# Supplementary Material (ESI) for Organic & Biomolecular Chemistry
# This journal is © The Royal Society of Chemistry 2005

data_global
_journal_name_full               Org.Biomol.Chem.

_journal_coden_Cambridge         0177

_publ_contact_author_name        'Dr Animesh Pramanik'
_publ_contact_author_address     
;
Chemistry
University of Calcutta
92, A. P. C. Road, Kolkata-700009
Kolkata
India
Kolkata-700 009
;

_publ_contact_author_email       'ANIMESH IN2001@YAHOO.CO.IN'

_publ_section_title              
;
b-Turn mimic in tripeptide with Phe(1)-Aib(2) as
corner residues and  b-strand structure in an isomeric tripeptide: An
X-ray diffraction study
;
loop_
_publ_author_name
'Animesh Pramanik'
'Anita Dutt'
'Roland Frohlich'

data_fro2721
_database_code_depnum_ccdc_archive 'CCDC 252275'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H39 N3 O6'
_chemical_formula_weight         477.59

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   P21

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

_cell_length_a                   8.889(1)
_cell_length_b                   11.196(1)
_cell_length_c                   13.856(1)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.09(1)
_cell_angle_gamma                90.00
_cell_volume                     1378.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    198(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             516
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      198(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode Nonius FR591'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11001
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_av_sigmaI/netI    0.0541
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.29
_diffrn_reflns_theta_max         27.89
_reflns_number_total             6281
_reflns_number_gt                4504
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinwoski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SCHAKAL (Keller, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR
and
goodness of fit S are based on F^2^, conventional R-factors R are
based
on F, with F set to zero for negative F^2^. The threshold expression
of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc.
and is
not relevant to the choice of reflections for refinement.  R-factors
based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0364P)^2^+0.4032P] where
P=(Fo^2^+2Fc^2^)/3
;
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   "at N's from difmap, other geom"
_refine_ls_hydrogen_treatment    riding
_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   0.0(11)
_refine_ls_number_reflns         6281
_refine_ls_number_parameters     324
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0601
_refine_ls_wR_factor_ref         0.1232
_refine_ls_wR_factor_gt          0.1092
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2649(4) 0.9662(3) 0.3904(2) 0.0533(7) Uani 1 1 d . . .
C2 C 0.3836(4) 0.9890(4) 0.4699(2) 0.0771(11) Uani 1 1 d . . .
H2A H 0.4239 0.9126 0.4938 0.116 Uiso 1 1 calc R . .
H2B H 0.3382 1.0323 0.5230 0.116 Uiso 1 1 calc R . .
H2C H 0.4654 1.0369 0.4443 0.116 Uiso 1 1 calc R . .
C3 C 0.1437(5) 0.8848(4) 0.4245(3) 0.0906(12) Uani 1 1 d . . .
H3A H 0.0673 0.8735 0.3725 0.136 Uiso 1 1 calc R . .
H3B H 0.0970 0.9204 0.4806 0.136 Uiso 1 1 calc R . .
H3C H 0.1878 0.8074 0.4426 0.136 Uiso 1 1 calc R . .
C4 C 0.2033(4) 1.0825(3) 0.3514(2) 0.0669(9) Uani 1 1 d . . .
H4A H 0.2849 1.1290 0.3241 0.100 Uiso 1 1 calc R . .
H4B H 0.1591 1.1279 0.4038 0.100 Uiso 1 1 calc R . .
H4C H 0.1258 1.0664 0.3010 0.100 Uiso 1 1 calc R . .
O5 O 0.3546(2) 0.90772(17) 0.31604(12) 0.0505(5) Uani 1 1 d . . .
C6 C 0.2938(3) 0.8823(2) 0.22766(17) 0.0397(6) Uani 1 1 d . . .
O7 O 0.16034(19) 0.88052(17) 0.20728(12) 0.0468(4) Uani 1 1 d . . .
N8 N 0.4021(2) 0.8579(2) 0.16569(15) 0.0413(5) Uani 1 1 d . . .
H8 H 0.489(3) 0.855(3) 0.185(2) 0.050 Uiso 1 1 d . . .
C9 C 0.3637(3) 0.8326(2) 0.06424(17) 0.0353(5) Uani 1 1 d . . .
H9 H 0.3071 0.9020 0.0356 0.042 Uiso 1 1 calc R . .
C10 C 0.5088(3) 0.8148(3) 0.00982(19) 0.0454(6) Uani 1 1 d . . .
H10A H 0.5734 0.8863 0.0185 0.054 Uiso 1 1 calc R . .
H10B H 0.5645 0.7454 0.0373 0.054 Uiso 1 1 calc R . .
C11 C 0.4767(3) 0.7943(2) -0.09610(19) 0.0422(6) Uani 1 1 d . . .
C12 C 0.4504(4) 0.8896(3) -0.1578(2) 0.0608(8) Uani 1 1 d . . .
H12 H 0.4602 0.9689 -0.1340 0.073 Uiso 1 1 calc R . .
C13 C 0.4095(4) 0.8704(4) -0.2544(2) 0.0791(11) Uani 1 1 d . . .
H13 H 0.3905 0.9366 -0.2960 0.095 Uiso 1 1 calc R . .
C14 C 0.3968(4) 0.7571(4) -0.2895(2) 0.0743(10) Uani 1 1 d . . .
H14 H 0.3680 0.7444 -0.3554 0.089 Uiso 1 1 calc R . .
C15 C 0.4255(4) 0.6608(3) -0.2299(2) 0.0640(9) Uani 1 1 d . . .
H15 H 0.4181 0.5818 -0.2546 0.077 Uiso 1 1 calc R . .
C16 C 0.4652(3) 0.6800(3) -0.1337(2) 0.0503(7) Uani 1 1 d . . .
H16 H 0.4849 0.6134 -0.0926 0.060 Uiso 1 1 calc R . .
C17 C 0.2655(2) 0.7207(2) 0.05499(17) 0.0330(5) Uani 1 1 d . . .
O18 O 0.30481(19) 0.62611(15) 0.09270(13) 0.0461(4) Uani 1 1 d . . .
N19 N 0.1372(2) 0.73471(18) 0.00227(14) 0.0325(4) Uani 1 1 d . . .
H19 H 0.111(3) 0.804(2) -0.0172(18) 0.039 Uiso 1 1 d . . .
C20 C 0.0313(3) 0.6374(2) -0.02085(17) 0.0378(6) Uani 1 1 d . . .
C21 C -0.1034(3) 0.6920(3) -0.0765(2) 0.0528(7) Uani 1 1 d . . .
H21A H -0.1505 0.7524 -0.0363 0.079 Uiso 1 1 calc R . .
H21B H -0.1767 0.6292 -0.0930 0.079 Uiso 1 1 calc R . .
H21C H -0.0693 0.7293 -0.1358 0.079 Uiso 1 1 calc R . .
C22 C 0.1046(3) 0.5405(3) -0.0798(2) 0.0548(8) Uani 1 1 d . . .
H22A H 0.1425 0.5753 -0.1390 0.082 Uiso 1 1 calc R . .
H22B H 0.0301 0.4786 -0.0965 0.082 Uiso 1 1 calc R . .
H22C H 0.1883 0.5050 -0.0418 0.082 Uiso 1 1 calc R . .
C23 C -0.0321(3) 0.5839(2) 0.07160(18) 0.0368(5) Uani 1 1 d . . .
O24 O -0.0858(2) 0.48318(15) 0.07155(13) 0.0505(5) Uani 1 1 d . . .
N25 N -0.0360(2) 0.65671(18) 0.14791(15) 0.0385(5) Uani 1 1 d . . .
H25 H 0.009(3) 0.723(3) 0.1481(19) 0.046 Uiso 1 1 d . . .
C26 C -0.0946(3) 0.6202(2) 0.23932(17) 0.0393(6) Uani 1 1 d . . .
H26 H -0.1491 0.5429 0.2288 0.047 Uiso 1 1 calc R . .
C27 C 0.0314(3) 0.5990(3) 0.3157(2) 0.0522(7) Uani 1 1 d . . .
H27A H 0.0946 0.6717 0.3207 0.063 Uiso 1 1 calc R . .
H27B H -0.0146 0.5871 0.3790 0.063 Uiso 1 1 calc R . .
C28 C 0.1311(5) 0.4940(5) 0.2964(3) 0.0995(16) Uani 1 1 d . . .
H28 H 0.1700 0.5009 0.2298 0.119 Uiso 1 1 calc R . .
C29 C 0.2658(6) 0.5004(7) 0.3715(4) 0.170(3) Uani 1 1 d . . .
H29A H 0.2282 0.4920 0.4368 0.255 Uiso 1 1 calc R . .
H29B H 0.3169 0.5774 0.3658 0.255 Uiso 1 1 calc R . .
H29C H 0.3368 0.4356 0.3592 0.255 Uiso 1 1 calc R . .
C30 C 0.0454(8) 0.3783(4) 0.3047(3) 0.152(3) Uani 1 1 d . . .
H30A H 0.0109 0.3696 0.3707 0.228 Uiso 1 1 calc R . .
H30B H 0.1114 0.3113 0.2896 0.228 Uiso 1 1 calc R . .
H30C H -0.0416 0.3790 0.2593 0.228 Uiso 1 1 calc R . .
C31 C -0.2078(3) 0.7118(2) 0.27037(19) 0.0441(6) Uani 1 1 d . . .
O32 O -0.2658(2) 0.7873(2) 0.22078(14) 0.0648(6) Uani 1 1 d . . .
O33 O -0.2370(3) 0.6993(2) 0.36385(15) 0.0773(8) Uani 1 1 d . . .
C34 C -0.3442(5) 0.7830(4) 0.4012(3) 0.1074(17) Uani 1 1 d . . .
H34A H -0.3175 0.8642 0.3816 0.161 Uiso 1 1 calc R . .
H34B H -0.3424 0.7780 0.4718 0.161 Uiso 1 1 calc R . .
H34C H -0.4453 0.7636 0.3753 0.161 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0661(19) 0.0594(17) 0.0348(15) -0.0071(13) 0.0082(14) 0.0172(14)
C2 0.095(3) 0.097(3) 0.0387(17) -0.0221(17) -0.0059(17) 0.033(2)
C3 0.122(3) 0.092(3) 0.061(2) -0.013(2) 0.045(2) -0.014(2)
C4 0.081(2) 0.0619(19) 0.058(2) -0.0078(15) 0.0014(17) 0.0243(17)
O5 0.0522(11) 0.0702(12) 0.0287(9) -0.0122(8) -0.0046(8) 0.0216(9)
C6 0.0422(15) 0.0446(14) 0.0323(13) -0.0012(11) 0.0006(11) 0.0059(11)
O7 0.0362(10) 0.0627(11) 0.0419(10) -0.0068(8) 0.0041(8) 0.0064(8)
N8 0.0299(11) 0.0614(14) 0.0325(12) -0.0094(10) -0.0022(9) 0.0018(10)
C9 0.0312(12) 0.0458(14) 0.0289(13) -0.0038(10) 0.0004(10) -0.0007(10)
C10 0.0328(13) 0.0622(16) 0.0414(16) -0.0103(12) 0.0055(11) -0.0051(12)
C11 0.0300(13) 0.0538(16) 0.0437(15) -0.0042(12) 0.0124(12) -0.0029(11)
C12 0.077(2) 0.0558(17) 0.0513(19) 0.0008(14) 0.0261(16) 0.0010(15)
C13 0.105(3) 0.091(3) 0.0427(19) 0.0159(18) 0.0244(18) 0.030(2)
C14 0.072(2) 0.113(3) 0.0384(17) -0.0091(19) 0.0066(16) 0.019(2)
C15 0.068(2) 0.075(2) 0.050(2) -0.0192(16) 0.0113(16) 0.0015(17)
C16 0.0511(16) 0.0563(16) 0.0442(17) -0.0019(12) 0.0110(13) 0.0042(12)
C17 0.0312(13) 0.0391(13) 0.0289(12) -0.0014(10) 0.0040(10) 0.0032(10)
O18 0.0445(10) 0.0429(10) 0.0505(11) 0.0088(8) -0.0028(8) 0.0069(8)
N19 0.0290(10) 0.0351(10) 0.0332(11) 0.0025(8) -0.0006(8) -0.0003(8)
C20 0.0301(13) 0.0444(14) 0.0388(14) -0.0023(11) -0.0002(10) -0.0063(10)
C21 0.0410(15) 0.0674(18) 0.0490(17) 0.0124(14) -0.0119(13) -0.0111(13)
C22 0.0543(18) 0.0610(17) 0.0499(18) -0.0196(14) 0.0116(14) -0.0143(14)
C23 0.0352(14) 0.0376(13) 0.0375(14) -0.0004(11) -0.0002(10) -0.0010(10)
O24 0.0628(12) 0.0409(10) 0.0479(11) -0.0035(8) 0.0030(9) -0.0168(9)
N25 0.0436(12) 0.0371(11) 0.0354(11) -0.0018(9) 0.0080(9) -0.0065(9)
C26 0.0427(14) 0.0402(13) 0.0353(13) 0.0027(10) 0.0075(11) -0.0030(11)
C27 0.0503(17) 0.0588(17) 0.0473(17) 0.0062(13) -0.0012(13) 0.0108(13)
C28 0.107(3) 0.144(4) 0.050(2) 0.029(2) 0.023(2) 0.081(3)
C29 0.105(4) 0.277(8) 0.126(5) 0.059(5) -0.007(3) 0.112(5)
C30 0.306(9) 0.069(3) 0.081(3) 0.012(2) 0.029(4) 0.090(4)
C31 0.0397(14) 0.0517(15) 0.0410(15) 0.0087(12) 0.0043(12) 0.0021(12)
O32 0.0574(13) 0.0891(15) 0.0485(12) 0.0223(11) 0.0082(10) 0.0313(11)
O33 0.0946(17) 0.0933(17) 0.0461(13) 0.0224(11) 0.0297(12) 0.0508(13)
C34 0.137(4) 0.124(3) 0.065(2) 0.018(2) 0.042(2) 0.083(3)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O5 1.478(3) . ?
C1 C3 1.500(5) . ?
C1 C4 1.506(4) . ?
C1 C2 1.519(4) . ?
O5 C6 1.351(3) . ?
C6 O7 1.210(3) . ?
C6 N8 1.341(3) . ?
N8 C9 1.462(3) . ?
C9 C17 1.529(3) . ?
C9 C10 1.531(3) . ?
C10 C11 1.502(4) . ?
C11 C12 1.382(4) . ?
C11 C16 1.385(4) . ?
C12 C13 1.391(5) . ?
C13 C14 1.363(5) . ?
C14 C15 1.376(5) . ?
C15 C16 1.383(4) . ?
C17 O18 1.226(3) . ?
C17 N19 1.341(3) . ?
N19 C20 1.467(3) . ?
C20 C22 1.519(4) . ?
C20 C21 1.527(3) . ?
C20 C23 1.539(3) . ?
C23 O24 1.225(3) . ?
C23 N25 1.336(3) . ?
N25 C26 1.446(3) . ?
C26 C31 1.510(3) . ?
C26 C27 1.532(4) . ?
C27 C28 1.502(4) . ?
C28 C30 1.509(8) . ?
C28 C29 1.559(7) . ?
C31 O32 1.194(3) . ?
C31 O33 1.337(3) . ?
O33 C34 1.445(4) . ?

