
N4 N 0.4418(3) 0.13198(16) -0.2563(2) 0.0216(9) Uani 1 1 d . . .
H4A H 0.4578 0.1517 -0.2200 0.026 Uiso 1 1 calc R . .
H4B H 0.4876 0.1244 -0.2785 0.026 Uiso 1 1 calc R . .
N5 N 0.6215(3) 0.13242(17) -0.0425(2) 0.0261(10) Uani 1 1 d . . .
H5A H 0.5728 0.1496 -0.0492 0.031 Uiso 1 1 calc R . .
H5B H 0.6253 0.1214 0.0009 0.031 Uiso 1 1 calc R . .
N6 N 0.9592(3) 0.10899(17) 0.1664(2) 0.0285(11) Uani 1 1 d . . .
N7 N 0.9102(3) 0.44217(16) 0.1010(2) 0.0222(9) Uani 1 1 d . . .
H7A H 0.9160 0.4071 0.1086 0.027 Uiso 1 1 calc R . .
N8 N 0.7779(3) 0.38698(16) 0.1975(2) 0.0237(10) Uani 1 1 d . . .
H8A H 0.7241 0.3894 0.1825 0.028 Uiso 1 1 calc R . .
H8B H 0.8040 0.3667 0.1681 0.028 Uiso 1 1 calc R . .
N9 N 0.9027(3) 0.36449(16) -0.0293(2) 0.0236(10) Uani 1 1 d . . .
H9A H 0.9452 0.3736 -0.0545 0.028 Uiso 1 1 calc R . .
H9B H 0.9244 0.3510 0.0100 0.028 Uiso 1 1 calc R . .
N10 N 1.0810(3) 0.40251(18) 0.1821(2) 0.0259(10) Uani 1 1 d . . .
H10C H 1.0360 0.3816 0.1828 0.031 Uiso 1 1 calc R . .
H10D H 1.0877 0.4183 0.2228 0.031 Uiso 1 1 calc R . .
N11 N 0.4531(3) 0.18677(16) -0.1070(2) 0.0210(9) Uani 1 1 d . . .
N12 N 0.9294(3) 0.32768(16) 0.1274(2) 0.0190(9) Uani 1 1 d . . .
N13 N 1.0815(3) 0.40263(16) -0.1002(2) 0.0239(10) Uani 1 1 d . . .
N14 N 0.2836(3) 0.00444(19) -0.3976(3) 0.0320(11) Uani 1 1 d . . .
N15 N 0.5779(3) 0.06999(17) -0.3564(2) 0.0246(10) Uani 1 1 d . . .
N16 N 0.7168(3) -0.01988(18) -0.1754(3) 0.0271(10) Uani 1 1 d . . .
N17 N 0.3791(5) -0.0878(3) -0.1145(4) 0.039 Uani 1 1 d . . .
N18 N 0.9598(10) 0.0431(4) -0.1390(5) 0.03(3) Uani 1 1 d . . .
C1 C 0.4647(3) 0.0518(2) -0.1839(3) 0.0252(11) Uani 1 1 d . . .
H1A H 0.4494 0.0150 -0.1854 0.030 Uiso 1 1 calc R . .
H1B H 0.5205 0.0547 -0.1998 0.030 Uiso 1 1 calc R . .
C2 C 0.4052(3) 0.0820(2) -0.2321(3) 0.0249(11) Uani 1 1 d . . .
H2A H 0.3899 0.0600 -0.2710 0.030 Uiso 1 1 calc R . .
H2B H 0.3549 0.0899 -0.2093 0.030 Uiso 1 1 calc R . .
C3 C 0.3840(3) 0.1631(2) -0.3017(3) 0.0268(12) Uani 1 1 d . . .
H3A H 0.3294 0.1636 -0.2833 0.032 Uiso 1 1 calc R . .
H3B H 0.3787 0.1465 -0.3459 0.032 Uiso 1 1 calc R . .
C4 C 0.4143(3) 0.2186(2) -0.3093(3) 0.0252(11) Uani 1 1 d . . .
C5 C 0.4662(3) 0.2324(2) -0.3613(3) 0.0288(12) Uani 1 1 d . . .
H5 H 0.4829 0.2070 -0.3915 0.035 Uiso 1 1 calc R . .
C6 C 0.4923(4) 0.2831(3) -0.3673(3) 0.0325(13) Uani 1 1 d . . .
H6 H 0.5245 0.2923 -0.4031 0.039 Uiso 1 1 calc R . .
C7 C 0.4712(3) 0.3220(2) -0.3201(3) 0.0271(12) Uani 1 1 d . . .
H7 H 0.4898 0.3563 -0.3240 0.032 Uiso 1 1 calc R . .
C8 C 0.4220(3) 0.3076(2) -0.2681(3) 0.0231(11) Uani 1 1 d . . .
C9 C 0.3924(3) 0.2564(2) -0.2635(3) 0.0240(11) Uani 1 1 d . . .
H9 H 0.3577 0.2476 -0.2292 0.029 Uiso 1 1 calc R . .
C10 C 0.4209(4) 0.3949(2) -0.2242(3) 0.0326(13) Uani 1 1 d . . .
H10A H 0.3970 0.4088 -0.2667 0.039 Uiso 1 1 calc R . .
H10B H 0.4809 0.3989 -0.2235 0.039 Uiso 1 1 calc R . .
C11 C 0.3868(4) 0.4234(2) -0.1656(3) 0.0344(14) Uani 1 1 d . . .
H11A H 0.3272 0.4177 -0.1659 0.041 Uiso 1 1 calc R . .
H11B H 0.3963 0.4607 -0.1707 0.041 Uiso 1 1 calc R . .
C12 C 0.3939(3) 0.04839(19) -0.0796(3) 0.0257(12) Uani 1 1 d . . .
H12A H 0.4036 0.0114 -0.0707 0.031 Uiso 1 1 calc R . .
H12B H 0.3453 0.0512 -0.1109 0.031 Uiso 1 1 calc R . .
C13 C 0.3751(3) 0.0754(2) -0.0136(3) 0.0275(12) Uani 1 1 d . . .
H13A H 0.3488 0.0505 0.0155 0.033 Uiso 1 1 calc R . .
H13B H 0.4270 0.0865 0.0095 0.033 Uiso 1 1 calc R . .
C14 C 0.3064(4) 0.1523(2) 0.0381(3) 0.0256(11) Uani 1 1 d . . .
H14A H 0.3596 0.1580 0.0627 0.031 Uiso 1 1 calc R . .
H14B H 0.2714 0.1323 0.0670 0.031 Uiso 1 1 calc R . .
C15 C 0.2662(3) 0.2043(2) 0.0221(3) 0.0262(12) Uani 1 1 d . . .
C16 C 0.1798(4) 0.2104(2) 0.0182(3) 0.0305(13) Uani 1 1 d . . .
H16 H 0.1455 0.1820 0.0263 0.037 Uiso 1 1 calc R . .
C17 C 0.1456(4) 0.2589(2) 0.0021(3) 0.0318(13) Uani 1 1 d . . .
H17 H 0.0880 0.2625 -0.0015 0.038 Uiso 1 1 calc R . .
C18 C 0.1947(3) 0.3016(2) -0.0086(3) 0.0284(12) Uani 1 1 d . . .
H18 H 0.1706 0.3341 -0.0182 0.034 Uiso 1 1 calc R . .
C19 C 0.2809(3) 0.2960(2) -0.0052(3) 0.0253(11) Uani 1 1 d . . .
C20 C 0.3163(3) 0.2480(2) 0.0103(3) 0.0240(11) Uani 1 1 d . . .
H20 H 0.3739 0.2445 0.0130 0.029 Uiso 1 1 calc R . .
C21 C 0.3028(4) 0.3863(2) -0.0324(3) 0.0322(13) Uani 1 1 d . . .
H21A H 0.2696 0.3988 0.0038 0.039 Uiso 1 1 calc R . .
H21B H 0.2676 0.3846 -0.0739 0.039 Uiso 1 1 calc R . .
C22 C 0.3736(4) 0.4218(2) -0.0410(3) 0.0323(13) Uani 1 1 d . . .
H22A H 0.4081 0.4229 0.0009 0.039 Uiso 1 1 calc R . .
H22B H 0.3527 0.4570 -0.0499 0.039 Uiso 1 1 calc R . .
C23 C 0.5435(3) 0.0507(2) -0.0774(3) 0.0281(12) Uani 1 1 d . . .
H23A H 0.5549 0.0156 -0.0935 0.034 Uiso 1 1 calc R . .
H23B H 0.5352 0.0484 -0.0292 0.034 Uiso 1 1 calc R . .
C24 C 0.6206(3) 0.0858(2) -0.0879(3) 0.0277(12) Uani 1 1 d . . .
H24A H 0.6710 0.0656 -0.0785 0.033 Uiso 1 1 calc R . .
H24B H 0.6197 0.0973 -0.1347 0.033 Uiso 1 1 calc R . .
C25 C 0.6900(3) 0.1693(2) -0.0529(3) 0.0269(12) Uani 1 1 d . . .
H25A H 0.6945 0.1751 -0.1011 0.032 Uiso 1 1 calc R . .
H25B H 0.7420 0.1543 -0.0347 0.032 Uiso 1 1 calc R . .
C26 C 0.6746(3) 0.2208(2) -0.0183(3) 0.0238(11) Uani 1 1 d . . .
C27 C 0.6976(3) 0.2280(2) 0.0505(3) 0.0251(11) Uani 1 1 d . . .
H27 H 0.7238 0.2010 0.0753 0.030 Uiso 1 1 calc R . .
C28 C 0.6813(3) 0.2751(2) 0.0815(3) 0.0250(11) Uani 1 1 d . . .
H28 H 0.6969 0.2797 0.1273 0.030 Uiso 1 1 calc R . .
C29 C 0.6422(3) 0.3155(2) 0.0457(3) 0.0253(12) Uani 1 1 d . . .
H29 H 0.6323 0.3473 0.0669 0.030 Uiso 1 1 calc R . .
C30 C 0.6178(3) 0.3084(2) -0.0221(3) 0.0220(11) Uani 1 1 d . . .
C31 C 0.6344(3) 0.2613(2) -0.0541(3) 0.0254(11) Uani 1 1 d . . .
H31 H 0.6186 0.2568 -0.0998 0.030 Uiso 1 1 calc R . .
C32 C 0.5643(4) 0.3955(2) -0.0337(3) 0.0302(13) Uani 1 1 d . . .
H32A H 0.6181 0.4116 -0.0234 0.036 Uiso 1 1 calc R . .
H32B H 0.5347 0.3935 0.0077 0.036 Uiso 1 1 calc R . .
C33 C 0.5150(4) 0.4262(2) -0.0872(3) 0.0316(13) Uani 1 1 d . . .
H33A H 0.5426 0.4243 -0.1295 0.038 Uiso 1 1 calc R . .
H33B H 0.5132 0.4628 -0.0736 0.038 Uiso 1 1 calc R . .
C34 C 0.9211(5) 0.0805(2) 0.1035(3) 0.0366(15) Uani 1 1 d . . .
H34A H 0.9382 0.0440 0.1049 0.044 Uiso 1 1 calc R . .
H34B H 0.8608 0.0815 0.1040 0.044 Uiso 1 1 calc R . .
C35 C 0.9478(5) 0.1053(2) 0.0392(3) 0.0357(14) Uani 1 1 d . . .
