data_global
_journal_name_full               Org.Biomol.Chem.

_journal_coden_Cambridge         0177

_publ_contact_author_name        'Enrique Garcia-Espana'
_publ_contact_author_email       ENRIQUE.GARCIA-ES@UV.ES

_publ_section_title              
;
Self-assembly of 3,5-Bis(ethoxycarbonyl)pyrazolate Anions and
Ammonium Cations of ?-Phenylethylamine or Homoveratrylamine into
Hetero-Double-Stranded Helical Structures
;
_publ_requested_category         FO
loop_
_publ_author_name
'Enrique Garcia-Espana'
'Julio Latorre'
'M. Liu-Gonzalez'
'Pilar Navarro'
;
F.Reviriego
;
'Ana Sanz'

# Attachment 'comp2_rev2.cif'

#\#CIF_1.1

# CIF produced by WinGX routine CIF_UPDATE
# Created on 2009-06-01 at 17:05:39
# Using CIFtbx version 2.6.2 16 Jun 1998

# Dictionary name : cif_core.dic
# Dictionary vers : 2.3
# Request file : c:\wingx\files\archive.dat
# CIF files read : ege7

data_ege7
_database_code_depnum_ccdc_archive 'CCDC 730786'

_audit_creation_date             2009-06-01T17:05:39-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
?
;
_chemical_formula_sum            'C17 H17 N3 O4'
_chemical_formula_weight         327.34

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

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                   16.2750(8)
_cell_length_b                   5.7027(2)
_cell_length_c                   20.1112(10)
_cell_angle_alpha                90
_cell_angle_beta                 100.273(2)
_cell_angle_gamma                90
_cell_volume                     1836.63(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_density_diffrn    1.184
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             688
_exptl_special_details           
;
?
;

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   none

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_reflns_av_R_equivalents  0.0656
_diffrn_reflns_av_unetI/netI     0.1311
_diffrn_reflns_number            6339
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.49
_diffrn_reflns_theta_max         26.91
_diffrn_reflns_theta_full        26.91
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_reflns_number_total             3771
_reflns_number_gt                1317
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_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^)+(0.1989P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    const
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3771
_refine_ls_number_parameters     223
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.2209
_refine_ls_R_factor_gt           0.0631
_refine_ls_wR_factor_ref         0.3011
_refine_ls_wR_factor_gt          0.1837
_refine_ls_goodness_of_fit_ref   0.811
_refine_ls_restrained_S_all      0.811
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.002
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.078