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
O5 C1 C3 111.2(2) . . ?
O5 C1 C4 109.4(2) . . ?
C3 C1 C4 112.5(3) . . ?
O5 C1 C2 101.7(2) . . ?
C3 C1 C2 111.2(3) . . ?
C4 C1 C2 110.4(3) . . ?
C6 O5 C1 121.2(2) . . ?
O7 C6 N8 124.6(2) . . ?
O7 C6 O5 124.9(2) . . ?
N8 C6 O5 110.5(2) . . ?
C6 N8 C9 120.5(2) . . ?
N8 C9 C17 110.6(2) . . ?
N8 C9 C10 109.11(19) . . ?
C17 C9 C10 109.93(19) . . ?
C11 C10 C9 111.6(2) . . ?
C12 C11 C16 118.2(3) . . ?
C12 C11 C10 120.6(2) . . ?
C16 C11 C10 121.1(2) . . ?
C11 C12 C13 120.6(3) . . ?
C14 C13 C12 120.2(3) . . ?
C13 C14 C15 120.2(3) . . ?
C14 C15 C16 119.5(3) . . ?
C15 C16 C11 121.2(3) . . ?
O18 C17 N19 123.8(2) . . ?
O18 C17 C9 121.3(2) . . ?
N19 C17 C9 114.9(2) . . ?
C17 N19 C20 124.0(2) . . ?
N19 C20 C22 111.30(19) . . ?
N19 C20 C21 107.4(2) . . ?
C22 C20 C21 111.0(2) . . ?
N19 C20 C23 111.01(19) . . ?
C22 C20 C23 110.3(2) . . ?
C21 C20 C23 105.77(19) . . ?
O24 C23 N25 122.7(2) . . ?
O24 C23 C20 120.8(2) . . ?
N25 C23 C20 116.2(2) . . ?
C23 N25 C26 122.8(2) . . ?
N25 C26 C31 108.8(2) . . ?
N25 C26 C27 111.9(2) . . ?
C31 C26 C27 112.8(2) . . ?
C28 C27 C26 114.8(3) . . ?
C27 C28 C30 110.8(4) . . ?
C27 C28 C29 106.8(4) . . ?
C30 C28 C29 111.4(4) . . ?
O32 C31 O33 122.4(2) . . ?
O32 C31 C26 126.5(2) . . ?
O33 C31 C26 111.1(2) . . ?
C31 O33 C34 115.6(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
C3 C1 O5 C6 68.1(3) . . . . ?
C4 C1 O5 C6 -56.7(3) . . . . ?
C2 C1 O5 C6 -173.5(3) . . . . ?
C1 O5 C6 O7 -16.1(4) . . . . ?
C1 O5 C6 N8 164.6(2) . . . . ?
O7 C6 N8 C9 3.2(4) . . . . ?
O5 C6 N8 C9 -177.4(2) . . . . ?
C6 N8 C9 C17 -62.0(3) . . . . ?
C6 N8 C9 C10 177.0(2) . . . . ?
N8 C9 C10 C11 -177.2(2) . . . . ?
C17 C9 C10 C11 61.3(3) . . . . ?
C9 C10 C11 C12 82.2(3) . . . . ?
C9 C10 C11 C16 -94.6(3) . . . . ?
C16 C11 C12 C13 1.7(4) . . . . ?
C10 C11 C12 C13 -175.1(3) . . . . ?
C11 C12 C13 C14 -0.8(5) . . . . ?
C12 C13 C14 C15 -0.6(6) . . . . ?
C13 C14 C15 C16 1.0(5) . . . . ?
C14 C15 C16 C11 0.0(4) . . . . ?
C12 C11 C16 C15 -1.3(4) . . . . ?
C10 C11 C16 C15 175.5(2) . . . . ?
N8 C9 C17 O18 -53.3(3) . . . . ?
C10 C9 C17 O18 67.2(3) . . . . ?
N8 C9 C17 N19 127.5(2) . . . . ?
C10 C9 C17 N19 -111.9(2) . . . . ?
O18 C17 N19 C20 -3.1(4) . . . . ?
C9 C17 N19 C20 176.0(2) . . . . ?
C17 N19 C20 C22 -61.7(3) . . . . ?
C17 N19 C20 C21 176.7(2) . . . . ?
C17 N19 C20 C23 61.5(3) . . . . ?
N19 C20 C23 O24 -158.7(2) . . . . ?
C22 C20 C23 O24 -34.9(3) . . . . ?
C21 C20 C23 O24 85.2(3) . . . . ?
N19 C20 C23 N25 26.6(3) . . . . ?
C22 C20 C23 N25 150.4(2) . . . . ?
C21 C20 C23 N25 -89.5(3) . . . . ?
O24 C23 N25 C26 4.4(4) . . . . ?
C20 C23 N25 C26 179.0(2) . . . . ?
C23 N25 C26 C31 -129.0(2) . . . . ?
C23 N25 C26 C27 105.7(3) . . . . ?
N25 C26 C27 C28 -67.3(3) . . . . ?
C31 C26 C27 C28 169.6(3) . . . . ?
C26 C27 C28 C30 -67.8(4) . . . . ?
C26 C27 C28 C29 170.7(3) . . . . ?
N25 C26 C31 O32 15.2(4) . . . . ?
C27 C26 C31 O32 139.9(3) . . . . ?
N25 C26 C31 O33 -164.4(2) . . . . ?
C27 C26 C31 O33 -39.6(3) . . . . ?
O32 C31 O33 C34 0.3(5) . . . . ?
C26 C31 O33 C34 179.9(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.89
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.039

data_fro2712
_database_code_depnum_ccdc_archive 'CCDC 255975'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C76 H123 N9 O20'
_chemical_formula_weight         1482.84