H35A H 1.0080 0.1046 0.0377 0.043 Uiso 1 1 calc R . .
H35B H 0.9236 0.0870 -0.0002 0.043 Uiso 1 1 calc R . .
C36 C 0.9295(3) 0.1893(2) -0.0145(3) 0.0237(11) Uani 1 1 d . . .
C37 C 0.9752(3) 0.1748(2) -0.0694(3) 0.0253(11) Uani 1 1 d . . .
H37 H 1.0007 0.1421 -0.0704 0.030 Uiso 1 1 calc R . .
C38 C 0.9820(3) 0.2094(2) -0.1218(3) 0.0271(12) Uani 1 1 d . . .
H38 H 1.0126 0.1998 -0.1584 0.032 Uiso 1 1 calc R . .
C39 C 0.9443(3) 0.2585(2) -0.1216(3) 0.0247(11) Uani 1 1 d . . .
H39 H 0.9509 0.2819 -0.1570 0.030 Uiso 1 1 calc R . .
C40 C 0.8969(3) 0.2720(2) -0.0680(3) 0.0223(11) Uani 1 1 d . . .
C41 C 0.8914(3) 0.2372(2) -0.0142(3) 0.0233(11) Uani 1 1 d . . .
H41 H 0.8612 0.2467 0.0227 0.028 Uiso 1 1 calc R . .
C42 C 0.8519(3) 0.3236(2) -0.0659(3) 0.0267(12) Uani 1 1 d . . .
H42A H 0.8381 0.3353 -0.1119 0.032 Uiso 1 1 calc R . .
H42B H 0.8003 0.3188 -0.0436 0.032 Uiso 1 1 calc R . .
C43 C 0.8539(3) 0.4123(2) -0.0143(3) 0.0236(11) Uani 1 1 d . . .
H43A H 0.8061 0.4024 0.0105 0.028 Uiso 1 1 calc R . .
H43B H 0.8337 0.4284 -0.0566 0.028 Uiso 1 1 calc R . .
C44 C 0.9068(3) 0.4523(2) 0.0276(3) 0.0251(12) Uani 1 1 d . . .
H44A H 0.9630 0.4520 0.0123 0.030 Uiso 1 1 calc R . .
H44B H 0.8840 0.4871 0.0192 0.030 Uiso 1 1 calc R . .
C45 C 0.9118(4) 0.0949(2) 0.2273(3) 0.0301(13) Uani 1 1 d . . .
H45A H 0.9009 0.0575 0.2268 0.036 Uiso 1 1 calc R . .
H45B H 0.9460 0.1027 0.2682 0.036 Uiso 1 1 calc R . .
C46 C 0.8317(4) 0.1235(2) 0.2295(3) 0.0301(12) Uani 1 1 d . . .
H46A H 0.7973 0.1171 0.1884 0.036 Uiso 1 1 calc R . .
H46B H 0.8016 0.1120 0.2680 0.036 Uiso 1 1 calc R . .
C47 C 0.7882(3) 0.2134(2) 0.2449(3) 0.0232(11) Uani 1 1 d . . .
C48 C 0.7054(4) 0.1991(2) 0.2500(3) 0.0270(12) Uani 1 1 d . . .
H48 H 0.6887 0.1642 0.2461 0.032 Uiso 1 1 calc R . .
C49 C 0.6478(3) 0.2392(2) 0.2613(3) 0.0265(12) Uani 1 1 d . . .
H49 H 0.5923 0.2304 0.2654 0.032 Uiso 1 1 calc R . .
C50 C 0.6708(3) 0.2904(2) 0.2662(3) 0.0242(11) Uani 1 1 d . . .
H50 H 0.6312 0.3161 0.2734 0.029 Uiso 1 1 calc R . .
C51 C 0.7551(3) 0.3046(2) 0.2605(3) 0.0221(11) Uani 1 1 d . . .
C52 C 0.8133(3) 0.2654(2) 0.2494(3) 0.0229(11) Uani 1 1 d . . .
H52 H 0.8689 0.2741 0.2449 0.027 Uiso 1 1 calc R . .
C53 C 0.7826(3) 0.3611(2) 0.2655(3) 0.0255(11) Uani 1 1 d . . .
H53A H 0.7474 0.3798 0.2956 0.031 Uiso 1 1 calc R . .
H53B H 0.8393 0.3627 0.2848 0.031 Uiso 1 1 calc R . .
C54 C 0.8159(4) 0.4405(2) 0.1980(3) 0.0285(12) Uani 1 1 d . . .
H54A H 0.8678 0.4397 0.2255 0.034 Uiso 1 1 calc R . .
H54B H 0.7788 0.4648 0.2191 0.034 Uiso 1 1 calc R . .
C55 C 0.8329(3) 0.4606(2) 0.1283(3) 0.0277(12) Uani 1 1 d . . .
H55A H 0.7868 0.4504 0.0972 0.033 Uiso 1 1 calc R . .
H55B H 0.8341 0.4986 0.1299 0.033 Uiso 1 1 calc R . .
C56 C 1.0508(4) 0.0976(2) 0.1784(3) 0.0368(15) Uani 1 1 d . . .
H56A H 1.0578 0.0632 0.1990 0.044 Uiso 1 1 calc R . .
H56B H 1.0765 0.0970 0.1352 0.044 Uiso 1 1 calc R . .
C57 C 1.0936(4) 0.1374(2) 0.2232(3) 0.0330(13) Uani 1 1 d . . .
H57A H 1.0663 0.1401 0.2656 0.040 Uiso 1 1 calc R . .
H57B H 1.1511 0.1272 0.2334 0.040 Uiso 1 1 calc R . .
C58 C 1.1244(3) 0.2284(2) 0.2230(3) 0.0317(13) Uani 1 1 d . . .
C59 C 1.1570(3) 0.2283(2) 0.2899(3) 0.0314(13) Uani 1 1 d . . .
H59 H 1.1583 0.1975 0.3152 0.038 Uiso 1 1 calc R . .
C60 C 1.1870(3) 0.2739(2) 0.3180(3) 0.0327(13) Uani 1 1 d . . .
H60 H 1.2082 0.2739 0.3628 0.039 Uiso 1 1 calc R . .
C61 C 1.1867(3) 0.3201(3) 0.2811(3) 0.0364(14) Uani 1 1 d . . .
H61 H 1.2069 0.3508 0.3013 0.044 Uiso 1 1 calc R . .
C62 C 1.1566(3) 0.3205(2) 0.2146(3) 0.0323(14) Uani 1 1 d . . .
C63 C 1.1268(4) 0.2745(2) 0.1846(3) 0.0320(13) Uani 1 1 d . . .
H63 H 1.1084 0.2743 0.1391 0.038 Uiso 1 1 calc R . .
C64 C 1.1562(3) 0.3694(3) 0.1711(4) 0.0375(15) Uani 1 1 d . . .
H64A H 1.2062 0.3896 0.1823 0.045 Uiso 1 1 calc R . .
H64B H 1.1563 0.3595 0.1237 0.045 Uiso 1 1 calc R . .
C65 C 1.0653(3) 0.4437(2) 0.1285(3) 0.0246(11) Uani 1 1 d . . .
H65A H 1.0672 0.4276 0.0841 0.030 Uiso 1 1 calc R . .
H65B H 1.1093 0.4697 0.1327 0.030 Uiso 1 1 calc R . .
C66 C 0.9824(3) 0.4704(2) 0.1337(3) 0.0250(11) Uani 1 1 d . . .
H66A H 0.9726 0.4752 0.1814 0.030 Uiso 1 1 calc R . .
H66B H 0.9854 0.5050 0.1134 0.030 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 C8 1.372(6) . ?
O1 C10 1.423(6) . ?
O2 C19 1.371(6) . ?
O2 C21 1.431(6) . ?
O3 C30 1.379(6) . ?
O3 C32 1.426(6) . ?
O4 C36 1.374(6) . ?
O4 C35 1.432(6) . ?
O5 C47 1.382(6) . ?
O5 C46 1.432(6) . ?
O6 C58 1.366(7) . ?
O6 C57 1.420(7) . ?
O7 N11 1.258(5) . ?
O8 N11 1.254(5) . ?
O9 N11 1.244(6) . ?
O10 N12 1.245(5) . ?
O11 N12 1.256(5) . ?
O12 N12 1.258(6) . ?
O13 N13 1.271(6) . ?
O14 N13 1.251(6) . ?
O15 N13 1.226(6) . ?
O16 N14 1.232(6) . ?
O18 N14 1.235(6) . ?
O19 N15 1.237(6) . ?
O20 N15 1.245(5) . ?
O21 N15 1.268(6) . ?
O22 N16 1.244(6) . ?
O25 N18 1.187(10) . ?
O26 N18 1.138(9) . ?
O28 N17 1.313(9) . ?
O29 N17 1.068(8) . ?
O30 N17 1.295(8) . ?
N1 C12 1.471(7) . ?
N1 C23 1.473(7) . ?
N1 C1 1.481(7) . ?
N1 H1 0.9100 . ?
N2 C22 1.511(8) . ?
N2 C11 1.513(8) . ?
N2 C33 1.522(7) . ?
N3 C14 1.487(7) . ?
N3 C13 1.491(7) . ?
N3 H3D 0.9000 . ?
N3 H3C 0.9000 . ?
N4 C3 1.484(7) . ?
N4 C2 1.494(7) . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
N5 C25 1.472(7) . ?
N5 C24 1.487(7) . ?
N5 H5A 0.9000 . ?
N5 H5B 0.9000 . ?
N6 C45 1.504(7) . ?
N6 C56 1.507(8) . ?
N6 C34 1.536(7) . ?
N7 C55 1.463(6) . ?
N7 C44 1.469(7) . ?
N7 C66 1.483(7) . ?
N7 H7A 0.9100 . ?
N8 C53 1.495(7) . ?
N8 C54 1.496(6) . ?
N8 H8A 0.9000 . ?
N8 H8B 0.9000 . ?
N9 C42 1.487(7) . ?
N9 C43 1.489(6) . ?
N9 H9A 0.9000 . ?
N9 H9B 0.9000 . ?
N10 C65 1.500(7) . ?
N10 C64 1.501(7) . ?
N10 H10C 0.9000 . ?
N10 H10D 0.9000 . ?
N14 O17 1.266(7) . ?
N16 O23 1.235(6) . ?
N16 O24 1.236(7) . ?
N18 O27 1.338(16) . ?
C1 C2 1.520(8) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C9 1.381(7) . ?
C4 C5 1.404(8) . ?
C4 C3 1.509(8) . ?
C5 C6 1.368(9) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C6 1.414(8) . ?
C7 H7 0.9300 . ?
C8 C7 1.382(8) . ?
C8 C9 1.395(7) . ?
C9 H9 0.9300 . ?
C10 C11 1.498(9) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.520(8) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.396(8) . ?
C15 C14 1.503(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.369(8) . ?
C17 C16 1.382(8) . ?
C17 H17 0.9300 . ?
C18 H18 0.9300 . ?
C19 C18 1.393(8) . ?
C20 C19 1.376(7) . ?
C20 C15 1.402(8) . ?
C20 H20 0.9300 . ?
C21 C22 1.474(8) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C23 1.553(8) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C31 1.388(8) . ?
C26 C27 1.399(8) . ?
C26 C25 1.509(7) . ?
C27 C28 1.381(8) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C29 C28 1.381(8) . ?
C29 C30 1.385(8) . ?