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
O6A O 0.3640(4) 0.1335(9) -0.01407(18) 0.160(2) Uani 1 1 d . . .
O6B O 0.4120(3) 0.3134(7) 0.08277(19) 0.1236(16) Uani 1 1 d . . .
O7A O 0.1462(2) -0.5486(5) 0.03432(13) 0.0757(9) Uani 1 1 d . . .
O7B O 0.1507(2) -0.5553(6) 0.14642(15) 0.0851(10) Uani 1 1 d . . .
N1 N 0.3125(2) 0.0021(6) 0.14604(15) 0.0646(10) Uani 1 1 d . A .
N2 N 0.2610(2) -0.1695(6) 0.15795(15) 0.0640(10) Uani 1 1 d . . .
N3 N -0.1663(2) 0.1085(6) -0.26227(15) 0.0617(9) Uani 1 1 d D . .
H3A H -0.1657 0.2257 -0.2914 0.093 Uiso 1 1 calc R . .
H3B H -0.2006 0.1441 -0.2338 0.093 Uiso 1 1 calc RD . .
H3C H -0.1841 -0.0217 -0.2848 0.093 Uiso 1 1 calc R . .
C3 C 0.2316(3) -0.2776(7) 0.09870(18) 0.0576(11) Uani 1 1 d . . .
C4 C 0.2652(3) -0.1776(8) 0.0479(2) 0.0709(13) Uani 1 1 d . A .
H4 H 0.2561 -0.2193 0.0025 0.085 Uiso 1 1 calc R . .
C5 C 0.3156(3) -0.0004(8) 0.07933(19) 0.0685(12) Uani 1 1 d . . .
C6 C 0.3690(4) 0.1661(10) 0.0518(2) 0.0933(17) Uani 1 1 d . A .
C7 C 0.1729(3) -0.4729(7) 0.0973(2) 0.0637(12) Uani 1 1 d . . .
C8A C 0.3919(11) 0.359(3) -0.0542(9) 0.122(5) Uiso 0.5 1 d P A 1
H8A1 H 0.3453 0.4418 -0.0809 0.147 Uiso 0.5 1 calc PR A 1
H8A2 H 0.4283 0.4668 -0.0254 0.147 Uiso 0.5 1 calc PR A 1
C9A C 0.4392(11) 0.194(3) -0.0970(9) 0.151(5) Uiso 0.5 1 d P A 1
H9A1 H 0.4368 0.0355 -0.0815 0.226 Uiso 0.5 1 calc PR A 1
H9A2 H 0.4965 0.2426 -0.0921 0.226 Uiso 0.5 1 calc PR A 1
H9A3 H 0.4134 0.2033 -0.1438 0.226 Uiso 0.5 1 calc PR A 1
C8B C 0.4391(7) 0.238(2) -0.0458(5) 0.084(3) Uiso 0.5 1 d P A 2
H8B1 H 0.4805 0.3164 -0.0124 0.101 Uiso 0.5 1 calc PR A 2
H8B2 H 0.4657 0.1214 -0.0699 0.101 Uiso 0.5 1 calc PR A 2
C9B C 0.390(2) 0.398(6) -0.0897(14) 0.250(14) Uiso 0.5 1 d P A 2
H9B1 H 0.3565 0.3128 -0.1262 0.375 Uiso 0.5 1 calc PR A 2
H9B2 H 0.4252 0.5063 -0.1075 0.375 Uiso 0.5 1 calc PR A 2
H9B3 H 0.3535 0.4817 -0.0652 0.375 Uiso 0.5 1 calc PR A 2
C10 C 0.0905(3) -0.7468(9) 0.0255(2) 0.0839(15) Uani 1 1 d . . .
H10A H 0.0393 -0.7091 0.0415 0.101 Uiso 1 1 calc R . .
H10B H 0.1164 -0.8801 0.051 0.101 Uiso 1 1 calc R . .
C11 C 0.0724(4) -0.8031(11) -0.0472(3) 0.116(2) Uani 1 1 d . . .
H11A H 0.0511 -0.6662 -0.0723 0.174 Uiso 1 1 calc R . .
H11B H 0.0316 -0.9262 -0.0551 0.174 Uiso 1 1 calc R . .
H11C H 0.1227 -0.8536 -0.0616 0.174 Uiso 1 1 calc R . .
C12 C -0.0265(3) -0.0529(11) -0.2656(2) 0.0937(17) Uani 1 1 d . . .
H12A H -0.0254 0.0372 -0.3064 0.113(19) Uiso 1 1 calc R . .
H12B H -0.0503 -0.2054 -0.2789 0.15(3) Uiso 1 1 calc R . .
C13 C -0.0801(3) 0.0702(9) -0.2233(2) 0.0741(13) Uani 1 1 d . . .
H13A H -0.0831 -0.0228 -0.1835 0.13(2) Uiso 1 1 calc R . .
H13B H -0.0553 0.2203 -0.2086 0.13(2) Uiso 1 1 calc R . .
C20 C 0.0626(3) -0.0842(9) -0.2271(2) 0.0736(13) Uani 1 1 d . . .
C21 C 0.0825(3) -0.2689(10) -0.1843(3) 0.0873(15) Uani 1 1 d . . .
H21 H 0.0414 -0.3765 -0.1785 0.105 Uiso 1 1 calc R . .
C22 C 0.1626(4) -0.2981(10) -0.1495(3) 0.0916(16) Uani 1 1 d . . .
H22 H 0.1756 -0.4264 -0.121 0.11 Uiso 1 1 calc R . .
C23 C 0.2234(3) -0.1390(11) -0.1567(2) 0.0884(16) Uani 1 1 d . . .
H23 H 0.2777 -0.1584 -0.1333 0.106 Uiso 1 1 calc R . .
C24 C 0.2034(4) 0.0474(11) -0.1984(3) 0.0908(16) Uani 1 1 d . . .
H24 H 0.2443 0.1571 -0.203 0.109 Uiso 1 1 calc R . .
C25 C 0.1245(4) 0.0762(10) -0.2335(2) 0.0862(15) Uani 1 1 d . . .
H25 H 0.1121 0.2047 -0.262 0.103 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
O6A 0.236(5) 0.186(5) 0.070(2) -0.020(2) 0.055(3) -0.147(4)
O6B 0.158(4) 0.117(3) 0.095(3) -0.023(2) 0.021(2) -0.077(3)
O7A 0.095(2) 0.072(2) 0.0592(18) -0.0039(14) 0.0116(15) -0.0281(18)
O7B 0.109(3) 0.086(2) 0.0643(19) 0.0033(16) 0.0264(17) -0.0214(19)
N1 0.078(2) 0.064(2) 0.052(2) -0.0053(17) 0.0127(17) -0.006(2)
N2 0.078(2) 0.065(2) 0.0494(19) -0.0037(16) 0.0118(17) -0.006(2)
N3 0.068(2) 0.064(2) 0.0536(19) 0.0016(15) 0.0120(17) 0.0030(18)
C3 0.069(3) 0.061(3) 0.043(2) -0.0017(19) 0.0094(19) -0.008(2)
C4 0.086(3) 0.080(3) 0.047(2) -0.009(2) 0.014(2) -0.015(3)
C5 0.081(3) 0.074(3) 0.052(2) -0.007(2) 0.016(2) -0.016(3)
C6 0.118(4) 0.098(4) 0.065(3) -0.011(3) 0.020(3) -0.044(4)
C7 0.073(3) 0.067(3) 0.052(2) -0.002(2) 0.012(2) 0.001(2)
C10 0.102(4) 0.074(3) 0.077(3) -0.006(2) 0.019(3) -0.031(3)
C11 0.154(6) 0.113(5) 0.081(4) -0.020(3) 0.022(3) -0.064(4)
C12 0.094(4) 0.115(5) 0.069(3) -0.018(3) 0.007(3) 0.018(4)
C13 0.078(3) 0.084(3) 0.059(3) 0.002(2) 0.006(2) 0.009(3)
C20 0.072(3) 0.090(3) 0.055(2) -0.004(2) 0.003(2) 0.011(3)
C21 0.079(4) 0.087(4) 0.091(3) 0.004(3) 0.001(3) -0.012(3)
C22 0.096(4) 0.081(4) 0.095(4) 0.011(3) 0.007(3) 0.006(3)
C23 0.074(4) 0.104(4) 0.083(3) -0.004(3) 0.004(3) 0.007(3)
C24 0.082(4) 0.099(4) 0.092(4) 0.007(3) 0.017(3) -0.012(3)
C25 0.090(4) 0.091(4) 0.077(3) 0.015(3) 0.013(3) 0.008(3)