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   C2

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

_cell_length_a                   47.011(1)
_cell_length_b                   13.325(1)
_cell_length_c                   14.106(1)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.26(1)
_cell_angle_gamma                90.00
_cell_volume                     8799.1(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    198(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3208
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      198(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode Nonius FR591'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            35335
_diffrn_reflns_av_R_equivalents  0.045
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_min       -60
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.01
_diffrn_reflns_theta_max         27.48
_reflns_number_total             18476
_reflns_number_gt                12183
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SCHAKAL (Keller, 1997)'
_computing_publication_material  'SHELXL (Sheldrick, 1997)'

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

Hydrogen atoms at water O101 not found, methanol refined with split
positions (PART command) and isotropic thermal parameters.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
calc w=1/[\s^2^(Fo^2^)+(0.0876P)^2^+5.4884P] where
P=(Fo^2^+2Fc^2^)/3
;
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   "at N's from difmap, other geom"
_refine_ls_hydrogen_treatment    riding
_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   0.5(9)
_refine_ls_number_reflns         18476
_refine_ls_number_parameters     976
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1121
_refine_ls_R_factor_gt           0.0665
_refine_ls_wR_factor_ref         0.1804
_refine_ls_wR_factor_gt          0.1548
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.021
_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
C1A C 0.07413(8) 0.3104(3) 0.3887(3) 0.0620(10) Uani 1 1 d . . .
C2A C 0.04786(9) 0.3300(4) 0.4401(3) 0.0687(11) Uani 1 1 d . . .
H2AA H 0.0310 0.3323 0.3939 0.103 Uiso 1 1 calc R . .
H2AB H 0.0499 0.3944 0.4736 0.103 Uiso 1 1 calc R . .
H2AC H 0.0456 0.2762 0.4862 0.103 Uiso 1 1 calc R . .
C3A C 0.08146(12) 0.4011(5) 0.3341(4) 0.107(2) Uani 1 1 d . . .
H3AA H 0.1010 0.3949 0.3160 0.160 Uiso 1 1 calc R . .
H3AB H 0.0800 0.4609 0.3738 0.160 Uiso 1 1 calc R . .
H3AC H 0.0682 0.4071 0.2767 0.160 Uiso 1 1 calc R . .
C4A C 0.07126(13) 0.2184(4) 0.3279(3) 0.1034(19) Uani 1 1 d . . .
H4AA H 0.0687 0.1596 0.3680 0.155 Uiso 1 1 calc R . .
H4AB H 0.0885 0.2099 0.2948 0.155 Uiso 1 1 calc R . .
H4AC H 0.0547 0.2254 0.2810 0.155 Uiso 1 1 calc R . .
O5A O 0.09931(5) 0.30068(19) 0.45998(17) 0.0578(6) Uani 1 1 d . . .
C6A C 0.10143(7) 0.2262(2) 0.5243(2) 0.0422(7) Uani 1 1 d . . .
O7A O 0.08360(5) 0.16150(18) 0.53186(18) 0.0564(6) Uani 1 1 d . . .
N8A N 0.12544(6) 0.2346(2) 0.5801(2) 0.0432(7) Uani 1 1 d . . .
H8A H 0.1354(9) 0.264(3) 0.569(3) 0.052 Uiso 1 1 d . . .
C9A C 0.13379(7) 0.1624(2) 0.6552(2) 0.0370(7) Uani 1 1 d . . .
H9A H 0.1232 0.0980 0.6415 0.044 Uiso 1 1 calc R . .
C10A C 0.16590(7) 0.1422(2) 0.6607(2) 0.0431(7) Uani 1 1 d . . .
H10A H 0.1763 0.2068 0.6692 0.052 Uiso 1 1 calc R . .
H10B H 0.1714 0.1000 0.7171 0.052 Uiso 1 1 calc R . .
C11A C 0.17482(7) 0.0900(3) 0.5724(2) 0.0459(8) Uani 1 1 d . . .
C12A C 0.18616(10) 0.1448(3) 0.5013(3) 0.0736(12) Uani 1 1 d . . .
H12A H 0.1888 0.2152 0.5085 0.088 Uiso 1 1 calc R . .
C13A C 0.19366(13) 0.0974(4) 0.4196(4) 0.0906(16) Uani 1 1 d . . .
H13A H 0.2011 0.1353 0.3704 0.109 Uiso 1 1 calc R . .
C14A C 0.19039(11) -0.0029(4) 0.4105(3) 0.0845(14) Uani 1 1 d . . .
H14A H 0.1959 -0.0352 0.3549 0.101 Uiso 1 1 calc R . .
C15A C 0.17935(9) -0.0590(3) 0.4796(3) 0.0707(12) Uani 1 1 d . . .
H15A H 0.1770 -0.1294 0.4721 0.085 Uiso 1 1 calc R . .
C16A C 0.17162(8) -0.0116(3) 0.5608(3) 0.0567(9) Uani 1 1 d . . .
H16A H 0.1640 -0.0502 0.6092 0.068 Uiso 1 1 calc R . .
C17A C 0.12623(7) 0.2038(2) 0.7514(2) 0.0378(7) Uani 1 1 d . . .
O18A O 0.13691(5) 0.28223(16) 0.78418(16) 0.0509(6) Uani 1 1 d . . .
N19A N 0.10752(6) 0.1519(2) 0.79533(19) 0.0445(7) Uani 1 1 d . . .
H19A H 0.1014(8) 0.096(3) 0.779(3) 0.053 Uiso 1 1 d . . .
C20A C 0.09990(7) 0.1834(2) 0.8894(2) 0.0443(8) Uani 1 1 d . . .
H20A H 0.0930 0.2543 0.8860 0.053 Uiso 1 1 calc R . .
C21A C 0.07627(7) 0.1152(3) 0.9200(2) 0.0476(8) Uani 1 1 d . . .
H21A H 0.0831 0.0450 0.9207 0.057 Uiso 1 1 calc R . .
H21B H 0.0596 0.1197 0.8719 0.057 Uiso 1 1 calc R . .
C22A C 0.06641(8) 0.1399(3) 1.0177(3) 0.0582(9) Uani 1 1 d . . .
H22A H 0.0837 0.1402 1.0648 0.070 Uiso 1 1 calc R . .
C23A C 0.04657(13) 0.0552(5) 1.0459(4) 0.109(2) Uani 1 1 d . . .
H23A H 0.0419 0.0655 1.1115 0.163 Uiso 1 1 calc R . .
H23B H 0.0562 -0.0096 1.0410 0.163 Uiso 1 1 calc R . .
H23C H 0.0289 0.0557 1.0030 0.163 Uiso 1 1 calc R . .
C24A C 0.05263(12) 0.2411(4) 1.0204(4) 0.0878(15) Uani 1 1 d . . .
H24A H 0.0351 0.2417 0.9773 0.132 Uiso 1 1 calc R . .
H24B H 0.0658 0.2923 1.0002 0.132 Uiso 1 1 calc R . .
H24C H 0.0480 0.2555 1.0854 0.132 Uiso 1 1 calc R . .
C25A C 0.12563(7) 0.1765(3) 0.9580(2) 0.0463(8) Uani 1 1 d . . .
O26A O 0.13953(5) 0.0980(2) 0.96737(17) 0.0592(6) Uani 1 1 d . . .
N27A N 0.13185(7) 0.2576(2) 1.0123(2) 0.0532(7) Uani 1 1 d . . .
H27A H 0.1210(8) 0.326(3) 0.993(3) 0.064 Uiso 1 1 d . . .
C28A C 0.15689(9) 0.2601(3) 1.0814(3) 0.0702(11) Uani 1 1 d . . .
C29A C 0.18412(11) 0.2707(5) 1.0302(4) 0.1068(19) Uani 1 1 d . . .
H29A H 0.2008 0.2550 1.0746 0.160 Uiso 1 1 calc R . .
H29B H 0.1856 0.3396 1.0071 0.160 Uiso 1 1 calc R . .
H29C H 0.1833 0.2241 0.9762 0.160 Uiso 1 1 calc R . .