C29 H29 0.9300 . ?
C31 C30 1.391(7) . ?
C31 H31 0.9300 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C32 1.504(8) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.504(8) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 C37 1.395(8) . ?
C37 C38 1.367(8) . ?
C37 H37 0.9300 . ?
C38 C39 1.392(7) . ?
C38 H38 0.9300 . ?
C39 H39 0.9300 . ?
C40 C39 1.384(8) . ?
C40 C42 1.502(7) . ?
C41 C36 1.367(7) . ?
C41 C40 1.391(8) . ?
C41 H41 0.9300 . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 C44 1.539(7) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 C45 1.484(8) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C47 C48 1.391(8) . ?
C48 C49 1.406(8) . ?
C48 H48 0.9300 . ?
C49 H49 0.9300 . ?
C50 C49 1.360(8) . ?
C50 C51 1.414(7) . ?
C50 H50 0.9300 . ?
C52 C47 1.386(7) . ?
C52 C51 1.397(7) . ?
C52 H52 0.9300 . ?
C53 C51 1.508(7) . ?
C53 H53A 0.9700 . ?
C53 H53B 0.9700 . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C55 C54 1.507(8) . ?
C55 H55A 0.9700 . ?
C55 H55B 0.9700 . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C57 C56 1.487(9) . ?
C57 H57A 0.9700 . ?
C57 H57B 0.9700 . ?
C58 C59 1.393(9) . ?
C59 H59 0.9300 . ?
C60 C59 1.364(9) . ?
C60 C61 1.385(8) . ?
C60 H60 0.9300 . ?
C61 H61 0.9300 . ?
C62 C61 1.373(9) . ?
C62 C64 1.514(8) . ?
C63 C62 1.386(9) . ?
C63 C58 1.402(8) . ?
C63 H63 0.9300 . ?
C64 H64A 0.9700 . ?
C64 H64B 0.9700 . ?
C65 H65A 0.9700 . ?
C65 H65B 0.9700 . ?
C66 C65 1.507(7) . ?
C66 H66A 0.9700 . ?
C66 H66B 0.9700 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C8 O1 C10 117.4(4) . . ?
C19 O2 C21 117.5(4) . . ?
C30 O3 C32 116.7(4) . . ?
C36 O4 C35 117.6(4) . . ?
C47 O5 C46 118.7(4) . . ?
C58 O6 C57 116.8(5) . . ?
C12 N1 C23 109.7(4) . . ?
C12 N1 C1 109.6(4) . . ?
C23 N1 C1 108.1(4) . . ?
C12 N1 H1 109.8 . . ?
C23 N1 H1 109.8 . . ?
C1 N1 H1 109.8 . . ?
C22 N2 C11 110.2(4) . . ?
C22 N2 C33 111.1(5) . . ?
C11 N2 C33 111.4(5) . . ?
C14 N3 C13 114.1(4) . . ?
C14 N3 H3D 108.7 . . ?
C13 N3 H3D 108.7 . . ?
C14 N3 H3C 108.7 . . ?
C13 N3 H3C 108.7 . . ?
H3D N3 H3C 107.6 . . ?
C3 N4 C2 113.8(4) . . ?
C3 N4 H4A 108.8 . . ?
C2 N4 H4A 108.8 . . ?
C3 N4 H4B 108.8 . . ?
C2 N4 H4B 108.8 . . ?
H4A N4 H4B 107.7 . . ?
C25 N5 C24 113.9(4) . . ?
C25 N5 H5A 108.8 . . ?
C24 N5 H5A 108.8 . . ?
C25 N5 H5B 108.8 . . ?
C24 N5 H5B 108.8 . . ?
H5A N5 H5B 107.7 . . ?
C45 N6 C56 111.4(5) . . ?
C45 N6 C34 109.6(5) . . ?
C56 N6 C34 112.2(5) . . ?
C55 N7 C44 108.9(4) . . ?
C55 N7 C66 110.1(4) . . ?
C44 N7 C66 109.2(4) . . ?
C55 N7 H7A 109.6 . . ?
C44 N7 H7A 109.6 . . ?
C66 N7 H7A 109.5 . . ?
C53 N8 C54 113.4(4) . . ?
C53 N8 H8A 108.9 . . ?
C54 N8 H8A 108.9 . . ?
C53 N8 H8B 108.9 . . ?
C54 N8 H8B 108.9 . . ?
H8A N8 H8B 107.7 . . ?
C42 N9 C43 113.0(4) . . ?
C42 N9 H9A 109.0 . . ?
C43 N9 H9A 109.0 . . ?
C42 N9 H9B 109.0 . . ?
C43 N9 H9B 109.0 . . ?
H9A N9 H9B 107.8 . . ?
C65 N10 C64 113.3(4) . . ?
C65 N10 H10C 108.9 . . ?
C64 N10 H10C 108.9 . . ?
C65 N10 H10D 108.9 . . ?
C64 N10 H10D 108.9 . . ?
H10C N10 H10D 107.7 . . ?
O9 N11 O8 119.7(4) . . ?
O9 N11 O7 120.5(4) . . ?
O8 N11 O7 119.8(4) . . ?
O10 N12 O11 119.7(4) . . ?
O10 N12 O12 121.1(4) . . ?
O11 N12 O12 119.1(4) . . ?
O15 N13 O14 121.9(4) . . ?
O15 N13 O13 119.9(5) . . ?
O14 N13 O13 118.2(4) . . ?
O16 N14 O18 120.7(5) . . ?
O16 N14 O17 121.7(5) . . ?
O18 N14 O17 117.5(6) . . ?
O19 N15 O20 121.9(5) . . ?
O19 N15 O21 118.6(4) . . ?
O20 N15 O21 119.5(4) . . ?
O23 N16 O24 122.3(5) . . ?
O23 N16 O22 117.0(5) . . ?
O24 N16 O22 120.5(5) . . ?
O29 N17 O30 126.6(9) . . ?
O29 N17 O28 121.3(9) . . ?
O30 N17 O28 111.9(7) . . ?
O26 N18 O25 134.7(11) . . ?
O26 N18 O27 110.4(16) . . ?
O25 N18 O27 109.8(13) . . ?
N1 C1 C2 114.4(4) . . ?
N1 C1 H1A 108.7 . . ?
C2 C1 H1A 108.7 . . ?
N1 C1 H1B 108.7 . . ?
C2 C1 H1B 108.7 . . ?
H1A C1 H1B 107.6 . . ?
N4 C2 C1 112.7(4) . . ?
N4 C2 H2A 109.1 . . ?
C1 C2 H2A 109.1 . . ?
N4 C2 H2B 109.1 . . ?
C1 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
N4 C3 C4 111.5(4) . . ?
N4 C3 H3A 109.3 . . ?
C4 C3 H3A 109.3 . . ?
N4 C3 H3B 109.3 . . ?
C4 C3 H3B 109.3 . . ?
H3A C3 H3B 108.0 . . ?
C9 C4 C5 119.4(5) . . ?
C9 C4 C3 119.5(5) . . ?
C5 C4 C3 121.1(5) . . ?
C6 C5 C4 119.9(5) . . ?
C6 C5 H5 120.1 . . ?
C4 C5 H5 120.1 . . ?
C5 C6 C7 121.2(5) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 H6 119.4 . . ?
C8 C7 C6 118.2(5) . . ?
C8 C7 H7 120.9 . . ?
C6 C7 H7 120.9 . . ?
O1 C8 C7 124.0(5) . . ?
O1 C8 C9 115.4(5) . . ?
C7 C8 C9 120.7(5) . . ?
C4 C9 C8 120.5(5) . . ?
C4 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
O1 C10 C11 107.4(5) . . ?
O1 C10 H10A 110.2 . . ?
C11 C10 H10A 110.2 . . ?
O1 C10 H10B 110.2 . . ?
C11 C10 H10B 110.2 . . ?
H10A C10 H10B 108.5 . . ?
C10 C11 N2 112.3(5) . . ?
C10 C11 H11A 109.1 . . ?
N2 C11 H11A 109.2 . . ?
C10 C11 H11B 109.1 . . ?
N2 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
N1 C12 C13 114.3(4) . . ?
N1 C12 H12A 108.7 . . ?
C13 C12 H12A 108.7 . . ?
N1 C12 H12B 108.7 . . ?
C13 C12 H12B 108.7 . . ?
H12A C12 H12B 107.6 . . ?
N3 C13 C12 112.4(5) . . ?
N3 C13 H13A 109.1 . . ?
C12 C13 H13A 109.1 . . ?
N3 C13 H13B 109.1 . . ?
C12 C13 H13B 109.1 . . ?
H13A C13 H13B 107.9 . . ?
N3 C14 C15 111.6(4) . . ?
N3 C14 H14A 109.3 . . ?
C15 C14 H14A 109.3 . . ?
N3 C14 H14B 109.3 . . ?
C15 C14 H14B 109.3 . . ?
H14A C14 H14B 108.0 . . ?
C16 C15 C20 118.9(5) . . ?
C16 C15 C14 121.6(5) . . ?
C20 C15 C14 119.4(5) . . ?
C17 C16 C15 119.5(5) . . ?
C17 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C18 C17 C16 121.4(5) . . ?
C18 C17 H17 119.3 . . ?
C16 C17 H17 119.3 . . ?
C17 C18 C19 119.5(5) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
O2 C19 C20 115.2(5) . . ?
O2 C19 C18 124.8(5) . . ?
C20 C19 C18 120.0(5) . . ?
C19 C20 C15 120.6(5) . . ?
C19 C20 H20 119.7 . . ?
C15 C20 H20 119.7 . . ?
O2 C21 C22 107.3(5) . . ?
O2 C21 H21A 110.2 . . ?
C22 C21 H21A 110.3 . . ?
O2 C21 H21B 110.2 . . ?
C22 C21 H21B 110.2 . . ?
H21A C21 H21B 108.5 . . ?
C21 C22 N2 113.0(5) . . ?
C21 C22 H22A 109.0 . . ?
N2 C22 H22A 109.0 . . ?
C21 C22 H22B 109.0 . . ?
N2 C22 H22B 109.0 . . ?
H22A C22 H22B 107.8 . . ?
N1 C23 C24 113.9(4) . . ?
N1 C23 H23A 108.8 . . ?
C24 C23 H23A 108.8 . . ?
N1 C23 H23B 108.8 . . ?
C24 C23 H23B 108.8 . . ?
H23A C23 H23B 107.7 . . ?
N5 C24 C23 111.1(4) . . ?
N5 C24 H24A 109.4 . . ?
C23 C24 H24A 109.4 . . ?
N5 C24 H24B 109.4 . . ?
C23 C24 H24B 109.4 . . ?
H24A C24 H24B 108.0 . . ?
N5 C25 C26 110.4(4) . . ?
N5 C25 H25A 109.6 . . ?
C26 C25 H25A 109.6 . . ?
N5 C25 H25B 109.6 . . ?
C26 C25 H25B 109.6 . . ?
H25A C25 H25B 108.1 . . ?
C31 C26 C27 119.1(5) . . ?
C31 C26 C25 120.0(5) . . ?
C27 C26 C25 120.8(5) . . ?
C28 C27 C26 119.9(5) . . ?
C28 C27 H27 120.1 . . ?
C26 C27 H27 120.1 . . ?
C29 C28 C27 121.0(5) . . ?
C29 C28 H28 119.5 . . ?
C27 C28 H28 119.5 . . ?