#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_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
O6A C6 1.326(6) . ?
O6A C8B 1.592(11) . ?
O6A C8A 1.625(17) . ?
O6B C6 1.195(6) . ?
O7A C7 1.335(5) . ?
O7A C10 1.440(5) . ?
O7B C7 1.206(5) . ?
N1 N2 1.338(5) . ?
N1 C5 1.352(5) . ?
N2 C3 1.351(5) . ?
N3 C13 1.495(6) . ?
N3 H3A 0.89 . ?
N3 H3B 0.89 . ?
N3 H3C 0.89 . ?
C3 C4 1.367(6) . ?
C3 C7 1.464(6) . ?
C4 C5 1.382(6) . ?
C4 H4 0.93 . ?
C5 C6 1.461(7) . ?
C8A C9A 1.57(2) . ?
C8A H8A1 0.97 . ?
C8A H8A2 0.97 . ?
C9A H9A1 0.96 . ?
C9A H9A2 0.96 . ?
C9A H9A3 0.96 . ?
C8B C9B 1.41(3) . ?
C8B H8B1 0.97 . ?
C8B H8B2 0.97 . ?
C9B H9B1 0.96 . ?
C9B H9B2 0.96 . ?
C9B H9B3 0.96 . ?
C10 C11 1.474(6) . ?
C10 H10A 0.97 . ?
C10 H10B 0.97 . ?
C11 H11A 0.96 . ?
C11 H11B 0.96 . ?
C11 H11C 0.96 . ?
C12 C13 1.498(6) . ?
C12 C20 1.527(7) . ?
C12 H12A 0.97 . ?
C12 H12B 0.97 . ?
C13 H13A 0.97 . ?
C13 H13B 0.97 . ?
C20 C21 1.362(7) . ?
C20 C25 1.384(7) . ?
C21 C22 1.376(7) . ?
C21 H21 0.93 . ?
C22 C23 1.369(7) . ?
C22 H22 0.93 . ?
C23 C24 1.357(7) . ?
C23 H23 0.93 . ?
C24 C25 1.361(7) . ?
C24 H24 0.93 . ?
C25 H25 0.93 . ?