C30A C 0.15297(13) 0.3518(5) 1.1460(4) 0.1076(19) Uani 1 1 d . . .
H30A H 0.1349 0.3457 1.1748 0.161 Uiso 1 1 calc R . .
H30B H 0.1528 0.4133 1.1078 0.161 Uiso 1 1 calc R . .
H30C H 0.1688 0.3547 1.1963 0.161 Uiso 1 1 calc R . .
C31A C 0.15800(10) 0.1668(4) 1.1442(3) 0.0739(12) Uani 1 1 d . . .
O32A O 0.17941(8) 0.1229(3) 1.1700(3) 0.1094(13) Uani 1 1 d . . .
O33A O 0.13226(7) 0.1451(3) 1.1716(2) 0.0832(9) Uani 1 1 d . . .
C34A C 0.13022(15) 0.0586(5) 1.2305(5) 0.122(2) Uani 1 1 d . . .
H34A H 0.1346 -0.0017 1.1947 0.183 Uiso 1 1 calc R . .
H34B H 0.1108 0.0535 1.2501 0.183 Uiso 1 1 calc R . .
H34C H 0.1439 0.0646 1.2870 0.183 Uiso 1 1 calc R . .
C1B C 0.07112(10) 0.6151(3) 1.0545(3) 0.0658(11) Uani 1 1 d . . .
C2B C 0.06157(13) 0.7228(3) 1.0698(3) 0.0864(15) Uani 1 1 d . . .
H2BA H 0.0782 0.7674 1.0728 0.130 Uiso 1 1 calc R . .
H2BB H 0.0526 0.7271 1.1297 0.130 Uiso 1 1 calc R . .
H2BC H 0.0478 0.7431 1.0169 0.130 Uiso 1 1 calc R . .
C3B C 0.04728(14) 0.5424(5) 1.0586(5) 0.123(3) Uani 1 1 d . . .
H3BA H 0.0326 0.5560 1.0063 0.185 Uiso 1 1 calc R . .
H3BB H 0.0390 0.5494 1.1196 0.185 Uiso 1 1 calc R . .
H3BC H 0.0545 0.4740 1.0526 0.185 Uiso 1 1 calc R . .
C4B C 0.09702(15) 0.5905(5) 1.1239(3) 0.1055(19) Uani 1 1 d . . .
H4BA H 0.1054 0.5269 1.1056 0.158 Uiso 1 1 calc R . .
H4BB H 0.0910 0.5847 1.1885 0.158 Uiso 1 1 calc R . .
H4BC H 0.1112 0.6443 1.1223 0.158 Uiso 1 1 calc R . .
O5B O 0.07930(6) 0.61960(17) 0.95636(16) 0.0544(6) Uani 1 1 d . . .
C6B C 0.09033(7) 0.5400(3) 0.9146(2) 0.0450(8) Uani 1 1 d . . .
O7B O 0.09824(6) 0.46204(19) 0.95249(17) 0.0572(6) Uani 1 1 d . . .
N8B N 0.09186(6) 0.5630(2) 0.82120(19) 0.0426(6) Uani 1 1 d . . .
H8B H 0.0833(8) 0.616(3) 0.796(3) 0.051 Uiso 1 1 d . . .
C9B C 0.10190(6) 0.4908(2) 0.7549(2) 0.0377(7) Uani 1 1 d . . .
H9B H 0.1069 0.4273 0.7905 0.045 Uiso 1 1 calc R . .
C10B C 0.07904(7) 0.4667(2) 0.6743(2) 0.0404(7) Uani 1 1 d . . .
H10C H 0.0725 0.5298 0.6422 0.049 Uiso 1 1 calc R . .
H10D H 0.0874 0.4237 0.6268 0.049 Uiso 1 1 calc R . .
C11B C 0.05363(7) 0.4135(2) 0.7101(2) 0.0410(7) Uani 1 1 d . . .
C12B C 0.05084(7) 0.3103(3) 0.7035(2) 0.0471(8) Uani 1 1 d . . .
H12B H 0.0648 0.2727 0.6740 0.057 Uiso 1 1 calc R . .
C13B C 0.02833(8) 0.2610(3) 0.7385(3) 0.0590(10) Uani 1 1 d . . .
H13B H 0.0267 0.1902 0.7327 0.071 Uiso 1 1 calc R . .
C14B C 0.00824(8) 0.3149(4) 0.7821(3) 0.0664(11) Uani 1 1 d . . .
H14B H -0.0071 0.2810 0.8078 0.080 Uiso 1 1 calc R . .
C15B C 0.01028(8) 0.4182(4) 0.7885(3) 0.0667(11) Uani 1 1 d . . .
H15B H -0.0038 0.4552 0.8181 0.080 Uiso 1 1 calc R . .
C16B C 0.03282(7) 0.4679(3) 0.7520(3) 0.0530(8) Uani 1 1 d . . .
H16B H 0.0340 0.5390 0.7555 0.064 Uiso 1 1 calc R . .
C17B C 0.12915(7) 0.5319(2) 0.7166(2) 0.0384(7) Uani 1 1 d . . .
O18B O 0.12987(5) 0.61693(17) 0.68144(17) 0.0513(6) Uani 1 1 d . . .
N19B N 0.15113(6) 0.4696(2) 0.72373(19) 0.0429(6) Uani 1 1 d . . .
H19B H 0.1493(8) 0.403(3) 0.745(3) 0.051 Uiso 1 1 d . . .
C20B C 0.17864(7) 0.4958(2) 0.6908(2) 0.0446(7) Uani 1 1 d . . .
H20B H 0.1823 0.5691 0.7008 0.054 Uiso 1 1 calc R . .
C21B C 0.20213(8) 0.4344(3) 0.7488(3) 0.0646(10) Uani 1 1 d . . .
H21C H 0.1998 0.4433 0.8173 0.077 Uiso 1 1 calc R . .
H21D H 0.1990 0.3624 0.7337 0.077 Uiso 1 1 calc R . .
C22B C 0.23245(10) 0.4610(6) 0.7319(4) 0.105(2) Uani 1 1 d . . .
H22B H 0.2339 0.4604 0.6616 0.126 Uiso 1 1 calc R . .
C23B C 0.25289(13) 0.3838(9) 0.7758(6) 0.181(5) Uani 1 1 d . . .
H23D H 0.2568 0.3339 0.7277 0.272 Uiso 1 1 calc R . .
H23E H 0.2444 0.3506 0.8285 0.272 Uiso 1 1 calc R . .
H23F H 0.2708 0.4166 0.7999 0.272 Uiso 1 1 calc R . .
C24B C 0.24017(16) 0.5710(8) 0.7697(7) 0.179(4) Uani 1 1 d . . .
H24D H 0.2250 0.6175 0.7463 0.269 Uiso 1 1 calc R . .
H24E H 0.2583 0.5922 0.7466 0.269 Uiso 1 1 calc R . .
H24F H 0.2420 0.5709 0.8395 0.269 Uiso 1 1 calc R . .
C25B C 0.17886(7) 0.4709(3) 0.5867(2) 0.0457(8) Uani 1 1 d . . .
O26B O 0.17167(6) 0.38768(19) 0.5562(2) 0.0623(7) Uani 1 1 d . . .
N27B N 0.18842(7) 0.5432(2) 0.5326(2) 0.0557(7) Uani 1 1 d . . .
H27B H 0.1891(9) 0.609(3) 0.555(3) 0.067 Uiso 1 1 d . . .
C28B C 0.19081(10) 0.5311(3) 0.4300(3) 0.0664(11) Uani 1 1 d . . .
C29B C 0.16191(13) 0.5257(5) 0.3753(4) 0.1062(19) Uani 1 1 d . . .
H29D H 0.1642 0.5203 0.3071 0.159 Uiso 1 1 calc R . .
H29E H 0.1511 0.5865 0.3872 0.159 Uiso 1 1 calc R . .
H29F H 0.1516 0.4668 0.3960 0.159 Uiso 1 1 calc R . .
C30B C 0.20897(16) 0.6200(4) 0.3997(4) 0.110(2) Uani 1 1 d . . .
H30D H 0.2284 0.6142 0.4308 0.164 Uiso 1 1 calc R . .
H30E H 0.2005 0.6831 0.4187 0.164 Uiso 1 1 calc R . .
H30F H 0.2096 0.6190 0.3305 0.164 Uiso 1 1 calc R . .
C31B C 0.20759(9) 0.4358(3) 0.4128(3) 0.0626(10) Uani 1 1 d . . .
O32B O 0.20239(7) 0.3828(3) 0.3443(2) 0.0916(10) Uani 1 1 d . . .
O33B O 0.22943(6) 0.4226(2) 0.4757(2) 0.0731(8) Uani 1 1 d . . .
C34B C 0.24766(11) 0.3359(4) 0.4632(5) 0.1006(17) Uani 1 1 d . . .
H34D H 0.2365 0.2742 0.4677 0.151 Uiso 1 1 calc R . .
H34E H 0.2637 0.3361 0.5129 0.151 Uiso 1 1 calc R . .
H34F H 0.2550 0.3393 0.4005 0.151 Uiso 1 1 calc R . .
C1C C 0.22857(8) -0.0088(4) 0.8686(4) 0.0795(13) Uani 1 1 d . . .
C2C C 0.23902(12) -0.0016(6) 0.7725(5) 0.133(3) Uani 1 1 d . . .
H2CA H 0.2599 -0.0087 0.7780 0.200 Uiso 1 1 calc R . .
H2CB H 0.2337 0.0638 0.7444 0.200 Uiso 1 1 calc R . .
H2CC H 0.2304 -0.0551 0.7318 0.200 Uiso 1 1 calc R . .
C3C C 0.23551(11) 0.0874(5) 0.9269(5) 0.121(2) Uani 1 1 d . . .
H3CA H 0.2248 0.0873 0.9833 0.181 Uiso 1 1 calc R . .
H3CB H 0.2301 0.1463 0.8877 0.181 Uiso 1 1 calc R . .
H3CC H 0.2560 0.0896 0.9469 0.181 Uiso 1 1 calc R . .
C4C C 0.23881(13) -0.1007(6) 0.9233(6) 0.145(3) Uani 1 1 d . . .
H4CA H 0.2303 -0.1026 0.9841 0.218 Uiso 1 1 calc R . .
H4CB H 0.2597 -0.0986 0.9353 0.218 Uiso 1 1 calc R . .
H4CC H 0.2332 -0.1608 0.8862 0.218 Uiso 1 1 calc R . .