C28 C29 C30 119.5(5) . . ?
C28 C29 H29 120.2 . . ?
C30 C29 H29 120.2 . . ?
O3 C30 C29 124.8(5) . . ?
O3 C30 C31 115.0(5) . . ?
C29 C30 C31 120.1(5) . . ?
C26 C31 C30 120.4(5) . . ?
C26 C31 H31 119.8 . . ?
C30 C31 H31 119.8 . . ?
O3 C32 C33 105.4(5) . . ?
O3 C32 H32A 110.7 . . ?
C33 C32 H32A 110.7 . . ?
O3 C32 H32B 110.7 . . ?
C33 C32 H32B 110.6 . . ?
H32A C32 H32B 108.8 . . ?
C32 C33 N2 111.7(5) . . ?
C32 C33 H33A 109.3 . . ?
N2 C33 H33A 109.3 . . ?
C32 C33 H33B 109.3 . . ?
N2 C33 H33B 109.3 . . ?
H33A C33 H33B 107.9 . . ?
C35 C34 N6 111.3(5) . . ?
C35 C34 H34A 109.4 . . ?
N6 C34 H34A 109.4 . . ?
C35 C34 H34B 109.4 . . ?
N6 C34 H34B 109.4 . . ?
H34A C34 H34B 108.0 . . ?
O4 C35 C34 105.3(5) . . ?
O4 C35 H35A 110.7 . . ?
C34 C35 H35A 110.7 . . ?
O4 C35 H35B 110.7 . . ?
C34 C35 H35B 110.7 . . ?
H35A C35 H35B 108.8 . . ?
C41 C36 O4 115.6(5) . . ?
C41 C36 C37 119.8(5) . . ?
O4 C36 C37 124.6(5) . . ?
C38 C37 C36 119.1(5) . . ?
C38 C37 H37 120.5 . . ?
C36 C37 H37 120.4 . . ?
C37 C38 C39 121.6(5) . . ?
C37 C38 H38 119.2 . . ?
C39 C38 H38 119.2 . . ?
C40 C39 C38 119.0(5) . . ?
C40 C39 H39 120.5 . . ?
C38 C39 H39 120.5 . . ?
C39 C40 C41 119.2(5) . . ?
C39 C40 C42 121.8(5) . . ?
C41 C40 C42 119.0(5) . . ?
C36 C41 C40 121.2(5) . . ?
C36 C41 H41 119.4 . . ?
C40 C41 H41 119.4 . . ?
N9 C42 C40 112.1(4) . . ?
N9 C42 H42A 109.2 . . ?
C40 C42 H42A 109.2 . . ?
N9 C42 H42B 109.2 . . ?
C40 C42 H42B 109.2 . . ?
H42A C42 H42B 107.9 . . ?
N9 C43 C44 111.6(4) . . ?
N9 C43 H43A 109.3 . . ?
C44 C43 H43A 109.3 . . ?
N9 C43 H43B 109.3 . . ?
C44 C43 H43B 109.3 . . ?
H43A C43 H43B 108.0 . . ?
N7 C44 C43 113.7(4) . . ?
N7 C44 H44A 108.8 . . ?
C43 C44 H44A 108.8 . . ?
N7 C44 H44B 108.8 . . ?
C43 C44 H44B 108.8 . . ?
H44A C44 H44B 107.7 . . ?
C46 C45 N6 112.8(5) . . ?
C46 C45 H45A 109.0 . . ?
N6 C45 H45A 109.0 . . ?
C46 C45 H45B 109.0 . . ?
N6 C45 H45B 109.1 . . ?
H45A C45 H45B 107.8 . . ?
O5 C46 C45 106.8(5) . . ?
O5 C46 H46A 110.4 . . ?
C45 C46 H46A 110.4 . . ?
O5 C46 H46B 110.4 . . ?
C45 C46 H46B 110.4 . . ?
H46A C46 H46B 108.6 . . ?
O5 C47 C52 114.6(5) . . ?
O5 C47 C48 123.8(5) . . ?
C52 C47 C48 121.5(5) . . ?
C47 C48 C49 117.6(5) . . ?
C47 C48 H48 121.2 . . ?
C49 C48 H48 121.2 . . ?
C50 C49 C48 122.1(5) . . ?
C50 C49 H49 118.9 . . ?
C48 C49 H49 118.9 . . ?
C49 C50 C51 119.8(5) . . ?
C49 C50 H50 120.1 . . ?
C51 C50 H50 120.1 . . ?
C52 C51 C50 119.0(5) . . ?
C52 C51 C53 119.8(5) . . ?
C50 C51 C53 121.2(5) . . ?
C47 C52 C51 119.9(5) . . ?
C47 C52 H52 120.0 . . ?
C51 C52 H52 120.0 . . ?
N8 C53 C51 111.3(4) . . ?
N8 C53 H53A 109.4 . . ?
C51 C53 H53A 109.4 . . ?
N8 C53 H53B 109.4 . . ?
C51 C53 H53B 109.4 . . ?
H53A C53 H53B 108.0 . . ?
N8 C54 C55 113.5(5) . . ?
N8 C54 H54A 108.9 . . ?
C55 C54 H54A 108.9 . . ?
N8 C54 H54B 108.9 . . ?
C55 C54 H54B 108.9 . . ?
H54A C54 H54B 107.7 . . ?
N7 C55 C54 115.6(5) . . ?
N7 C55 H55A 108.4 . . ?
C54 C55 H55A 108.4 . . ?
N7 C55 H55B 108.4 . . ?
C54 C55 H55B 108.4 . . ?
H55A C55 H55B 107.4 . . ?
C57 C56 N6 112.2(5) . . ?
C57 C56 H56A 109.2 . . ?
N6 C56 H56A 109.1 . . ?
C57 C56 H56B 109.2 . . ?
N6 C56 H56B 109.2 . . ?
H56A C56 H56B 107.9 . . ?
O6 C57 C56 108.1(5) . . ?
O6 C57 H57A 110.1 . . ?
C56 C57 H57A 110.1 . . ?
O6 C57 H57B 110.1 . . ?
C56 C57 H57B 110.1 . . ?
H57A C57 H57B 108.4 . . ?
O6 C58 C59 125.9(5) . . ?
O6 C58 C63 114.5(5) . . ?
C59 C58 C63 119.6(6) . . ?
C60 C59 C58 119.2(6) . . ?
C60 C59 H59 120.4 . . ?
C58 C59 H59 120.4 . . ?
C59 C60 C61 121.4(6) . . ?
C59 C60 H60 119.3 . . ?
C61 C60 H60 119.3 . . ?
C62 C61 C60 120.0(6) . . ?
C62 C61 H61 120.0 . . ?
C60 C61 H61 120.0 . . ?
C61 C62 C63 119.8(6) . . ?
C61 C62 C64 122.6(6) . . ?
C63 C62 C64 117.6(6) . . ?
C62 C63 C58 119.9(6) . . ?
C62 C63 H63 120.1 . . ?
C58 C63 H63 120.1 . . ?
N10 C64 C62 111.0(5) . . ?
N10 C64 H64A 109.4 . . ?
C62 C64 H64A 109.4 . . ?
N10 C64 H64B 109.4 . . ?
C62 C64 H64B 109.4 . . ?
H64A C64 H64B 108.0 . . ?
N10 C65 C66 112.4(4) . . ?
N10 C65 H65A 109.1 . . ?
C66 C65 H65A 109.1 . . ?
N10 C65 H65B 109.1 . . ?
C66 C65 H65B 109.1 . . ?
H65A C65 H65B 107.8 . . ?
N7 C66 C65 115.1(4) . . ?
N7 C66 H66A 108.5 . . ?
C65 C66 H66A 108.5 . . ?
N7 C66 H66B 108.5 . . ?
C65 C66 H66B 108.5 . . ?
H66A C66 H66B 107.5 . . ?

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
C12 N1 C1 C2 79.3(5) . . . . ?
C23 N1 C1 C2 -161.2(4) . . . . ?
C3 N4 C2 C1 -178.1(4) . . . . ?
N1 C1 C2 N4 82.7(6) . . . . ?
C2 N4 C3 C4 164.7(4) . . . . ?
C9 C4 C3 N4 -87.9(6) . . . . ?
C5 C4 C3 N4 90.4(6) . . . . ?
C9 C4 C5 C6 -2.2(8) . . . . ?
C3 C4 C5 C6 179.6(5) . . . . ?
C4 C5 C6 C7 3.0(8) . . . . ?
C8 C7 C6 C5 -1.1(8) . . . . ?
O1 C8 C7 C6 177.5(5) . . . . ?
C9 C8 C7 C6 -1.6(8) . . . . ?
C10 O1 C8 C7 7.3(8) . . . . ?
C10 O1 C8 C9 -173.5(5) . . . . ?
C5 C4 C9 C8 -0.5(8) . . . . ?
C3 C4 C9 C8 177.8(5) . . . . ?
O1 C8 C9 C4 -176.8(5) . . . . ?
C7 C8 C9 C4 2.5(8) . . . . ?
C8 O1 C10 C11 177.4(5) . . . . ?
O1 C10 C11 N2 63.7(6) . . . . ?
C22 N2 C11 C10 -162.3(5) . . . . ?
C33 N2 C11 C10 73.8(6) . . . . ?
C23 N1 C12 C13 77.3(6) . . . . ?
C1 N1 C12 C13 -164.2(4) . . . . ?
C14 N3 C13 C12 -174.4(4) . . . . ?
N1 C12 C13 N3 87.6(6) . . . . ?
C13 N3 C14 C15 167.6(4) . . . . ?
C16 C15 C14 N3 90.6(6) . . . . ?
C20 C15 C14 N3 -88.9(6) . . . . ?
C19 C20 C15 C16 -0.2(8) . . . . ?
C19 C20 C15 C14 179.3(5) . . . . ?
C18 C17 C16 C15 -1.5(9) . . . . ?
C20 C15 C16 C17 0.7(9) . . . . ?
C14 C15 C16 C17 -178.8(5) . . . . ?
C16 C17 C18 C19 1.8(9) . . . . ?
O2 C19 C18 C17 179.1(5) . . . . ?
C20 C19 C18 C17 -1.4(9) . . . . ?
C21 O2 C19 C20 179.8(5) . . . . ?
C21 O2 C19 C18 -0.6(8) . . . . ?
C15 C20 C19 O2 -179.8(5) . . . . ?
C15 C20 C19 C18 0.6(8) . . . . ?
C19 O2 C21 C22 179.8(5) . . . . ?
O2 C21 C22 N2 61.7(6) . . . . ?
C11 N2 C22 C21 80.8(6) . . . . ?
C33 N2 C22 C21 -155.2(5) . . . . ?
C12 N1 C23 C24 -157.5(4) . . . . ?
C1 N1 C23 C24 83.1(5) . . . . ?
N5 C24 C23 N1 79.9(6) . . . . ?
C25 N5 C24 C23 -176.2(4) . . . . ?
C24 N5 C25 C26 166.0(5) . . . . ?
C31 C26 C25 N5 -92.9(6) . . . . ?
C27 C26 C25 N5 84.7(6) . . . . ?
C31 C26 C27 C28 -1.0(8) . . . . ?
C25 C26 C27 C28 -178.6(5) . . . . ?
C30 C29 C28 C27 1.0(8) . . . . ?
C26 C27 C28 C29 0.3(8) . . . . ?
C32 O3 C30 C29 9.7(7) . . . . ?