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
C6 O6A C8B 115.6(5) . . ?
C6 O6A C8A 114.3(7) . . ?
C8B O6A C8A 37.1(6) . . ?
C7 O7A C10 117.5(3) . . ?
N2 N1 C5 107.8(3) . . ?
N1 N2 C3 108.1(3) . . ?
C13 N3 H3A 109.5 . . ?
C13 N3 H3B 109.5 . . ?
H3A N3 H3B 109.5 . . ?
C13 N3 H3C 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
N2 C3 C4 110.0(4) . . ?
N2 C3 C7 119.4(3) . . ?
C4 C3 C7 130.5(4) . . ?
C3 C4 C5 104.3(4) . . ?
C3 C4 H4 127.8 . . ?
C5 C4 H4 127.8 . . ?
N1 C5 C4 109.7(4) . . ?
N1 C5 C6 120.0(4) . . ?
C4 C5 C6 130.3(4) . . ?
O6B C6 O6A 123.0(5) . . ?
O6B C6 C5 126.3(4) . . ?
O6A C6 C5 110.7(4) . . ?
O7B C7 O7A 123.8(4) . . ?
O7B C7 C3 124.8(4) . . ?
O7A C7 C3 111.4(3) . . ?
C9A C8A O6A 90.3(12) . . ?
C9A C8A H8A1 113.6 . . ?
O6A C8A H8A1 113.6 . . ?
C9A C8A H8A2 113.6 . . ?
O6A C8A H8A2 113.6 . . ?
H8A1 C8A H8A2 110.9 . . ?
C9B C8B O6A 95.6(15) . . ?
C9B C8B H8B1 112.6 . . ?
O6A C8B H8B1 112.6 . . ?
C9B C8B H8B2 112.7 . . ?
O6A C8B H8B2 112.6 . . ?
H8B1 C8B H8B2 110.1 . . ?
C8B C9B H9B1 109.4 . . ?
C8B C9B H9B2 109.5 . . ?
H9B1 C9B H9B2 109.5 . . ?
C8B C9B H9B3 109.5 . . ?
H9B1 C9B H9B3 109.5 . . ?
H9B2 C9B H9B3 109.5 . . ?
O7A C10 C11 107.6(4) . . ?
O7A C10 H10A 110.2 . . ?
C11 C10 H10A 110.2 . . ?
O7A C10 H10B 110.2 . . ?
C11 C10 H10B 110.2 . . ?
H10A C10 H10B 108.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 C20 111.3(4) . . ?
C13 C12 H12A 109.4 . . ?
C20 C12 H12A 109.4 . . ?
C13 C12 H12B 109.4 . . ?
C20 C12 H12B 109.4 . . ?
H12A C12 H12B 108 . . ?
N3 C13 C12 111.0(4) . . ?
N3 C13 H13A 109.4 . . ?
C12 C13 H13A 109.4 . . ?
N3 C13 H13B 109.4 . . ?
C12 C13 H13B 109.4 . . ?
H13A C13 H13B 108 . . ?
C21 C20 C25 118.4(5) . . ?
C21 C20 C12 120.5(5) . . ?
C25 C20 C12 121.1(5) . . ?
C20 C21 C22 120.8(5) . . ?
C20 C21 H21 119.6 . . ?
C22 C21 H21 119.6 . . ?
C23 C22 C21 120.2(5) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C24 C23 C22 119.1(5) . . ?
C24 C23 H23 120.4 . . ?
C22 C23 H23 120.4 . . ?
C23 C24 C25 121.0(5) . . ?
C23 C24 H24 119.5 . . ?
C25 C24 H24 119.5 . . ?
C24 C25 C20 120.5(5) . . ?
C24 C25 H25 119.8 . . ?
C20 C25 H25 119.8 . . ?