O5C O 0.19747(5) -0.00789(19) 0.86071(17) 0.0563(6) Uani 1 1 d . . .
C6C C 0.18243(7) -0.0858(3) 0.8207(2) 0.0485(8) Uani 1 1 d . . .
O7C O 0.19228(5) -0.1553(2) 0.7803(2) 0.0680(7) Uani 1 1 d . . .
N8C N 0.15446(6) -0.0711(2) 0.8303(2) 0.0441(7) Uani 1 1 d . . .
H8C H 0.1500(9) -0.036(3) 0.860(3) 0.053 Uiso 1 1 d . . .
C9C C 0.13445(7) -0.1533(2) 0.8135(2) 0.0419(7) Uani 1 1 d . . .
H9C H 0.1448 -0.2122 0.7894 0.050 Uiso 1 1 calc R . .
C10C C 0.12176(7) -0.1837(3) 0.9051(3) 0.0529(8) Uani 1 1 d . . .
H10E H 0.1119 -0.1252 0.9304 0.063 Uiso 1 1 calc R . .
H10F H 0.1073 -0.2370 0.8905 0.063 Uiso 1 1 calc R . .
C11C C 0.14392(8) -0.2210(4) 0.9794(3) 0.0646(11) Uani 1 1 d . . .
C12C C 0.15390(12) -0.1613(5) 1.0536(4) 0.1018(17) Uani 1 1 d . . .
H12C H 0.1463 -0.0956 1.0583 0.122 Uiso 1 1 calc R . .
C13C C 0.17468(17) -0.1935(9) 1.1216(5) 0.153(3) Uani 1 1 d . . .
H13C H 0.1813 -0.1502 1.1723 0.183 Uiso 1 1 calc R . .
C14C C 0.18575(16) -0.2869(9) 1.1164(5) 0.138(3) Uani 1 1 d . . .
H14C H 0.1997 -0.3093 1.1648 0.166 Uiso 1 1 calc R . .
C15C C 0.17687(12) -0.3519(6) 1.0395(6) 0.132(3) Uani 1 1 d . . .
H15C H 0.1850 -0.4166 1.0338 0.158 Uiso 1 1 calc R . .
C16C C 0.15533(10) -0.3158(4) 0.9720(4) 0.0879(15) Uani 1 1 d . . .
H16C H 0.1485 -0.3576 0.9203 0.105 Uiso 1 1 calc R . .
C17C C 0.11009(7) -0.1251(2) 0.7396(2) 0.0402(7) Uani 1 1 d . . .
O18C O 0.09705(6) -0.04538(17) 0.74531(19) 0.0601(7) Uani 1 1 d . . .
N19C N 0.10279(5) -0.1924(2) 0.67232(18) 0.0381(6) Uani 1 1 d . . .
H19C H 0.1100(8) -0.249(3) 0.674(2) 0.046 Uiso 1 1 d . . .
C20C C 0.07671(6) -0.1792(2) 0.6098(2) 0.0398(7) Uani 1 1 d . . .
H20C H 0.0741 -0.1062 0.5948 0.048 Uiso 1 1 calc R . .
C21C C 0.07836(7) -0.2370(3) 0.5171(2) 0.0467(8) Uani 1 1 d . . .
H21E H 0.0598 -0.2306 0.4782 0.056 Uiso 1 1 calc R . .
H21F H 0.0813 -0.3089 0.5324 0.056 Uiso 1 1 calc R . .
C22C C 0.10219(8) -0.2016(3) 0.4578(2) 0.0543(9) Uani 1 1 d . . .
H22C H 0.1210 -0.2145 0.4950 0.065 Uiso 1 1 calc R . .
C23C C 0.10022(10) -0.0916(3) 0.4350(3) 0.0764(12) Uani 1 1 d . . .
H23G H 0.1160 -0.0725 0.3979 0.115 Uiso 1 1 calc R . .
H23H H 0.1014 -0.0529 0.4943 0.115 Uiso 1 1 calc R . .
H23I H 0.0820 -0.0776 0.3979 0.115 Uiso 1 1 calc R . .
C24C C 0.10100(11) -0.2633(4) 0.3666(3) 0.0840(14) Uani 1 1 d . . .
H24G H 0.1043 -0.3342 0.3826 0.126 Uiso 1 1 calc R . .
H24H H 0.1157 -0.2397 0.3271 0.126 Uiso 1 1 calc R . .
H24I H 0.0821 -0.2558 0.3314 0.126 Uiso 1 1 calc R . .
C25C C 0.05176(7) -0.2152(3) 0.6632(2) 0.0447(8) Uani 1 1 d . . .
O26C O 0.05234(5) -0.29630(19) 0.70333(19) 0.0584(6) Uani 1 1 d . . .
N27C N 0.02986(6) -0.1524(2) 0.6630(2) 0.0503(7) Uani 1 1 d . . .
H27C H 0.0319(8) -0.094(3) 0.641(3) 0.060 Uiso 1 1 d . . .
C28C C 0.00625(8) -0.1703(3) 0.7232(3) 0.0598(10) Uani 1 1 d . . .
C29C C -0.01761(9) -0.0927(3) 0.6912(4) 0.0842(14) Uani 1 1 d . . .
H29G H -0.0108 -0.0248 0.7073 0.126 Uiso 1 1 calc R . .
H29H H -0.0347 -0.1070 0.7238 0.126 Uiso 1 1 calc R . .
H29I H -0.0223 -0.0978 0.6222 0.126 Uiso 1 1 calc R . .
C30C C 0.01692(12) -0.1567(5) 0.8269(4) 0.0950(16) Uani 1 1 d . . .
H30G H 0.0302 -0.2112 0.8467 0.143 Uiso 1 1 calc R . .
H30H H 0.0007 -0.1581 0.8658 0.143 Uiso 1 1 calc R . .
H30I H 0.0268 -0.0922 0.8353 0.143 Uiso 1 1 calc R . .
C31C C -0.00618(8) -0.2745(3) 0.7045(3) 0.0578(9) Uani 1 1 d . . .
O32C O -0.01380(7) -0.3275(2) 0.7666(2) 0.0877(10) Uani 1 1 d . . .
O33C O -0.00971(5) -0.29725(18) 0.6138(2) 0.0624(7) Uani 1 1 d . . .
C34C C -0.02275(10) -0.3928(3) 0.5890(4) 0.0823(14) Uani 1 1 d . . .
H34G H -0.0100 -0.4471 0.6131 0.124 Uiso 1 1 calc R . .
H34H H -0.0262 -0.3981 0.5195 0.124 Uiso 1 1 calc R . .
H34I H -0.0410 -0.3983 0.6173 0.124 Uiso 1 1 calc R . .
O101 O 0.17616(8) 0.7349(2) 0.6110(2) 0.0893(10) Uani 1 1 d . . .
O201 O 0.04946(14) 0.0477(4) 0.6474(5) 0.070(2) Uiso 0.499(10) 1 d PD A 1
H201 H 0.0623 0.0917 0.6485 0.105 Uiso 0.499(10) 1 calc PR A 1
C202 C 0.0346(3) 0.0412(9) 0.5504(9) 0.079(4) Uiso 0.499(10) 1 d PD A 1
H20D H 0.0141 0.0530 0.5534 0.119 Uiso 0.499(10) 1 calc PR A 1
H20E H 0.0375 -0.0257 0.5241 0.119 Uiso 0.499(10) 1 calc PR A 1
H20F H 0.0423 0.0920 0.5096 0.119 Uiso 0.499(10) 1 calc PR A 1
O203 O 0.0376(3) 0.0523(11) 0.5905(11) 0.150(5) Uiso 0.501(10) 1 d PD A 2
H203 H 0.0533 0.0595 0.5677 0.225 Uiso 0.501(10) 1 calc PR A 2
C204 C 0.0120(2) 0.0901(8) 0.5136(9) 0.096(4) Uiso 0.501(10) 1 d PD A 2
H20G H -0.0045 0.1098 0.5470 0.144 Uiso 0.501(10) 1 calc PR A 2
H20H H 0.0065 0.0356 0.4691 0.144 Uiso 0.501(10) 1 calc PR A 2
H20I H 0.0185 0.1478 0.4784 0.144 Uiso 0.501(10) 1 calc PR A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1A 0.059(2) 0.083(3) 0.041(2) 0.0081(18) -0.0127(17) 0.0195(19)
C2A 0.057(2) 0.090(3) 0.056(2) 0.001(2) -0.0103(19) 0.020(2)
C3A 0.089(4) 0.148(5) 0.080(3) 0.066(3) -0.012(3) 0.015(3)
C4A 0.121(5) 0.129(4) 0.054(3) -0.024(3) -0.027(3) 0.052(4)
O5A 0.0513(15) 0.0689(16) 0.0511(14) 0.0206(12) -0.0065(11) 0.0042(12)
C6A 0.0435(19) 0.0434(18) 0.0396(17) 0.0014(13) 0.0040(15) 0.0070(15)
O7A 0.0509(15) 0.0547(15) 0.0612(15) 0.0024(11) -0.0083(12) -0.0036(12)
N8A 0.0425(18) 0.0484(17) 0.0384(15) 0.0115(12) 0.0023(13) -0.0032(12)
C9A 0.0433(18) 0.0378(16) 0.0294(15) 0.0012(11) 0.0010(13) 0.0051(12)
C10A 0.0445(19) 0.0467(18) 0.0376(17) 0.0020(13) 0.0003(14) 0.0100(13)
C11A 0.0381(18) 0.061(2) 0.0383(18) -0.0029(14) 0.0005(14) 0.0106(14)
C12A 0.095(3) 0.071(3) 0.060(2) -0.002(2) 0.032(2) -0.004(2)
C13A 0.122(4) 0.084(4) 0.074(3) -0.007(2) 0.054(3) -0.006(3)
C14A 0.090(3) 0.107(4) 0.060(3) -0.020(3) 0.028(3) 0.013(3)
C15A 0.066(3) 0.068(3) 0.077(3) -0.017(2) 0.005(2) 0.016(2)
C16A 0.056(2) 0.055(2) 0.060(2) -0.0002(17) 0.0112(18) 0.0103(16)
C17A 0.0413(18) 0.0350(18) 0.0375(16) 0.0051(12) 0.0058(14) 0.0078(13)