C32 O3 C30 C31 -172.7(5) . . . . ?
C28 C29 C30 O3 175.9(5) . . . . ?
C28 C29 C30 C31 -1.6(8) . . . . ?
C26 C31 C30 O3 -176.9(5) . . . . ?
C26 C31 C30 C29 0.9(8) . . . . ?
C27 C26 C31 C30 0.4(8) . . . . ?
C25 C26 C31 C30 178.0(5) . . . . ?
C30 O3 C32 C33 179.9(4) . . . . ?
N2 C33 C32 O3 67.1(6) . . . . ?
C22 N2 C33 C32 75.5(6) . . . . ?
C11 N2 C33 C32 -161.2(5) . . . . ?
C45 N6 C34 C35 162.4(5) . . . . ?
C56 N6 C34 C35 -73.3(6) . . . . ?
C36 O4 C35 C34 -175.8(5) . . . . ?
N6 C34 C35 O4 -60.5(7) . . . . ?
C40 C41 C36 O4 -179.0(5) . . . . ?
C40 C41 C36 C37 0.3(8) . . . . ?
C35 O4 C36 C41 172.3(5) . . . . ?
C35 O4 C36 C37 -6.9(8) . . . . ?
C41 C36 C37 C38 0.9(8) . . . . ?
O4 C36 C37 C38 -179.9(5) . . . . ?
C36 C37 C38 C39 -0.1(8) . . . . ?
C41 C40 C39 C38 3.0(8) . . . . ?
C42 C40 C39 C38 -177.7(5) . . . . ?
C37 C38 C39 C40 -1.8(8) . . . . ?
C36 C41 C40 C39 -2.3(8) . . . . ?
C36 C41 C40 C42 178.4(5) . . . . ?
C43 N9 C42 C40 -168.4(4) . . . . ?
C39 C40 C42 N9 -92.8(6) . . . . ?
C41 C40 C42 N9 86.6(6) . . . . ?
C42 N9 C43 C44 176.3(4) . . . . ?
C55 N7 C44 C43 -78.4(5) . . . . ?
C66 N7 C44 C43 161.3(4) . . . . ?
N9 C43 C44 N7 -84.1(5) . . . . ?
O5 C46 C45 N6 -63.0(6) . . . . ?
C56 N6 C45 C46 157.3(5) . . . . ?
C34 N6 C45 C46 -78.0(6) . . . . ?
C47 O5 C46 C45 -174.0(4) . . . . ?
C46 O5 C47 C52 -179.3(5) . . . . ?
C46 O5 C47 C48 0.9(8) . . . . ?
C51 C52 C47 O5 -178.5(5) . . . . ?
C51 C52 C47 C48 1.3(8) . . . . ?
O5 C47 C48 C49 178.5(5) . . . . ?
C52 C47 C48 C49 -1.3(8) . . . . ?
C51 C50 C49 C48 -0.5(8) . . . . ?
C47 C48 C49 C50 0.9(8) . . . . ?
C47 C52 C51 C50 -0.8(8) . . . . ?
C47 C52 C51 C53 179.9(5) . . . . ?
C49 C50 C51 C52 0.4(8) . . . . ?
C49 C50 C51 C53 179.7(5) . . . . ?
N8 C53 C51 C52 89.5(6) . . . . ?
N8 C53 C51 C50 -89.8(6) . . . . ?
C54 N8 C53 C51 -171.7(4) . . . . ?
C53 N8 C54 C55 164.1(4) . . . . ?
N7 C55 C54 N8 -82.3(6) . . . . ?
C44 N7 C55 C54 164.2(4) . . . . ?
C66 N7 C55 C54 -76.1(6) . . . . ?
O6 C57 C56 N6 -65.1(6) . . . . ?
C45 N6 C56 C57 -75.8(6) . . . . ?
C34 N6 C56 C57 160.9(5) . . . . ?
C58 O6 C57 C56 178.0(5) . . . . ?
C57 O6 C58 C59 -4.5(8) . . . . ?
C57 O6 C58 C63 174.1(5) . . . . ?
C62 C63 C58 O6 177.1(5) . . . . ?
C62 C63 C58 C59 -4.2(8) . . . . ?
C61 C60 C59 C58 -0.8(8) . . . . ?
O6 C58 C59 C60 -178.2(5) . . . . ?
C63 C58 C59 C60 3.3(8) . . . . ?
C63 C62 C61 C60 -0.2(8) . . . . ?
C64 C62 C61 C60 -178.7(5) . . . . ?
C59 C60 C61 C62 -0.7(9) . . . . ?
C58 C63 C62 C61 2.7(8) . . . . ?
C58 C63 C62 C64 -178.8(5) . . . . ?
C65 N10 C64 C62 -165.2(5) . . . . ?
C61 C62 C64 N10 -83.9(7) . . . . ?
C63 C62 C64 N10 97.6(6) . . . . ?
C64 N10 C65 C66 170.5(5) . . . . ?
N7 C66 C65 N10 -83.2(6) . . . . ?
C55 N7 C66 C65 160.2(5) . . . . ?
C44 N7 C66 C65 -80.3(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        28.36
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.766
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.148

data_complex4
_database_code_depnum_ccdc_archive 'CCDC 727167'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C11 H26 N1.67 O8 S0.50'
_chemical_formula_sum            'C11 H26 N1.67 O8 S0.50'
_chemical_formula_weight         325.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           Cubic
_symmetry_space_group_name_H-M   'P 43 3 2'

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

_cell_length_a                   21.972(5)
_cell_length_b                   21.972(5)
_cell_length_c                   21.972(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     10607(4)
_cell_formula_units_Z            24
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.1
_cell_measurement_theta_max      28.3

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4036
_exptl_absorpt_coefficient_mu    0.159
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9690
_exptl_absorpt_correction_T_max  0.9735
_exptl_absorpt_process_details   'SADABS 2.10 (Bruker 2003)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       /w-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            71603
_diffrn_reflns_av_R_equivalents  0.0769
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.07
_diffrn_reflns_theta_max         28.28
_reflns_number_total             4417
_reflns_number_gt                3451
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART 5.628 (Bruker, 2003)'
_computing_cell_refinement       'SAINT 6.45 ( Bruker, 2003)'
_computing_data_reduction        'SAINT 6.45 (Bruker, 2003)'
_computing_structure_solution    SIR-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond 2.1e'
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.1(2)
_refine_ls_number_reflns         4417
_refine_ls_number_parameters     187
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1109
_refine_ls_R_factor_gt           0.0701
_refine_ls_wR_factor_ref         0.2485
_refine_ls_wR_factor_gt          0.1844
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_restrained_S_all      1.103
_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
S1 S 0.8750 0.92696(5) 0.67696(5) 0.0363(4) Uani 1 2 d S . .
O1 O 1.04387(15) 0.92817(15) 0.90679(15) 0.0411(8) Uani 1 1 d . . .
O2 O 0.86921(15) 0.91546(14) 0.74351(14) 0.0390(7) Uani 1 1 d . . .
O3 O 0.92917(17) 0.89537(17) 0.65581(16) 0.0514(9) Uani 1 1 d . . .
N1 N 1.00332(17) 1.00332(17) 1.00332(17) 0.0379(13) Uani 1 3 d S . .
N2 N 0.78170(16) 0.78170(16) 0.78170(16) 0.0361(14) Uani 1 3 d S . .
N3 N 0.91487(16) 0.79741(17) 0.75830(16) 0.0343(8) Uani 1 1 d . . .
H3A H 0.9056 0.8365 0.7503 0.041 Uiso 1 1 calc R . .
H3B H 0.9073 0.7905 0.7979 0.041 Uiso 1 1 calc R . .
C1 C 0.8089(2) 0.7750(2) 0.7208(2) 0.0386(10) Uani 1 1 d . . .
H1A H 0.8049 0.8134 0.6994 0.046 Uiso 1 1 calc R . .
H1B H 0.7858 0.7448 0.6984 0.046 Uiso 1 1 calc R . .
C2 C 0.8753(2) 0.7566(2) 0.7203(2) 0.0375(9) Uani 1 1 d . . .
H2A H 0.8788 0.7152 0.7353 0.045 Uiso 1 1 calc R . .
H2B H 0.8901 0.7570 0.6787 0.045 Uiso 1 1 calc R . .
C3 C 0.9814(2) 0.7870(2) 0.7459(2) 0.0382(10) Uani 1 1 d . . .
H3C H 0.9876 0.7827 0.7024 0.046 Uiso 1 1 calc R . .
H3D H 0.9941 0.7494 0.7653 0.046 Uiso 1 1 calc R . .
C4 C 1.0205(2) 0.8392(2) 0.7696(2) 0.0373(9) Uani 1 1 d . . .
C5 C 1.0633(2) 0.8650(2) 0.7303(2) 0.0402(10) Uani 1 1 d . . .
H5 H 1.0664 0.8510 0.6904 0.048 Uiso 1 1 calc R . .
C6 C 1.1006(2) 0.9103(2) 0.7500(2) 0.0407(10) Uani 1 1 d . . .
H6 H 1.1297 0.9263 0.7237 0.049 Uiso 1 1 calc R . .
C7 C 1.0956(2) 0.9332(2) 0.8092(2) 0.0392(10) Uani 1 1 d . . .
H7 H 1.1207 0.9646 0.8224 0.047 Uiso 1 1 calc R . .
C8 C 1.0526(2) 0.9083(2) 0.8478(2) 0.0378(9) Uani 1 1 d . . .
C9 C 1.0151(2) 0.8602(2) 0.8288(2) 0.0372(9) Uani 1 1 d . . .
H9 H 0.9872 0.8428 0.8554 0.045 Uiso 1 1 calc R . .
C10 C 1.0826(2) 0.9749(2) 0.9273(2) 0.0418(10) Uani 1 1 d . . .
H10A H 1.0752 1.0121 0.9046 0.050 Uiso 1 1 calc R . .
H10B H 1.1249 0.9633 0.9219 0.050 Uiso 1 1 calc R . .
C11 C 1.0689(2) 0.9845(2) 0.9933(2) 0.0419(10) Uani 1 1 d . . .
H11A H 1.0956 1.0157 1.0094 0.050 Uiso 1 1 calc R . .
H11B H 1.0768 0.9471 1.0154 0.050 Uiso 1 1 calc R . .
OW1 O 1.1250 0.7418(8) 0.5082(8) 0.054(12) Uani 1 2 d S . .
OW2 O 1.0953(8) 0.8632(7) 0.5319(5) 0.048(7) Uani 1 1 d . . .
OW3 O 1.0873(4) 0.9127(4) 0.4127(4) 0.048(4) Uani 1 3 d S . .
OW4 O 1.2490(13) 0.774(2) 0.5305(10) 0.045(6) Uani 1 1 d . . .
OW5 O 1.1786(8) 0.9147(18) 0.6165(6) 0.045(4) Uani 1 1 d . . .
OW6 O 1.1841(4) 1.0801(4) 0.5200(9) 0.049 Uani 1 1 d . . .
OW7 O 1.1250 1.1250 1.1250 0.044(4) Uani 1 6 d S . .


_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
S1 O3 1.454(4) 23_654 ?
S1 O3 1.454(4) . ?
S1 O2 1.489(3) 23_654 ?
S1 O2 1.489(3) . ?
O1 C8 1.381(6) . ?
O1 C10 1.408(6) . ?