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
C5 N1 N2 C3 -0.4(5) . . . . ?
N1 N2 C3 C4 0.8(5) . . . . ?
N1 N2 C3 C7 -179.6(4) . . . . ?
N2 C3 C4 C5 -0.9(5) . . . . ?
C7 C3 C4 C5 179.6(4) . . . . ?
N2 N1 C5 C4 -0.1(5) . . . . ?
N2 N1 C5 C6 -178.7(4) . . . . ?
C3 C4 C5 N1 0.6(5) . . . . ?
C3 C4 C5 C6 178.9(5) . . . . ?
C8B O6A C6 O6B 19.7(10) . . . . ?
C8A O6A C6 O6B -21.4(11) . . . . ?
C8B O6A C6 C5 -160.2(7) . . . . ?
C8A O6A C6 C5 158.7(8) . . . . ?
N1 C5 C6 O6B -0.7(9) . . . . ?
C4 C5 C6 O6B -178.8(6) . . . . ?
N1 C5 C6 O6A 179.3(5) . . . . ?
C4 C5 C6 O6A 1.1(9) . . . . ?
C10 O7A C7 O7B -2.7(7) . . . . ?
C10 O7A C7 C3 177.6(4) . . . . ?
N2 C3 C7 O7B -3.7(7) . . . . ?
C4 C3 C7 O7B 175.8(5) . . . . ?
N2 C3 C7 O7A 176.0(4) . . . . ?
C4 C3 C7 O7A -4.5(7) . . . . ?
C6 O6A C8A C9A 138.5(10) . . . . ?
C8B O6A C8A C9A 37.6(10) . . . . ?
C6 O6A C8B C9B -117.7(15) . . . . ?
C8A O6A C8B C9B -20.7(19) . . . . ?
C7 O7A C10 C11 -177.9(5) . . . . ?
C20 C12 C13 N3 177.8(4) . . . . ?
C13 C12 C20 C21 84.0(6) . . . . ?
C13 C12 C20 C25 -94.6(6) . . . . ?
C25 C20 C21 C22 -1.5(8) . . . . ?
C12 C20 C21 C22 179.9(5) . . . . ?
C20 C21 C22 C23 1.1(8) . . . . ?
C21 C22 C23 C24 0.1(8) . . . . ?
C22 C23 C24 C25 -0.8(8) . . . . ?
C23 C24 C25 C20 0.4(8) . . . . ?
C21 C20 C25 C24 0.8(7) . . . . ?
C12 C20 C25 C24 179.4(5) . . . . ?

# Attachment 'comp3_homo.cif'

data_ege4
_database_code_depnum_ccdc_archive 'CCDC 730787'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            'Compound ege4v09'
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H16 N O2, C9 H11 N2 O4'
_chemical_formula_sum            'C19 H27 N3 O6'
_chemical_formula_weight         393.44

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/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                   13.1760(5)
_cell_length_b                   5.4360(2)
_cell_length_c                   29.7130(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.289(2)
_cell_angle_gamma                90.00
_cell_volume                     2100.28(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3901
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      25.35