O18A 0.0677(16) 0.0402(13) 0.0472(13) -0.0019(10) 0.0180(12) -0.0108(11)
N19A 0.0562(18) 0.0374(15) 0.0418(15) -0.0051(12) 0.0142(13) -0.0039(12)
C20A 0.053(2) 0.0423(18) 0.0398(18) -0.0026(13) 0.0148(15) -0.0034(14)
C21A 0.0462(19) 0.0517(19) 0.0462(19) 0.0028(15) 0.0102(15) -0.0024(15)
C22A 0.050(2) 0.079(3) 0.048(2) 0.0046(17) 0.0141(17) -0.0079(18)
C23A 0.107(4) 0.129(5) 0.100(4) -0.003(3) 0.059(3) -0.047(4)
C24A 0.091(3) 0.107(4) 0.070(3) -0.008(3) 0.034(3) 0.024(3)
C25A 0.047(2) 0.056(2) 0.0387(18) -0.0056(15) 0.0157(15) -0.0037(16)
O26A 0.0517(15) 0.0774(18) 0.0473(14) -0.0043(12) -0.0014(12) 0.0049(13)
N27A 0.0569(19) 0.0590(19) 0.0437(16) -0.0084(13) 0.0048(14) -0.0093(14)
C28A 0.060(3) 0.093(3) 0.056(2) -0.019(2) -0.006(2) -0.004(2)
C29A 0.065(3) 0.155(5) 0.100(4) -0.015(4) 0.006(3) -0.030(3)
C30A 0.111(4) 0.113(4) 0.092(4) -0.043(3) -0.028(3) 0.002(3)
C31A 0.066(3) 0.109(3) 0.043(2) -0.014(2) -0.012(2) 0.022(3)
O32A 0.086(2) 0.161(4) 0.077(2) 0.000(2) -0.0122(19) 0.046(2)
O33A 0.086(2) 0.109(2) 0.0564(17) 0.0162(16) 0.0111(16) 0.0219(18)
C34A 0.138(5) 0.122(5) 0.110(5) 0.053(4) 0.029(4) 0.043(4)
C1B 0.090(3) 0.065(2) 0.049(2) -0.0083(18) 0.039(2) -0.011(2)
C2B 0.132(4) 0.071(3) 0.064(3) -0.019(2) 0.053(3) 0.003(3)
C3B 0.144(5) 0.112(4) 0.131(5) -0.045(4) 0.104(5) -0.056(4)
C4B 0.153(6) 0.118(4) 0.047(3) -0.010(3) 0.019(3) 0.012(4)
O5B 0.0681(16) 0.0556(14) 0.0433(13) -0.0084(10) 0.0260(12) -0.0059(11)
C6B 0.0440(18) 0.055(2) 0.0375(18) -0.0109(16) 0.0134(14) -0.0093(15)
O7B 0.0766(18) 0.0550(16) 0.0418(13) 0.0003(11) 0.0149(12) -0.0010(12)
N8B 0.0401(15) 0.0506(17) 0.0378(15) -0.0030(12) 0.0075(12) 0.0018(12)
C9B 0.0369(16) 0.0414(17) 0.0356(16) -0.0016(12) 0.0077(13) -0.0011(12)
C10B 0.0422(18) 0.0452(18) 0.0349(16) -0.0052(13) 0.0093(13) -0.0010(13)
C11B 0.0371(17) 0.053(2) 0.0314(16) -0.0010(13) -0.0018(13) -0.0024(13)
C12B 0.0425(19) 0.049(2) 0.0483(19) -0.0010(15) -0.0025(15) -0.0007(14)
C13B 0.052(2) 0.064(2) 0.058(2) 0.0087(17) -0.0102(19) -0.0098(18)
C14B 0.040(2) 0.094(3) 0.065(3) 0.017(2) 0.0010(18) -0.018(2)
C15B 0.037(2) 0.091(3) 0.073(3) -0.010(2) 0.0077(18) 0.0009(19)
C16B 0.0421(19) 0.055(2) 0.062(2) -0.0023(16) 0.0055(16) 0.0028(15)
C17B 0.0447(18) 0.0376(18) 0.0341(16) -0.0046(13) 0.0107(13) -0.0038(13)
O18B 0.0516(14) 0.0409(14) 0.0640(15) 0.0072(11) 0.0187(12) 0.0046(10)
N19B 0.0364(14) 0.0415(15) 0.0519(17) 0.0044(12) 0.0101(12) -0.0022(11)
C20B 0.0399(18) 0.0452(18) 0.050(2) -0.0001(14) 0.0125(15) -0.0040(13)
C21B 0.043(2) 0.077(3) 0.073(3) 0.010(2) 0.0039(18) 0.0077(18)
C22B 0.044(2) 0.203(7) 0.067(3) 0.033(4) 0.002(2) 0.005(3)
C23B 0.065(4) 0.350(13) 0.129(6) 0.097(7) 0.010(4) 0.064(6)
C24B 0.098(5) 0.256(11) 0.180(8) 0.003(8) -0.011(5) -0.094(7)
C25B 0.0379(17) 0.049(2) 0.051(2) 0.0004(15) 0.0112(15) -0.0047(14)
O26B 0.0649(17) 0.0575(16) 0.0674(18) -0.0124(12) 0.0219(14) -0.0143(12)
N27B 0.070(2) 0.0520(18) 0.0481(17) 0.0014(14) 0.0209(15) 0.0003(14)
C28B 0.079(3) 0.074(3) 0.048(2) 0.0045(18) 0.016(2) 0.015(2)
C29B 0.107(4) 0.143(5) 0.066(3) 0.000(3) -0.006(3) 0.057(4)
C30B 0.184(6) 0.075(3) 0.080(3) 0.017(3) 0.074(4) 0.002(3)
C31B 0.054(2) 0.084(3) 0.051(2) -0.007(2) 0.0124(19) -0.006(2)
O32B 0.086(2) 0.111(3) 0.076(2) -0.0399(19) -0.0019(17) 0.0105(18)
O33B 0.0531(17) 0.093(2) 0.0725(19) -0.0061(15) 0.0013(15) -0.0028(14)
C34B 0.061(3) 0.104(4) 0.138(5) -0.003(3) 0.015(3) 0.023(3)
C1C 0.0300(19) 0.115(4) 0.092(3) -0.017(3) 0.001(2) -0.010(2)
C2C 0.067(3) 0.197(7) 0.144(6) -0.031(5) 0.055(4) -0.044(4)
C3C 0.052(3) 0.168(6) 0.139(5) -0.055(4) -0.007(3) -0.036(3)
C4C 0.069(4) 0.175(7) 0.181(7) -0.006(6) -0.055(4) 0.034(4)
O5C 0.0380(13) 0.0719(16) 0.0576(15) -0.0044(12) -0.0022(11) -0.0143(11)
C6C 0.044(2) 0.062(2) 0.0395(18) 0.0013(16) -0.0013(15) -0.0054(16)
O7C 0.0462(14) 0.0813(19) 0.0764(19) -0.0191(15) 0.0057(13) 0.0069(13)
N8C 0.0379(16) 0.0491(18) 0.0454(17) -0.0091(12) 0.0043(12) -0.0091(12)
C9C 0.0394(17) 0.0430(18) 0.0423(18) -0.0035(13) -0.0021(14) -0.0045(13)
C10C 0.0430(19) 0.063(2) 0.051(2) 0.0067(16) -0.0040(16) -0.0124(16)
C11C 0.049(2) 0.089(3) 0.054(2) 0.022(2) -0.0030(18) -0.013(2)
C12C 0.085(4) 0.151(5) 0.065(3) -0.010(3) -0.015(3) -0.003(3)
C13C 0.110(6) 0.257(11) 0.081(5) -0.013(6) -0.046(4) 0.009(6)
C14C 0.088(5) 0.241(10) 0.078(4) 0.057(6) -0.040(4) -0.001(5)
C15C 0.063(3) 0.174(7) 0.154(6) 0.087(6) -0.011(4) 0.014(4)
C16C 0.058(3) 0.109(4) 0.092(3) 0.038(3) -0.016(2) -0.009(3)
C17C 0.0370(17) 0.0367(18) 0.0465(19) -0.0004(13) 0.0019(14) -0.0066(13)
O18C 0.0654(17) 0.0384(14) 0.0716(17) -0.0134(11) -0.0194(13) 0.0059(11)
N19C 0.0355(14) 0.0344(14) 0.0432(15) -0.0043(11) -0.0028(11) 0.0005(11)
C20C 0.0338(16) 0.0395(17) 0.0450(18) 0.0017(13) -0.0031(13) -0.0030(12)
C21C 0.0420(19) 0.052(2) 0.0441(19) -0.0064(14) -0.0061(15) -0.0033(14)
C22C 0.046(2) 0.075(3) 0.0414(19) -0.0006(16) -0.0002(16) 0.0018(17)
C23C 0.071(3) 0.085(3) 0.074(3) 0.015(2) 0.013(2) -0.014(2)
C24C 0.089(3) 0.111(4) 0.052(3) -0.008(2) 0.008(2) 0.011(3)
C25C 0.0357(17) 0.050(2) 0.0476(19) -0.0043(15) -0.0002(14) -0.0050(14)
O26C 0.0444(14) 0.0597(16) 0.0716(17) 0.0177(13) 0.0078(12) 0.0001(11)
N27C 0.0389(16) 0.0489(17) 0.064(2) -0.0019(14) 0.0089(13) -0.0009(13)
C28C 0.046(2) 0.064(2) 0.071(3) -0.0083(18) 0.0120(18) 0.0000(17)
C29C 0.049(2) 0.075(3) 0.131(4) -0.015(3) 0.027(3) 0.007(2)
C30C 0.089(4) 0.128(4) 0.072(3) -0.022(3) 0.024(3) -0.005(3)
C31C 0.0357(19) 0.066(2) 0.075(3) 0.001(2) 0.0187(19) 0.0032(16)
O32C 0.084(2) 0.088(2) 0.099(2) 0.0107(18) 0.0512(19) -0.0048(17)
O33C 0.0513(15) 0.0560(15) 0.0776(19) 0.0045(13) -0.0065(13) -0.0096(11)
C34C 0.062(3) 0.052(2) 0.128(4) -0.002(2) -0.016(3) -0.0070(19)
O101 0.111(3) 0.0675(19) 0.094(2) -0.0022(16) 0.032(2) -0.0052(17)