N1 C11 1.514(5) 5 ?
N1 C11 1.515(5) . ?
N1 C11 1.514(5) 6 ?
N2 C1 1.473(5) 5 ?
N2 C1 1.473(5) . ?
N2 C1 1.473(5) 6 ?
N3 C3 1.505(5) . ?
N3 C2 1.502(6) . ?
N3 H3A 0.9000 . ?
N3 H3B 0.9000 . ?
C1 C2 1.515(7) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C4 C5 1.397(7) . ?
C4 C3 1.524(6) . ?
C5 C6 1.361(7) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.382(7) . ?
C7 C6 1.401(7) . ?
C7 H7 0.9300 . ?
C8 C9 1.403(6) . ?
C9 C4 1.386(6) . ?
C9 H9 0.9300 . ?
C10 C11 1.496(7) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 S1 O3 111.4(3) 23_654 . ?
O3 S1 O2 107.62(19) 23_654 23_654 ?
O3 S1 O2 110.1(2) . 23_654 ?
O3 S1 O2 110.2(2) 23_654 . ?
O3 S1 O2 107.63(19) . . ?
O2 S1 O2 109.9(3) 23_654 . ?
C8 O1 C10 116.6(3) . . ?
C11 N1 C11 111.0(3) 5 . ?
C11 N1 C11 111.0(3) 5 6 ?
C11 N1 C11 111.0(3) . 6 ?
C1 N2 C1 108.6(3) 5 . ?
C1 N2 C1 108.6(3) 5 6 ?
C1 N2 C1 108.6(3) . 6 ?
C3 N3 C2 111.8(3) . . ?
C3 N3 H3A 109.3 . . ?
C2 N3 H3A 109.3 . . ?
C3 N3 H3B 109.3 . . ?
C2 N3 H3B 109.2 . . ?
H3A N3 H3B 107.9 . . ?
N2 C1 C2 115.1(3) . . ?
N2 C1 H1A 108.5 . . ?
C2 C1 H1A 108.5 . . ?
N2 C1 H1B 108.5 . . ?
C2 C1 H1B 108.5 . . ?
H1A C1 H1B 107.5 . . ?
N3 C2 C1 113.2(3) . . ?
N3 C2 H2A 109.0 . . ?
C1 C2 H2A 109.0 . . ?
N3 C2 H2B 108.9 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
N3 C3 C4 111.8(3) . . ?
N3 C3 H3C 109.3 . . ?
C4 C3 H3C 109.3 . . ?
N3 C3 H3D 109.2 . . ?
C4 C3 H3D 109.2 . . ?
H3C C3 H3D 107.9 . . ?
C9 C4 C5 120.2(4) . . ?
C9 C4 C3 121.5(4) . . ?
C5 C4 C3 118.3(4) . . ?
C6 C5 C4 120.4(5) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C5 C6 C7 120.8(4) . . ?
C5 C6 H6 119.7 . . ?
C7 C6 H6 119.6 . . ?
C8 C7 C6 118.8(4) . . ?
C8 C7 H7 120.7 . . ?
C6 C7 H7 120.6 . . ?
O1 C8 C7 123.0(4) . . ?
O1 C8 C9 115.8(4) . . ?
C7 C8 C9 121.2(4) . . ?
C4 C9 C8 118.7(4) . . ?
C4 C9 H9 120.7 . . ?
C8 C9 H9 120.7 . . ?
O1 C10 C11 106.9(4) . . ?
O1 C10 H10A 110.4 . . ?
C11 C10 H10A 110.4 . . ?
O1 C10 H10B 110.4 . . ?
C11 C10 H10B 110.3 . . ?
H10A C10 H10B 108.6 . . ?
C10 C11 N1 111.8(4) . . ?
C10 C11 H11A 109.3 . . ?
N1 C11 H11A 109.2 . . ?
C10 C11 H11B 109.3 . . ?
N1 C11 H11B 109.3 . . ?
H11A C11 H11B 107.9 . . ?

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
C1 N2 C1 C2 171.1(4) 5 . . . ?
C1 N2 C1 C2 -71.0(6) 6 . . . ?
C3 N3 C2 C1 -167.1(4) . . . . ?
N2 C1 C2 N3 -53.4(5) . . . . ?
C2 N3 C3 C4 163.5(4) . . . . ?
C9 C4 C3 N3 51.1(5) . . . . ?
C5 C4 C3 N3 -130.3(4) . . . . ?
C8 C9 C4 C5 1.1(6) . . . . ?
C8 C9 C4 C3 179.8(4) . . . . ?
C9 C4 C5 C6 0.8(6) . . . . ?
C3 C4 C5 C6 -177.9(4) . . . . ?
C4 C5 C6 C7 -1.8(7) . . . . ?
C8 C7 C6 C5 0.9(7) . . . . ?
C10 O1 C8 C7 -1.7(6) . . . . ?
C10 O1 C8 C9 177.8(4) . . . . ?
C6 C7 C8 O1 -179.4(4) . . . . ?
C6 C7 C8 C9 1.1(7) . . . . ?
O1 C8 C9 C4 178.4(4) . . . . ?
C7 C8 C9 C4 -2.1(7) . . . . ?
C8 O1 C10 C11 -174.7(4) . . . . ?
O1 C10 C11 N1 -60.6(5) . . . . ?
C11 N1 C11 C10 -74.2(6) 5 . . . ?
C11 N1 C11 C10 161.8(4) 6 . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.150

data_complex5
_database_code_depnum_ccdc_archive 'CCDC 727168'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H54 N8 O18 S'
_chemical_formula_sum            'C33 H54 N8 O18 S'
_chemical_formula_weight         882.90

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           Monoclinic
_symmetry_space_group_name_H-M   'P 21/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                   9.810(3)
_cell_length_b                   25.932(6)
_cell_length_c                   16.314(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.869(6)
_cell_angle_gamma                90.00
_cell_volume                     4101(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      28.4

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1872
_exptl_absorpt_coefficient_mu    0.165
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9663
_exptl_absorpt_correction_T_max  0.9741
_exptl_absorpt_process_details   'SADABS 2.10 (Bruker 2003)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       /w-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27061
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_sigmaI/netI    0.0789
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.02
_diffrn_reflns_theta_max         28.36
_reflns_number_total             10139
_reflns_number_gt                5197
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART 5.628 (Bruker, 2003)'
_computing_cell_refinement       'SAINT 6.45 ( Bruker, 2003)'
_computing_data_reduction        'SAINT 6.45 (Bruker, 2003)'
_computing_structure_solution    SIR-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond 2.1e'
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10139
_refine_ls_number_parameters     536
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.0787
_refine_ls_wR_factor_ref         0.2255
_refine_ls_wR_factor_gt          0.1945
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_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
S1 S 1.1867(4) -0.05037(10) -0.33122(17) 0.0432(12) Uani 1 1 d . . .
O1 O 0.5102(4) 0.32916(15) 0.0725(2) 0.0401(10) Uani 1 1 d . . .
O2 O 0.9137(4) 0.33313(15) 0.1567(2) 0.0411(10) Uani 1 1 d . . .
O3 O 0.7933(4) 0.33776(15) -0.0928(2) 0.0407(10) Uani 1 1 d . . .
O4 O 0.8935(3) 0.18337(14) 0.0244(2) 0.0349(9) Uani 1 1 d . . .
O5 O 0.6760(3) 0.18121(15) -0.0293(2) 0.0346(9) Uani 1 1 d . . .
O6 O 0.7363(3) 0.17881(15) 0.1039(2) 0.0348(9) Uani 1 1 d . . .
O7 O 1.1788(4) 0.08848(16) -0.0382(2) 0.0418(10) Uani 1 1 d . . .
O8 O 1.1314(4) 0.10256(18) -0.1711(2) 0.0475(11) Uani 1 1 d . . .
O9 O 1.3418(4) 0.08868(15) -0.1141(2) 0.0382(9) Uani 1 1 d . . .
O10 O 1.5445(13) -0.0155(6) -0.3239(5) 0.045(8) Uani 1 1 d . . .
O11 O 1.6894(5) -0.0386(2) -0.2154(4) 0.0386(16) Uani 1 1 d . . .
O12 O 1.5164(8) 0.0113(2) -0.2050(4) 0.041(2) Uani 1 1 d . . .
O13 O 1.2454(7) -0.0021(3) -0.2760(4) 0.045(2) Uani 1 1 d . . .
H13 H 1.3264 0.0027 -0.2809 0.146 Uiso 1 1 calc R . .
O14 O 1.1992(9) -0.0388(2) -0.4151(4) 0.038(3) Uani 1 1 d . . .
O15 O 1.2683(15) -0.0921(3) -0.2902(7) 0.040(6) Uani 1 1 d . . .
O16 O 1.0518(7) -0.0577(4) -0.3222(4) 0.038(4) Uani 1 1 d . . .
OW1 O 1.6014(8) 0.0376(3) -0.4821(4) 0.046(3) Uani 1 1 d . . .
OW2 O 1.8519(15) 0.0409(4) -0.3218(6) 0.045(7) Uani 1 1 d . . .
N1 N 0.7815(4) 0.06623(18) 0.0262(3) 0.0318(10) Uani 1 1 d . . .
H1 H 0.7792 0.1012 0.0301 0.038 Uiso 1 1 calc R . .
N2 N 0.7265(5) 0.39718(19) 0.0466(3) 0.0342(12) Uani 1 1 d . . .
N3 N 0.4860(4) 0.11993(17) 0.0428(3) 0.0310(10) Uani 1 1 d . . .
H3C H 0.5504 0.1408 0.0268 0.037 Uiso 1 1 calc R . .
H3D H 0.4248 0.1121 -0.0025 0.037 Uiso 1 1 calc R . .
N4 N 0.9565(4) 0.12156(17) 0.1830(3) 0.0325(10) Uani 1 1 d . . .
H4A H 0.8873 0.1393 0.1530 0.039 Uiso 1 1 calc R . .
H4B H 0.9243 0.1086 0.2274 0.039 Uiso 1 1 calc R . .
N5 N 0.8740(4) 0.13117(18) -0.1284(3) 0.0337(11) Uani 1 1 d . . .
H5A H 0.9612 0.1215 -0.1312 0.040 Uiso 1 1 calc R . .
H5B H 0.8747 0.1488 -0.0809 0.040 Uiso 1 1 calc R . .
N6 N 0.7687(4) 0.18211(17) 0.0336(3) 0.0381(10) Uani 1 1 d . . .
N7 N 1.2172(5) 0.09319(17) -0.1077(3) 0.0349(11) Uani 1 1 d . . .
N8 N 1.5916(6) -0.0140(2) -0.2502(4) 0.0414(16) Uani 1 1 d . . .
C1 C 0.6398(5) 0.0453(2) 0.0205(4) 0.0349(13) Uani 1 1 d . . .
H1A H 0.6455 0.0088 0.0329 0.042 Uiso 1 1 calc R . .
H1B H 0.5932 0.0492 -0.0361 0.042 Uiso 1 1 calc R . .
C2 C 0.5537(5) 0.0713(2) 0.0786(3) 0.0330(12) Uani 1 1 d . . .
H2A H 0.4831 0.0474 0.0906 0.040 Uiso 1 1 calc R . .
H2B H 0.6124 0.0793 0.1305 0.040 Uiso 1 1 calc R . .
C3 C 0.4132(5) 0.1480(2) 0.1039(3) 0.0350(13) Uani 1 1 d . . .