_exptl_crystal_description       flat
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.015
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             840
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean 9
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6300
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_sigmaI/netI    0.0637
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         1.61
_diffrn_reflns_theta_max         25.36
_reflns_number_total             3791
_reflns_number_gt                1827
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 19)'
_computing_structure_solution    'SIR97(Altomare & Al., 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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^)+(0.1101P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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         3791
_refine_ls_number_parameters     258
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1286
_refine_ls_R_factor_gt           0.0513
_refine_ls_wR_factor_ref         0.1827
_refine_ls_wR_factor_gt          0.1399
_refine_ls_goodness_of_fit_ref   0.917
_refine_ls_restrained_S_all      0.917
_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
O6A O 0.14831(13) -0.0757(4) 0.19326(6) 0.0879(7) Uani 1 1 d . . .
O6B O 0.07698(15) -0.2143(4) 0.25157(8) 0.0946(7) Uani 1 1 d . . .
O7A O -0.09759(14) 0.6700(4) 0.11288(6) 0.0798(6) Uani 1 1 d . . .
O7B O -0.22781(16) 0.7110(4) 0.15260(7) 0.0977(7) Uani 1 1 d . . .
O15 O 0.29073(17) -0.1729(4) 0.00013(7) 0.1016(7) Uani 1 1 d . . .
O16 O 0.23013(17) 0.1825(5) 0.04566(8) 0.1059(8) Uani 1 1 d . . .
N1 N -0.08264(15) 0.1327(4) 0.22834(7) 0.0678(6) Uani 1 1 d . . .
N2 N -0.14352(15) 0.3140(4) 0.20854(7) 0.0663(6) Uani 1 1 d . . .
N3 N 0.65192(14) 0.2176(4) 0.22504(6) 0.0638(6) Uani 1 1 d . . .
H3A H 0.7124 0.2556 0.2172 0.096 Uiso 1 1 calc R . .
H3B H 0.6615 0.1173 0.2490 0.096 Uiso 1 1 calc R . .
H3C H 0.6209 0.3543 0.2321 0.096 Uiso 1 1 calc R . .
C3 C -0.09952(18) 0.4073(5) 0.17377(8) 0.0608(7) Uani 1 1 d . . .
C4 C -0.00923(18) 0.2823(5) 0.17128(8) 0.0656(7) Uani 1 1 d . . .
H4 H 0.0362 0.3079 0.1508 0.079 Uiso 1 1 calc R . .
C5 C -0.00175(17) 0.1121(5) 0.20573(8) 0.0614(7) Uani 1 1 d . . .
C6 C 0.07608(19) -0.0758(6) 0.22000(10) 0.0725(8) Uani 1 1 d . . .
C7 C -0.1497(2) 0.6098(6) 0.14646(9) 0.0702(8) Uani 1 1 d . . .
C8 C 0.2299(2) -0.2587(7) 0.20361(12) 0.1011(11) Uani 1 1 d . . .
H8A H 0.2601 -0.2499 0.2356 0.121 Uiso 1 1 calc R . .
H8B H 0.2022 -0.4227 0.1973 0.121 Uiso 1 1 calc R . .
C9 C 0.3070(3) -0.2070(7) 0.17537(13) 0.1177(13) Uani 1 1 d . . .
H9A H 0.2766 -0.2174 0.1438 0.177 Uiso 1 1 calc R . .
H9B H 0.3618 -0.3248 0.1817 0.177 Uiso 1 1 calc R . .
H9C H 0.3339 -0.0445 0.1819 0.177 Uiso 1 1 calc R . .
C10 C -0.1347(2) 0.8744(6) 0.08434(10) 0.0879(9) Uani 1 1 d . . .
H10A H -0.1427 1.0180 0.1028 0.106 Uiso 1 1 calc R . .
H10B H -0.2009 0.8354 0.0664 0.106 Uiso 1 1 calc R . .
C11 C -0.0577(3) 0.9236(9) 0.05393(13) 0.1324(15) Uani 1 1 d . . .
H11A H 0.0090 0.9437 0.0720 0.199 Uiso 1 1 calc R . .
H11B H -0.0762 1.0710 0.0368 0.199 Uiso 1 1 calc R . .
H11C H -0.0563 0.7878 0.0334 0.199 Uiso 1 1 calc R . .
C12 C 0.5671(2) 0.2549(6) 0.14567(10) 0.0948(10) Uani 1 1 d . . .