_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
C1A O5A 1.487(4) . ?
C1A C3A 1.490(7) . ?
C1A C4A 1.495(6) . ?
C1A C2A 1.511(6) . ?
O5A C6A 1.342(4) . ?
C6A O7A 1.214(4) . ?
C6A N8A 1.320(4) . ?
N8A C9A 1.459(4) . ?
C9A C10A 1.528(4) . ?
C9A C17A 1.536(4) . ?
C10A C11A 1.520(4) . ?
C11A C16A 1.371(5) . ?
C11A C12A 1.386(5) . ?
C12A C13A 1.387(6) . ?
C13A C14A 1.350(7) . ?
C14A C15A 1.368(7) . ?
C15A C16A 1.385(6) . ?
C17A O18A 1.231(4) . ?
C17A N19A 1.318(4) . ?
N19A C20A 1.467(4) . ?
C20A C25A 1.481(5) . ?
C20A C21A 1.528(5) . ?
C21A C22A 1.529(5) . ?
C22A C24A 1.499(6) . ?
C22A C23A 1.539(6) . ?
C25A O26A 1.235(4) . ?
C25A N27A 1.342(4) . ?
N27A C28A 1.458(5) . ?
C28A C31A 1.524(7) . ?
C28A C29A 1.533(7) . ?
C28A C30A 1.546(7) . ?
C31A O32A 1.192(5) . ?
C31A O33A 1.335(6) . ?
O33A C34A 1.429(6) . ?
C1B O5B 1.471(4) . ?
C1B C3B 1.486(6) . ?
C1B C4B 1.527(8) . ?
C1B C2B 1.526(6) . ?
O5B C6B 1.340(4) . ?
C6B O7B 1.212(4) . ?
C6B N8B 1.360(4) . ?
N8B C9B 1.450(4) . ?
C9B C10B 1.526(4) . ?
C9B C17B 1.537(4) . ?
C10B C11B 1.515(4) . ?
C11B C12B 1.383(5) . ?
C11B C16B 1.392(5) . ?
C12B C13B 1.375(5) . ?
C13B C14B 1.376(6) . ?
C14B C15B 1.382(6) . ?
C15B C16B 1.389(6) . ?
C17B O18B 1.238(4) . ?
C17B N19B 1.322(4) . ?
N19B C20B 1.456(4) . ?
C20B C25B 1.506(5) . ?
C20B C21B 1.547(5) . ?
C21B C22B 1.509(6) . ?
C22B C23B 1.502(9) . ?
C22B C24B 1.590(12) . ?
C25B O26B 1.225(4) . ?
C25B N27B 1.332(4) . ?
N27B C28B 1.471(5) . ?
C28B C29B 1.501(7) . ?
C28B C31B 1.526(6) . ?
C28B C30B 1.543(7) . ?
C31B O32B 1.203(5) . ?
C31B O33B 1.306(5) . ?
O33B C34B 1.458(6) . ?
C1C O5C 1.456(5) . ?
C1C C2C 1.486(8) . ?
C1C C4C 1.504(9) . ?
C1C C3C 1.542(7) . ?
O5C C6C 1.350(4) . ?
C6C O7C 1.202(4) . ?
C6C N8C 1.348(5) . ?
N8C C9C 1.449(4) . ?
C9C C17C 1.524(5) . ?
C9C C10C 1.526(5) . ?
C10C C11C 1.494(5) . ?
C11C C12C 1.363(7) . ?
C11C C16C 1.380(7) . ?
C12C C13C 1.373(9) . ?
C13C C14C 1.354(12) . ?
C14C C15C 1.420(12) . ?
C15C C16C 1.410(7) . ?
C17C O18C 1.232(4) . ?
C17C N19C 1.328(4) . ?
N19C C20C 1.454(4) . ?
C20C C21C 1.525(5) . ?
C20C C25C 1.529(5) . ?
C21C C22C 1.533(5) . ?
C22C C23C 1.502(6) . ?
C22C C24C 1.523(6) . ?
C25C O26C 1.219(4) . ?
C25C N27C 1.326(4) . ?
N27C C28C 1.477(5) . ?
C28C C30C 1.513(6) . ?
C28C C31C 1.520(6) . ?
C28C C29C 1.561(6) . ?
C31C O32C 1.205(5) . ?
C31C O33C 1.310(5) . ?
O33C C34C 1.443(5) . ?
O201 C202 1.481(14) . ?
O203 C204 1.625(16) . ?