C4 C 0.3648(5) 0.2009(2) 0.0723(3) 0.0320(12) Uani 1 1 d . . .
H3A H 0.4753 0.1516 0.1559 0.042 Uiso 1 1 calc R . .
H3B H 0.3344 0.1279 0.1143 0.042 Uiso 1 1 calc R . .
C5 C 0.2305(5) 0.2082(2) 0.0319(3) 0.0356(13) Uani 1 1 d . . .
H5 H 0.1702 0.1804 0.0226 0.043 Uiso 1 1 calc R . .
C6 C 0.1873(6) 0.2571(2) 0.0056(3) 0.0391(14) Uani 1 1 d . . .
H6 H 0.0974 0.2623 -0.0207 0.047 Uiso 1 1 calc R . .
C7 C 0.2783(6) 0.2986(2) 0.0185(3) 0.0385(14) Uani 1 1 d . . .
H7 H 0.2491 0.3315 0.0009 0.046 Uiso 1 1 calc R . .
C8 C 0.4104(5) 0.2909(2) 0.0571(3) 0.0343(13) Uani 1 1 d . . .
C9 C 0.4543(5) 0.2421(2) 0.0836(3) 0.0327(12) Uani 1 1 d . . .
H9 H 0.5448 0.2371 0.1092 0.039 Uiso 1 1 calc R . .
C10 C 0.4735(6) 0.3805(2) 0.0424(4) 0.0346(15) Uani 1 1 d . . .
H10A H 0.3903 0.3922 0.0621 0.055 Uiso 1 1 calc R . .
H10B H 0.4581 0.3812 -0.0178 0.055 Uiso 1 1 calc R . .
C11 C 0.5933(6) 0.4137(2) 0.0761(4) 0.0332(16) Uani 1 1 d . . .
H11A H 0.6062 0.4124 0.1363 0.060 Uiso 1 1 calc R . .
H11B H 0.5730 0.4491 0.0594 0.060 Uiso 1 1 calc R . .
C12 C 0.8685(5) 0.0450(2) 0.0991(3) 0.0337(12) Uani 1 1 d . . .
H12A H 0.8994 0.0110 0.0854 0.040 Uiso 1 1 calc R . .
H12B H 0.8133 0.0410 0.1431 0.040 Uiso 1 1 calc R . .
C13 C 0.9941(5) 0.0775(2) 0.1313(4) 0.0344(13) Uani 1 1 d . . .
H13A H 1.0628 0.0562 0.1644 0.041 Uiso 1 1 calc R . .
H13B H 1.0341 0.0909 0.0848 0.041 Uiso 1 1 calc R . .
C14 C 1.0697(5) 0.1580(2) 0.2126(3) 0.0334(12) Uani 1 1 d . . .
H14A H 1.1216 0.1653 0.1679 0.040 Uiso 1 1 calc R . .
H14B H 1.1319 0.1424 0.2577 0.040 Uiso 1 1 calc R . .
C15 C 1.0138(5) 0.2074(2) 0.2418(3) 0.0311(12) Uani 1 1 d . . .
C16B C 0.9794(5) 0.2108(2) 0.3221(3) 0.0370(13) Uani 1 1 d . . .
H16B H 0.9927 0.1827 0.3579 0.044 Uiso 1 1 calc R . .
C17 C 0.9253(6) 0.2565(2) 0.3475(3) 0.0388(14) Uani 1 1 d . . .
H17 H 0.9028 0.2587 0.4007 0.047 Uiso 1 1 calc R . .
C18 C 0.9042(6) 0.2984(2) 0.2959(3) 0.0379(13) Uani 1 1 d . . .
H18 H 0.8700 0.3290 0.3143 0.045 Uiso 1 1 calc R . .
C19 C 0.9350(5) 0.2944(2) 0.2151(3) 0.0337(12) Uani 1 1 d . . .
C20 C 0.9932(5) 0.2493(2) 0.1884(3) 0.0304(12) Uani 1 1 d . . .
H20 H 1.0177 0.2475 0.1356 0.036 Uiso 1 1 calc R . .
C21 C 0.8740(7) 0.3825(2) 0.1832(4) 0.0390(14) Uani 1 1 d . . .
H21A H 0.9467 0.3972 0.2235 0.051 Uiso 1 1 calc R . .
H21B H 0.7908 0.3799 0.2083 0.051 Uiso 1 1 calc R . .
C22 C 0.8491(6) 0.4153(2) 0.1067(4) 0.0386(15) Uani 1 1 d . . .
H22A H 0.9304 0.4146 0.0796 0.055 Uiso 1 1 calc R . .
H22B H 0.8341 0.4507 0.1224 0.055 Uiso 1 1 calc R . .
C23 C 0.8369(5) 0.0513(2) -0.0496(3) 0.0332(12) Uani 1 1 d . . .
H23A H 0.8117 0.0157 -0.0625 0.040 Uiso 1 1 calc R . .
H23B H 0.9368 0.0530 -0.0381 0.040 Uiso 1 1 calc R . .
C24 C 0.7874(6) 0.0844(2) -0.1264(3) 0.0403(14) Uani 1 1 d . . .
H24A H 0.7906 0.0642 -0.1760 0.048 Uiso 1 1 calc R . .
H24B H 0.6923 0.0946 -0.1260 0.048 Uiso 1 1 calc R . .
C25 C 0.8248(6) 0.1659(2) -0.1999(3) 0.0412(14) Uani 1 1 d . . .
H25A H 0.7250 0.1685 -0.2070 0.049 Uiso 1 1 calc R . .
H25B H 0.8498 0.1513 -0.2503 0.049 Uiso 1 1 calc R . .
C26 C 0.8876(6) 0.2198(2) -0.1862(3) 0.0369(13) Uani 1 1 d . . .
C27 C 1.0100(6) 0.2329(2) -0.2142(3) 0.0362(14) Uani 1 1 d . . .
H27 H 1.0569 0.2086 -0.2410 0.047 Uiso 1 1 calc R . .
C28 C 1.0613(6) 0.2825(3) -0.2018(3) 0.0328(16) Uani 1 1 d . . .
H28 H 1.1444 0.2909 -0.2191 0.055 Uiso 1 1 calc R . .
C29 C 0.9902(6) 0.3200(2) -0.1636(3) 0.0374(13) Uani 1 1 d . . .
H29 H 1.0225 0.3538 -0.1577 0.045 Uiso 1 1 calc R . .
C30 C 0.8688(5) 0.3052(2) -0.1344(3) 0.0333(12) Uani 1 1 d . . .
C31 C 0.8180(5) 0.2564(2) -0.1468(3) 0.0343(13) Uani 1 1 d . . .
H31 H 0.7358 0.2476 -0.1285 0.041 Uiso 1 1 calc R . .
C32 C 0.8364(6) 0.3903(2) -0.0819(4) 0.0435(15) Uani 1 1 d . . .
H32A H 0.8409 0.4063 -0.1352 0.052 Uiso 1 1 calc R . .
H32B H 0.9269 0.3923 -0.0484 0.052 Uiso 1 1 calc R . .
C33 C 0.7306(7) 0.4174(2) -0.0389(4) 0.0389(16) Uani 1 1 d . . .
H33A H 0.7516 0.4540 -0.0355 0.059 Uiso 1 1 calc R . .
H33B H 0.6402 0.4133 -0.0719 0.059 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
S1 O13 1.597(7) . ?
S1 O14 1.424(6) . ?
S1 O15 1.448(10) . ?
S1 O16 1.367(7) . ?
O1 C8 1.389(7) . ?
O1 C10 1.446(7) . ?
O2 C19 1.379(6) . ?
O2 C21 1.425(7) . ?
O3 C30 1.370(6) . ?
O3 C32 1.431(7) . ?
O4 N6 1.257(5) . ?
O5 N6 1.262(5) . ?
O6 N6 1.240(5) . ?
O7 N7 1.255(6) . ?
O8 N7 1.252(6) . ?
O9 N7 1.249(6) . ?
N1 C12 1.461(7) . ?
N1 C23 1.478(7) . ?
N1 C1 1.481(7) . ?
N1 H1 0.9100 . ?
N2 C33 1.497(8) . ?
N2 C22 1.505(7) . ?
N2 C11 1.521(8) . ?
N3 C3 1.500(6) . ?
N3 C2 1.502(7) . ?
N3 H3C 0.9000 . ?
N3 H3D 0.9000 . ?
N4 C14 1.482(7) . ?
N4 C13 1.499(7) . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
N5 C24 1.484(7) . ?
N5 C25 1.495(7) . ?
N5 H5A 0.9000 . ?
N5 H5B 0.9000 . ?
N8 O11 1.217(7) . ?
N8 O10 1.220(8) . ?
N8 O12 1.299(8) . ?
C1 C2 1.520(7) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C9 1.377(8) . ?
C4 C5 1.392(7) . ?
C4 C3 1.517(8) . ?
C5 C6 1.384(8) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C6 1.394(8) . ?
C7 H7 0.9300 . ?
C8 C7 1.365(8) . ?
C8 C9 1.385(8) . ?
C9 H9 0.9300 . ?
C10 C11 1.492(9) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.518(8) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
O13 H13 0.8200 . ?
C14 C15 1.500(7) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C16B C17 1.387(8) . ?
C16B C15 1.405(7) . ?
C16B H16B 0.9300 . ?
C17 H17 0.9300 . ?
C18 C17 1.369(8) . ?
C18 H18 0.9300 . ?
C19 C20 1.399(7) . ?
C19 C18 1.401(7) . ?
C20 C15 1.389(7) . ?
C20 H20 0.9300 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C21 1.498(8) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C23 1.534(8) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C26 1.529(8) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C31 1.383(8) . ?
C26 C27 1.391(8) . ?
C27 H27 0.9300 . ?
C28 C27 1.383(9) . ?
C28 H28 0.9300 . ?
C29 C28 1.399(9) . ?
C29 H29 0.9300 . ?
C30 C31 1.365(7) . ?
C30 C29 1.402(7) . ?
C31 H31 0.9300 . ?
C32 C33 1.512(9) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O14 S1 O13 107.4(3) . . ?
O14 S1 O15 118.6(5) . . ?
O15 S1 O13 101.5(6) . . ?
O16 S1 O13 108.6(5) . . ?
O16 S1 O14 111.1(5) . . ?
O16 S1 O15 108.8(6) . . ?
C8 O1 C10 117.6(4) . . ?
C19 O2 C21 117.7(4) . . ?
C30 O3 C32 118.4(4) . . ?
S1 O13 H13 109.5 . . ?
C12 N1 C23 109.8(4) . . ?
C12 N1 C1 109.8(4) . . ?
C23 N1 C1 108.4(4) . . ?
C12 N1 H1 109.6 . . ?
C23 N1 H1 109.6 . . ?
C1 N1 H1 109.6 . . ?
C33 N2 C22 111.3(5) . . ?
C33 N2 C11 110.1(5) . . ?
C22 N2 C11 110.2(5) . . ?
C3 N3 C2 112.1(4) . . ?
C3 N3 H3C 109.2 . . ?
C2 N3 H3C 109.2 . . ?
C3 N3 H3D 109.2 . . ?
C2 N3 H3D 109.2 . . ?
H3C N3 H3D 107.9 . . ?
C14 N4 C13 115.6(4) . . ?
C14 N4 H4A 108.4 . . ?
C13 N4 H4A 108.4 . . ?