H12A H 0.6318 0.2942 0.1358 0.114 Uiso 1 1 calc R . .
H12B H 0.5365 0.4075 0.1538 0.114 Uiso 1 1 calc R . .
C13 C 0.58661(19) 0.0930(6) 0.18614(9) 0.0730(8) Uani 1 1 d . . .
H13A H 0.6206 -0.0559 0.1785 0.088 Uiso 1 1 calc R . .
H13B H 0.5216 0.0465 0.1951 0.088 Uiso 1 1 calc R . .
C15 C 0.3206(3) -0.3699(7) -0.02656(11) 0.1127(12) Uani 1 1 d . . .
H15A H 0.3833 -0.3276 -0.0372 0.169 Uiso 1 1 calc R . .
H15B H 0.2675 -0.3989 -0.0522 0.169 Uiso 1 1 calc R . .
H15C H 0.3310 -0.5160 -0.0082 0.169 Uiso 1 1 calc R . .
C16 C 0.1904(3) 0.3712(8) 0.07066(14) 0.1245(14) Uani 1 1 d . . .
H16A H 0.1965 0.3233 0.1021 0.187 Uiso 1 1 calc R . .
H16B H 0.1192 0.3981 0.0584 0.187 Uiso 1 1 calc R . .
H16C H 0.2283 0.5202 0.0684 0.187 Uiso 1 1 calc R . .
C20 C 0.4955(2) 0.1332(6) 0.10651(9) 0.0804(9) Uani 1 1 d . . .
C21 C 0.5253(2) -0.0658(7) 0.08317(12) 0.0945(10) Uani 1 1 d . . .
H21 H 0.5910 -0.1303 0.0916 0.113 Uiso 1 1 calc R . .
C22 C 0.4591(3) -0.1727(6) 0.04720(11) 0.0921(10) Uani 1 1 d . . .
H22 H 0.4816 -0.3046 0.0315 0.110 Uiso 1 1 calc R . .
C23 C 0.3621(2) -0.0859(6) 0.03494(9) 0.0756(8) Uani 1 1 d . . .
C24 C 0.3294(2) 0.1092(6) 0.05935(9) 0.0777(8) Uani 1 1 d . . .
C25 C 0.3959(2) 0.2183(6) 0.09423(9) 0.0785(8) Uani 1 1 d . . .
H25 H 0.3735 0.3511 0.1097 0.094 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
O6A 0.0605(11) 0.1193(18) 0.0878(13) 0.0152(12) 0.0241(10) 0.0189(11)
O6B 0.0820(14) 0.1087(17) 0.0980(15) 0.0245(14) 0.0289(11) 0.0091(11)
O7A 0.0776(12) 0.0955(16) 0.0686(11) 0.0109(11) 0.0182(10) 0.0035(10)
O7B 0.0717(13) 0.1039(17) 0.1225(18) 0.0073(13) 0.0301(12) 0.0168(12)
O15 0.1097(16) 0.0991(18) 0.0883(14) -0.0203(13) -0.0068(13) 0.0032(13)
O16 0.0785(14) 0.122(2) 0.1119(16) -0.0244(14) -0.0019(12) 0.0109(13)
N1 0.0572(13) 0.0856(17) 0.0629(12) -0.0023(12) 0.0169(11) -0.0044(12)
N2 0.0538(12) 0.0840(17) 0.0645(13) -0.0049(12) 0.0197(10) -0.0023(12)
N3 0.0483(11) 0.0782(15) 0.0664(13) 0.0017(11) 0.0142(10) 0.0018(10)
C3 0.0523(15) 0.0773(19) 0.0541(14) -0.0059(14) 0.0121(12) -0.0073(14)
C4 0.0489(15) 0.091(2) 0.0595(15) -0.0048(16) 0.0168(12) -0.0053(14)
C5 0.0469(14) 0.0830(19) 0.0567(14) -0.0057(15) 0.0157(11) -0.0059(14)
C6 0.0563(16) 0.095(2) 0.0692(17) -0.0033(18) 0.0177(14) -0.0052(16)
C7 0.0586(17) 0.081(2) 0.0715(17) -0.0119(16) 0.0110(14) -0.0093(16)
C8 0.074(2) 0.119(3) 0.115(3) 0.013(2) 0.0271(19) 0.0198(19)
C9 0.088(2) 0.139(3) 0.135(3) -0.007(3) 0.043(2) 0.025(2)
C10 0.088(2) 0.088(2) 0.0842(19) 0.0099(18) 0.0033(17) -0.0095(17)
C11 0.122(3) 0.164(4) 0.110(3) 0.054(3) 0.015(2) -0.013(3)
C12 0.092(2) 0.096(2) 0.092(2) 0.0171(19) 0.0011(18) -0.0182(18)
C13 0.0617(15) 0.087(2) 0.0733(16) 0.0009(17) 0.0183(13) -0.0011(14)
C15 0.154(3) 0.096(3) 0.086(2) -0.018(2) 0.010(2) -0.008(2)
C16 0.091(2) 0.138(4) 0.146(3) -0.028(3) 0.024(2) 0.017(2)
C20 0.081(2) 0.091(2) 0.0665(17) 0.0070(17) 0.0057(15) -0.0123(18)
C21 0.079(2) 0.106(3) 0.096(2) 0.005(2) 0.0052(18) 0.0064(19)
C22 0.099(2) 0.089(2) 0.088(2) -0.0058(18) 0.0142(19) 0.0085(19)
C23 0.080(2) 0.078(2) 0.0656(16) -0.0012(17) 0.0034(15) -0.0018(17)
C24 0.0726(19) 0.087(2) 0.0724(17) 0.0025(17) 0.0084(15) -0.0023(17)
C25 0.083(2) 0.082(2) 0.0704(18) -0.0011(16) 0.0128(16) -0.0060(16)