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
O5A C1A C3A 102.3(4) . . ?
O5A C1A C4A 110.0(3) . . ?
C3A C1A C4A 112.4(4) . . ?
O5A C1A C2A 109.0(3) . . ?
C3A C1A C2A 110.2(4) . . ?
C4A C1A C2A 112.5(4) . . ?
C6A O5A C1A 121.8(3) . . ?
O7A C6A N8A 124.5(3) . . ?
O7A C6A O5A 125.1(3) . . ?
N8A C6A O5A 110.3(3) . . ?
C6A N8A C9A 122.4(3) . . ?
N8A C9A C10A 110.6(3) . . ?
N8A C9A C17A 109.6(2) . . ?
C10A C9A C17A 109.0(2) . . ?
C11A C10A C9A 112.6(3) . . ?
C16A C11A C12A 118.7(3) . . ?
C16A C11A C10A 121.0(3) . . ?
C12A C11A C10A 120.4(3) . . ?
C11A C12A C13A 120.3(4) . . ?
C14A C13A C12A 119.7(4) . . ?
C13A C14A C15A 121.3(4) . . ?
C14A C15A C16A 119.1(4) . . ?
C11A C16A C15A 120.9(4) . . ?
O18A C17A N19A 122.4(3) . . ?
O18A C17A C9A 121.2(3) . . ?
N19A C17A C9A 116.4(3) . . ?
C17A N19A C20A 120.3(3) . . ?
N19A C20A C25A 108.7(3) . . ?
N19A C20A C21A 109.3(3) . . ?
C25A C20A C21A 110.5(3) . . ?
C20A C21A C22A 114.6(3) . . ?
C24A C22A C21A 112.6(3) . . ?
C24A C22A C23A 112.3(4) . . ?
C21A C22A C23A 108.4(4) . . ?
O26A C25A N27A 122.4(3) . . ?
O26A C25A C20A 121.0(3) . . ?
N27A C25A C20A 116.5(3) . . ?
C25A N27A C28A 121.3(3) . . ?
N27A C28A C31A 110.7(4) . . ?
N27A C28A C29A 110.2(4) . . ?
C31A C28A C29A 111.3(4) . . ?
N27A C28A C30A 106.2(4) . . ?
C31A C28A C30A 107.6(4) . . ?
C29A C28A C30A 110.8(4) . . ?
O32A C31A O33A 124.6(5) . . ?
O32A C31A C28A 124.1(5) . . ?
O33A C31A C28A 111.2(4) . . ?
C31A O33A C34A 117.0(4) . . ?
O5B C1B C3B 109.1(4) . . ?
O5B C1B C4B 110.5(4) . . ?
C3B C1B C4B 113.3(5) . . ?
O5B C1B C2B 101.6(3) . . ?
C3B C1B C2B 112.0(4) . . ?
C4B C1B C2B 109.8(4) . . ?
C6B O5B C1B 121.8(3) . . ?
O7B C6B O5B 126.9(3) . . ?
O7B C6B N8B 125.4(3) . . ?
O5B C6B N8B 107.8(3) . . ?
C6B N8B C9B 121.6(3) . . ?
N8B C9B C10B 111.8(2) . . ?
N8B C9B C17B 108.7(2) . . ?
C10B C9B C17B 111.4(2) . . ?
C11B C10B C9B 111.8(2) . . ?
C12B C11B C16B 118.7(3) . . ?
C12B C11B C10B 121.0(3) . . ?
C16B C11B C10B 120.2(3) . . ?
C13B C12B C11B 121.4(3) . . ?
C12B C13B C14B 119.6(4) . . ?
C13B C14B C15B 120.2(4) . . ?
C14B C15B C16B 120.1(4) . . ?
C15B C16B C11B 119.9(4) . . ?
O18B C17B N19B 123.7(3) . . ?
O18B C17B C9B 121.4(3) . . ?
N19B C17B C9B 114.8(3) . . ?
C17B N19B C20B 122.4(3) . . ?
N19B C20B C25B 110.1(3) . . ?
N19B C20B C21B 108.4(3) . . ?
C25B C20B C21B 109.3(3) . . ?
C22B C21B C20B 115.5(4) . . ?
C23B C22B C21B 110.6(5) . . ?
C23B C22B C24B 112.0(7) . . ?
C21B C22B C24B 110.7(5) . . ?
O26B C25B N27B 123.4(3) . . ?
O26B C25B C20B 121.0(3) . . ?
N27B C25B C20B 115.6(3) . . ?
C25B N27B C28B 123.0(3) . . ?
N27B C28B C29B 111.3(4) . . ?
N27B C28B C31B 109.6(3) . . ?
C29B C28B C31B 109.6(4) . . ?
N27B C28B C30B 106.4(4) . . ?
C29B C28B C30B 113.1(4) . . ?
C31B C28B C30B 106.7(4) . . ?
O32B C31B O33B 123.8(4) . . ?
O32B C31B C28B 123.1(4) . . ?
O33B C31B C28B 112.9(4) . . ?
C31B O33B C34B 117.3(4) . . ?
O5C C1C C2C 110.1(4) . . ?
O5C C1C C4C 108.5(4) . . ?
C2C C1C C4C 113.8(6) . . ?
O5C C1C C3C 101.3(4) . . ?
C2C C1C C3C 111.2(5) . . ?
C4C C1C C3C 111.1(5) . . ?
C6C O5C C1C 120.6(3) . . ?
O7C C6C N8C 125.5(3) . . ?
O7C C6C O5C 125.5(3) . . ?
N8C C6C O5C 109.0(3) . . ?
C6C N8C C9C 119.9(3) . . ?
N8C C9C C17C 111.2(3) . . ?
N8C C9C C10C 111.2(3) . . ?
C17C C9C C10C 108.5(3) . . ?
C11C C10C C9C 112.4(3) . . ?
C12C C11C C16C 118.9(5) . . ?
C12C C11C C10C 120.9(5) . . ?
C16C C11C C10C 120.1(4) . . ?
C11C C12C C13C 121.8(7) . . ?
C14C C13C C12C 120.1(8) . . ?
C13C C14C C15C 120.9(6) . . ?
C16C C15C C14C 116.8(7) . . ?
C11C C16C C15C 121.4(6) . . ?
O18C C17C N19C 122.1(3) . . ?
O18C C17C C9C 121.0(3) . . ?
N19C C17C C9C 116.8(3) . . ?
C17C N19C C20C 120.0(3) . . ?
N19C C20C C21C 110.6(3) . . ?
N19C C20C C25C 107.7(3) . . ?
C21C C20C C25C 111.5(3) . . ?
C20C C21C C22C 114.2(3) . . ?
C23C C22C C24C 110.5(4) . . ?
C23C C22C C21C 112.5(3) . . ?
C24C C22C C21C 108.9(3) . . ?
O26C C25C N27C 123.0(3) . . ?
O26C C25C C20C 121.4(3) . . ?
N27C C25C C20C 115.6(3) . . ?
C25C N27C C28C 121.4(3) . . ?
N27C C28C C30C 109.6(3) . . ?
N27C C28C C31C 110.2(3) . . ?
C30C C28C C31C 111.4(4) . . ?
N27C C28C C29C 106.5(3) . . ?
C30C C28C C29C 111.5(4) . . ?
C31C C28C C29C 107.5(3) . . ?
O32C C31C O33C 123.7(4) . . ?
O32C C31C C28C 123.0(4) . . ?
O33C C31C C28C 113.2(3) . . ?
C31C O33C C34C 117.1(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3A C1A O5A C6A -179.5(4) . . . . ?
C4A C1A O5A C6A -59.9(5) . . . . ?
C2A C1A O5A C6A 63.9(4) . . . . ?
C1A O5A C6A O7A -0.8(5) . . . . ?
C1A O5A C6A N8A -179.2(3) . . . . ?
O7A C6A N8A C9A 3.1(5) . . . . ?
O5A C6A N8A C9A -178.4(3) . . . . ?
C6A N8A C9A C10A 141.0(3) . . . . ?
C6A N8A C9A C17A -98.8(3) . . . . ?
N8A C9A C10A C11A -65.9(3) . . . . ?
C17A C9A C10A C11A 173.5(3) . . . . ?
C9A C10A C11A C16A -80.7(4) . . . . ?
C9A C10A C11A C12A 98.7(4) . . . . ?
C16A C11A C12A C13A 1.0(7) . . . . ?
C10A C11A C12A C13A -178.5(4) . . . . ?
C11A C12A C13A C14A -1.3(8) . . . . ?
C12A C13A C14A C15A 1.1(9) . . . . ?
C13A C14A C15A C16A -0.5(8) . . . . ?
C12A C11A C16A C15A -0.4(6) . . . . ?
C10A C11A C16A C15A 179.0(3) . . . . ?
C14A C15A C16A C11A 0.2(6) . . . . ?
N8A C9A C17A O18A -61.3(4) . . . . ?
C10A C9A C17A O18A 59.9(4) . . . . ?
N8A C9A C17A N19A 117.7(3) . . . . ?
C10A C9A C17A N19A -121.1(3) . . . . ?
O18A C17A N19A C20A -3.6(5) . . . . ?
C9A C17A N19A C20A 177.4(3) . . . . ?
C17A N19A C20A C25A -63.7(4) . . . . ?
C17A N19A C20A C21A 175.6(3) . . . . ?
N19A C20A C21A C22A 179.7(3) . . . . ?
C25A C20A C21A C22A 60.1(4) . . . . ?
C20A C21A C22A C24A 64.6(5) . . . . ?
C20A C21A C22A C23A -170.5(4) . . . . ?
N19A C20A C25A O26A -53.6(4) . . . . ?
C21A C20A C25A O26A 66.3(4) . . . . ?
N19A C20A C25A N27A 130.1(3) . . . . ?
C21A C20A C25A N27A -110.0(3) . . . . ?
O26A C25A N27A C28A 4.6(5) . . . . ?
C20A C25A N27A C28A -179.1(3) . . . . ?
C25A N27A C28A C31A -49.9(5) . . . . ?
C25A N27A C28A C29A 73.6(5) . . . . ?
C25A N27A C28A C30A -166.4(4) . . . . ?
N27A C28A C31A O32A 141.1(4) . . . . ?
C29A C28A C31A O32A 18.2(6) . . . . ?
C30A C28A C31A O32A -103.3(5) . . . . ?
N27A C28A C31A O33A -43.2(4) . . . . ?
C29A C28A C31A O33A -166.0(4) . . . . ?
C30A C28A C31A O33A 72.4(5) . . . . ?
O32A C31A O33A C34A -4.7(7) . . . . ?
C28A C31A O33A C34A 179.6(4) . . . . ?
C3B C1B O5B C6B -64.5(5) . . . . ?
C4B C1B O5B C6B 60.7(5) . . . . ?
C2B C1B O5B C6B 177.1(4) . . . . ?
C1B O5B C6B O7B -10.0(5) . . . . ?
C1B O5B C6B N8B 171.6(3) . . . . ?
O7B C6B N8B C9B 4.0(5) . . . . ?
O5B C6B N8B C9B -177.6(3) . . . . ?
C6B N8B C9B C10B 119.1(3) . . . . ?
C6B N8B C9B C17B -117.5(3) . . . . ?
N8B C9B C10B C11B -65.6(3) . . . . ?
C17B C9B C10B C11B 172.5(3) . . . . ?
C9B C10B C11B C12B -98.9(3) . . . . ?
C9B C10B C11B C16B 80.0(4) . . . . ?
C16B C11B C12B C13B -1.1(5) . . . . ?
C10B C11B C12B C13B 177.9(3) . . . . ?
C11B C12B C13B C14B -0.7(5) . . . . ?
C12B C13B C14B C15B 1.5(6) . . . . ?
C13B C14B C15B C16B -0.7(6) . . . . ?
C14B C15B C16B C11B -1.1(6) . . . . ?
C12B C11B C16B C15B 1.9(5) . . . . ?
C10B C11B C16B C15B -177.1(3) . . . . ?
N8B C9B C17B O18B -52.3(4) . . . . ?
C10B C9B C17B O18B 71.4(4) . . . . ?
N8B C9B C17B N19B 128.1(3) . . . . ?
C10B C9B C17B N19B -108.2(3) . . . . ?
O18B C17B N19B C20B 0.2(5) . . . . ?
C9B C17B N19B C20B 179.8(3) . . . . ?
C17B N19B C20B C25B -86.7(4) . . . . ?
C17B N19B C20B C21B 153.7(3) . . . . ?
N19B C20B C21B C22B -173.1(4) . . . . ?
C25B C20B C21B C22B 66.8(5) . . . . ?
C20B C21B C22B C23B -168.5(6) . . . . ?
C20B C21B C22B C24B 66.8(6) . . . . ?
N19B C20B C25B O26B -51.0(4) . . . . ?
C21B C20B C25B O26B 68.0(4) . . . . ?
N19B C20B C25B N27B 131.7(3) . . . . ?
C21B C20B C25B N27B -109.3(4) . . . . ?
O26B C25B N27B C28B 1.2(6) . . . . ?
C20B C25B N27B C28B 178.4(3) . . . . ?
C25B N27B C28B C29B 69.4(5) . . . . ?
C25B N27B C28B C31B -52.0(5) . . . . ?
C25B N27B C28B C30B -167.0(4) . . . . ?
N27B C28B C31B O32B 144.5(4) . . . . ?
C29B C28B C31B O32B 22.1(6) . . . . ?
C30B C28B C31B O32B -100.7(5) . . . . ?
N27B C28B C31B O33B -40.7(5) . . . . ?
C29B C28B C31B O33B -163.1(4) . . . . ?
C30B C28B C31B O33B 74.1(5) . . . . ?
O32B C31B O33B C34B -2.6(6) . . . . ?
C28B C31B O33B C34B -177.3(4) . . . . ?
C2C C1C O5C C6C 68.1(6) . . . . ?
C4C C1C O5C C6C -57.1(5) . . . . ?
C3C C1C O5C C6C -174.2(4) . . . . ?
C1C O5C C6C O7C -8.2(5) . . . . ?
C1C O5C C6C N8C 174.2(3) . . . . ?
O7C C6C N8C C9C 16.6(5) . . . . ?
O5C C6C N8C C9C -165.8(3) . . . . ?
C6C N8C C9C C17C -125.2(3) . . . . ?
C6C N8C C9C C10C 113.8(3) . . . . ?
N8C C9C C10C C11C -62.3(4) . . . . ?
C17C C9C C10C C11C 175.2(3) . . . . ?
C9C C10C C11C C12C 102.0(5) . . . . ?
C9C C10C C11C C16C -75.7(5) . . . . ?
C16C C11C C12C C13C -0.9(8) . . . . ?
C10C C11C C12C C13C -178.7(6) . . . . ?
C11C C12C C13C C14C -0.3(12) . . . . ?
C12C C13C C14C C15C 2.0(13) . . . . ?
C13C C14C C15C C16C -2.5(11) . . . . ?
C12C C11C C16C C15C 0.3(7) . . . . ?
C10C C11C C16C C15C 178.1(4) . . . . ?
C14C C15C C16C C11C 1.3(8) . . . . ?
N8C C9C C17C O18C -48.6(4) . . . . ?
C10C C9C C17C O18C 73.9(4) . . . . ?
N8C C9C C17C N19C 134.7(3) . . . . ?
C10C C9C C17C N19C -102.8(3) . . . . ?
O18C C17C N19C C20C -7.7(5) . . . . ?
C9C C17C N19C C20C 169.0(3) . . . . ?
C17C N19C C20C C21C 157.3(3) . . . . ?
C17C N19C C20C C25C -80.7(3) . . . . ?
N19C C20C C21C C22C -62.6(4) . . . . ?
C25C C20C C21C C22C 177.6(3) . . . . ?
C20C C21C C22C C23C -55.8(4) . . . . ?
C20C C21C C22C C24C -178.6(3) . . . . ?
N19C C20C C25C O26C -49.3(4) . . . . ?
C21C C20C C25C O26C 72.2(4) . . . . ?
N19C C20C C25C N27C 130.5(3) . . . . ?
C21C C20C C25C N27C -108.0(3) . . . . ?
O26C C25C N27C C28C 8.9(5) . . . . ?
C20C C25C N27C C28C -170.9(3) . . . . ?
C25C N27C C28C C30C 68.8(5) . . . . ?
C25C N27C C28C C31C -54.1(4) . . . . ?
C25C N27C C28C C29C -170.4(3) . . . . ?
N27C C28C C31C O32C 141.2(4) . . . . ?
C30C C28C C31C O32C 19.3(5) . . . . ?
C29C C28C C31C O32C -103.1(5) . . . . ?
N27C C28C C31C O33C -43.7(4) . . . . ?
C30C C28C C31C O33C -165.6(3) . . . . ?
C29C C28C C31C O33C 72.0(4) . . . . ?
O32C C31C O33C C34C -1.8(5) . . . . ?
C28C C31C O33C C34C -177.0(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.713
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.045