C14 N4 H4B 108.4 . . ?
C13 N4 H4B 108.4 . . ?
H4A N4 H4B 107.4 . . ?
C24 N5 C25 113.2(4) . . ?
C24 N5 H5A 108.9 . . ?
C25 N5 H5A 108.9 . . ?
C24 N5 H5B 108.9 . . ?
C25 N5 H5B 108.9 . . ?
H5A N5 H5B 107.8 . . ?
O6 N6 O4 120.4(4) . . ?
O6 N6 O5 119.7(4) . . ?
O4 N6 O5 119.8(4) . . ?
O9 N7 O8 119.5(5) . . ?
O9 N7 O7 120.0(5) . . ?
O8 N7 O7 120.5(4) . . ?
O11 N8 O10 126.6(7) . . ?
O11 N8 O12 118.4(6) . . ?
O10 N8 O12 114.3(7) . . ?
N1 C1 C2 113.9(4) . . ?
N1 C1 H1A 108.8 . . ?
N1 C1 H1B 108.8 . . ?
C2 C1 H1A 108.8 . . ?
C2 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
N3 C2 C1 112.5(4) . . ?
N3 C2 H2A 109.1 . . ?
C1 C2 H2A 109.1 . . ?
N3 C2 H2B 109.1 . . ?
C1 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
N3 C3 C4 111.7(4) . . ?
N3 C3 H3A 109.3 . . ?
C4 C3 H3A 109.3 . . ?
N3 C3 H3B 109.3 . . ?
C4 C3 H3B 109.3 . . ?
H3A C3 H3B 107.9 . . ?
C9 C4 C5 119.7(5) . . ?
C9 C4 C3 119.8(5) . . ?
C5 C4 C3 120.5(5) . . ?
C6 C5 C4 119.5(6) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C7 120.2(5) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C8 C7 C6 119.8(6) . . ?
C8 C7 H7 120.1 . . ?
C6 C7 H7 120.1 . . ?
C7 C8 C9 120.3(5) . . ?
C7 C8 O1 124.9(5) . . ?
C9 C8 O1 114.8(5) . . ?
C4 C9 C8 120.4(5) . . ?
C4 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
O1 C10 C11 105.3(5) . . ?
O1 C10 H10A 110.7 . . ?
C11 C10 H10A 110.7 . . ?
O1 C10 H10B 110.7 . . ?
C11 C10 H10B 110.7 . . ?
H10A C10 H10B 108.8 . . ?
C10 C11 N2 112.8(5) . . ?
C10 C11 H11A 109.0 . . ?
N2 C11 H11A 109.0 . . ?
C10 C11 H11B 109.0 . . ?
N2 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
N1 C12 C13 114.5(4) . . ?
N1 C12 H12A 108.6 . . ?
C13 C12 H12A 108.6 . . ?
N1 C12 H12B 108.6 . . ?
C13 C12 H12B 108.6 . . ?
H12A C12 H12B 107.6 . . ?
N4 C13 C12 111.1(4) . . ?
N4 C13 H13A 109.4 . . ?
C12 C13 H13A 109.4 . . ?
N4 C13 H13B 109.4 . . ?
C12 C13 H13B 109.4 . . ?
H13A C13 H13B 108.0 . . ?
N4 C14 C15 110.9(4) . . ?
N4 C14 H14A 109.5 . . ?
C15 C14 H14A 109.5 . . ?
N4 C14 H14B 109.5 . . ?
C15 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
C20 C15 C16B 120.2(5) . . ?
C20 C15 C14 119.6(5) . . ?
C16B C15 C14 120.2(5) . . ?
C17 C16B C15 119.3(5) . . ?
C17 C16B H16B 120.3 . . ?
C15 C16B H16B 120.3 . . ?
C18 C17 C16B 121.5(5) . . ?
C18 C17 H17 119.3 . . ?
C16B C17 H17 119.3 . . ?
C17 C18 C19 119.1(5) . . ?
C17 C18 H18 120.5 . . ?
C19 C18 H18 120.5 . . ?
O2 C19 C20 114.7(5) . . ?
O2 C19 C18 124.4(5) . . ?
C20 C19 C18 120.8(5) . . ?
C15 C20 C19 119.0(5) . . ?
C15 C20 H20 120.5 . . ?
C19 C20 H20 120.5 . . ?
O2 C21 C22 105.9(5) . . ?
O2 C21 H21A 110.6 . . ?
C22 C21 H21A 110.6 . . ?
O2 C21 H21B 110.6 . . ?
C22 C21 H21B 110.6 . . ?
H21A C21 H21B 108.7 . . ?
C21 C22 N2 112.2(5) . . ?
C21 C22 H22A 109.2 . . ?
N2 C22 H22A 109.2 . . ?
C21 C22 H22B 109.2 . . ?
N2 C22 H22B 109.2 . . ?
H22A C22 H22B 107.9 . . ?
N1 C23 C24 115.1(4) . . ?
N1 C23 H23A 108.5 . . ?
C24 C23 H23A 108.5 . . ?
N1 C23 H23B 108.5 . . ?
C24 C23 H23B 108.5 . . ?
H23A C23 H23B 107.5 . . ?
N5 C24 C23 111.4(4) . . ?
N5 C24 H24A 109.3 . . ?
C23 C24 H24A 109.3 . . ?
N5 C24 H24B 109.3 . . ?
C23 C24 H24B 109.3 . . ?
H24A C24 H24B 108.0 . . ?
N5 C25 C26 111.2(4) . . ?
N5 C25 H25A 109.4 . . ?
C26 C25 H25A 109.4 . . ?
N5 C25 H25B 109.4 . . ?
C26 C25 H25B 109.4 . . ?
H25A C25 H25B 108.0 . . ?
C31 C26 C27 119.8(6) . . ?
C31 C26 C25 118.5(5) . . ?
C27 C26 C25 121.6(5) . . ?
C28 C27 C26 119.5(6) . . ?
C28 C27 H27 120.2 . . ?
C26 C27 H27 120.2 . . ?
C27 C28 C29 121.1(5) . . ?
C27 C28 H28 119.4 . . ?
C29 C28 H28 119.4 . . ?
C28 C29 C30 117.9(6) . . ?
C28 C29 H29 121.1 . . ?
C30 C29 H29 121.1 . . ?
C31 C30 O3 115.5(5) . . ?
C31 C30 C29 120.9(5) . . ?
O3 C30 C29 123.5(5) . . ?
C30 C31 C26 120.6(5) . . ?
C30 C31 H31 119.7 . . ?
C26 C31 H31 119.7 . . ?
O3 C32 C33 106.8(5) . . ?
O3 C32 H32A 110.4 . . ?
C33 C32 H32A 110.4 . . ?
O3 C32 H32B 110.4 . . ?
C33 C32 H32B 110.4 . . ?
H32A C32 H32B 108.6 . . ?
N2 C33 C32 112.9(5) . . ?
N2 C33 H33A 109.0 . . ?
C32 C33 H33A 109.0 . . ?
N2 C33 H33B 109.0 . . ?
C32 C33 H33B 109.0 . . ?
H33A C33 H33B 107.8 . . ?

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
C12 N1 C1 C2 78.8(6) . . . . ?
C23 N1 C1 C2 -161.4(4) . . . . ?
C3 N3 C2 C1 -174.2(4) . . . . ?
N1 C1 C2 N3 84.3(5) . . . . ?
C2 N3 C3 C4 171.0(4) . . . . ?
C9 C4 C3 N3 -84.5(6) . . . . ?
C5 C4 C3 N3 95.5(5) . . . . ?
C9 C4 C5 C6 -1.8(8) . . . . ?
C3 C4 C5 C6 178.2(5) . . . . ?
C4 C5 C6 C7 0.9(8) . . . . ?
C8 C7 C6 C5 0.1(8) . . . . ?
C9 C8 C7 C6 -0.2(8) . . . . ?
O1 C8 C7 C6 179.4(5) . . . . ?
C10 O1 C8 C7 -2.9(8) . . . . ?
C10 O1 C8 C9 176.7(5) . . . . ?
C5 C4 C9 C8 1.8(8) . . . . ?
C3 C4 C9 C8 -178.2(5) . . . . ?
C7 C8 C9 C4 -0.8(8) . . . . ?
O1 C8 C9 C4 179.6(5) . . . . ?
C8 O1 C10 C11 173.8(5) . . . . ?
O1 C10 C11 N2 60.7(7) . . . . ?
C33 N2 C11 C10 80.6(6) . . . . ?
C22 N2 C11 C10 -156.2(5) . . . . ?
C23 N1 C12 C13 84.1(5) . . . . ?
C1 N1 C12 C13 -156.9(4) . . . . ?
C14 N4 C13 C12 -175.7(4) . . . . ?
N1 C12 C13 N4 80.4(6) . . . . ?
C13 N4 C14 C15 163.8(4) . . . . ?
C19 C20 C15 C16B -1.4(7) . . . . ?
C19 C20 C15 C14 177.1(4) . . . . ?
C17 C16B C15 C20 -0.3(8) . . . . ?
C17 C16B C15 C14 -178.8(5) . . . . ?
N4 C14 C15 C20 -96.4(6) . . . . ?
N4 C14 C15 C16B 82.1(6) . . . . ?
C19 C18 C17 C16B 1.6(8) . . . . ?
C15 C16B C17 C18 0.2(8) . . . . ?
O2 C19 C18 C17 177.6(5) . . . . ?
C20 C19 C18 C17 -3.3(8) . . . . ?
C21 O2 C19 C20 -171.0(5) . . . . ?
C21 O2 C19 C18 8.1(8) . . . . ?
O2 C19 C20 C15 -177.6(4) . . . . ?
C18 C19 C20 C15 3.3(8) . . . . ?
C19 O2 C21 C22 -176.2(5) . . . . ?
N2 C22 C21 O2 66.7(6) . . . . ?
C33 N2 C22 C21 -160.5(5) . . . . ?
C11 N2 C22 C21 76.9(6) . . . . ?
C12 N1 C23 C24 -160.6(5) . . . . ?
C1 N1 C23 C24 79.5(6) . . . . ?
N5 C24 C23 N1 85.6(6) . . . . ?
C25 N5 C24 C23 -177.0(5) . . . . ?
C24 N5 C25 C26 163.1(5) . . . . ?
N5 C25 C26 C31 -90.0(6) . . . . ?
N5 C25 C26 C27 91.7(6) . . . . ?
C29 C28 C27 C26 -1.8(8) . . . . ?
C31 C26 C27 C28 0.4(8) . . . . ?
C25 C26 C27 C28 178.7(5) . . . . ?
C30 C29 C28 C27 3.2(8) . . . . ?
C31 C30 C29 C28 -3.3(8) . . . . ?
O3 C30 C29 C28 177.1(5) . . . . ?
C32 O3 C30 C31 -176.5(5) . . . . ?
C32 O3 C30 C29 3.2(7) . . . . ?
O3 C30 C31 C26 -178.3(4) . . . . ?
C29 C30 C31 C26 2.0(8) . . . . ?
C27 C26 C31 C30 -0.5(8) . . . . ?
C25 C26 C31 C30 -178.8(5) . . . . ?
C30 O3 C32 C33 176.8(4) . . . . ?
C22 N2 C33 C32 74.4(6) . . . . ?
C11 N2 C33 C32 -163.1(5) . . . . ?
O3 C32 C33 N2 64.4(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        28.36
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.768
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.117