_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
O6A C6 1.334(3) . ?
O6A C8 1.461(4) . ?
O6B C6 1.202(3) . ?
O7A C7 1.340(3) . ?
O7A C10 1.435(3) . ?
O7B C7 1.206(3) . ?
O15 C23 1.365(3) . ?
O15 C15 1.425(4) . ?
O16 C24 1.365(3) . ?
O16 C16 1.416(4) . ?
N1 N2 1.345(3) . ?
N1 C5 1.353(3) . ?
N2 C3 1.362(3) . ?
N3 C13 1.488(3) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 H3C 0.8900 . ?
C3 C4 1.382(3) . ?
C3 C7 1.461(4) . ?
C4 C5 1.372(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.461(4) . ?
C8 C9 1.446(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 C11 1.487(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.479(4) . ?
C12 C20 1.525(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C20 C21 1.376(4) . ?
C20 C25 1.384(4) . ?
C21 C22 1.393(4) . ?
C21 H21 0.9300 . ?
C22 C23 1.356(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.392(4) . ?
C24 C25 1.379(4) . ?
C25 H25 0.9300 . ?

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
C6 O6A C8 116.5(2) . . ?
C7 O7A C10 117.5(2) . . ?
C23 O15 C15 117.6(3) . . ?
C24 O16 C16 118.2(3) . . ?
N2 N1 C5 107.8(2) . . ?
N1 N2 C3 107.94(19) . . ?
C13 N3 H3A 109.5 . . ?
C13 N3 H3B 109.5 . . ?
H3A N3 H3B 109.5 . . ?
C13 N3 H3C 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
N2 C3 C4 109.4(2) . . ?
N2 C3 C7 119.5(2) . . ?
C4 C3 C7 131.1(2) . . ?
C5 C4 C3 104.5(2) . . ?
C5 C4 H4 127.7 . . ?
C3 C4 H4 127.7 . . ?
N1 C5 C4 110.3(2) . . ?
N1 C5 C6 119.1(2) . . ?
C4 C5 C6 130.6(2) . . ?
O6B C6 O6A 123.1(3) . . ?
O6B C6 C5 125.6(2) . . ?
O6A C6 C5 111.2(3) . . ?
O7B C7 O7A 123.6(3) . . ?
O7B C7 C3 125.5(3) . . ?
O7A C7 C3 110.9(2) . . ?
C9 C8 O6A 107.9(3) . . ?
C9 C8 H8A 110.1 . . ?
O6A C8 H8A 110.1 . . ?
C9 C8 H8B 110.1 . . ?
O6A C8 H8B 110.1 . . ?
H8A C8 H8B 108.4 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O7A C10 C11 107.3(3) . . ?
O7A C10 H10A 110.3 . . ?
C11 C10 H10A 110.3 . . ?
O7A C10 H10B 110.3 . . ?
C11 C10 H10B 110.3 . . ?
H10A C10 H10B 108.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 C20 111.6(3) . . ?
C13 C12 H12A 109.3 . . ?
C20 C12 H12A 109.3 . . ?
C13 C12 H12B 109.3 . . ?
C20 C12 H12B 109.3 . . ?
H12A C12 H12B 108.0 . . ?
C12 C13 N3 111.3(2) . . ?
C12 C13 H13A 109.4 . . ?
N3 C13 H13A 109.4 . . ?
C12 C13 H13B 109.4 . . ?
N3 C13 H13B 109.4 . . ?
H13A C13 H13B 108.0 . . ?
O15 C15 H15A 109.5 . . ?
O15 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O15 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O16 C16 H16A 109.5 . . ?
O16 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O16 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C21 C20 C25 117.8(3) . . ?
C21 C20 C12 122.3(3) . . ?
C25 C20 C12 119.9(3) . . ?
C20 C21 C22 121.3(3) . . ?
C20 C21 H21 119.3 . . ?
C22 C21 H21 119.3 . . ?
C23 C22 C21 120.5(3) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C22 C23 O15 126.0(3) . . ?
C22 C23 C24 118.8(3) . . ?
O15 C23 C24 115.2(3) . . ?
O16 C24 C25 124.1(3) . . ?
O16 C24 C23 115.4(3) . . ?
C25 C24 C23 120.5(3) . . ?
C24 C25 C20 121.0(3) . . ?
C24 C25 H25 119.5 . . ?
C20 C25 H25 119.5 . . ?

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
C5 N1 N2 C3 -0.5(3) . . . . ?
N1 N2 C3 C4 0.3(3) . . . . ?
N1 N2 C3 C7 -179.6(2) . . . . ?
N2 C3 C4 C5 0.1(3) . . . . ?
C7 C3 C4 C5 179.9(3) . . . . ?
N2 N1 C5 C4 0.6(3) . . . . ?
N2 N1 C5 C6 -179.1(2) . . . . ?
C3 C4 C5 N1 -0.4(3) . . . . ?
C3 C4 C5 C6 179.2(3) . . . . ?
C8 O6A C6 O6B 1.1(4) . . . . ?
C8 O6A C6 C5 -179.0(3) . . . . ?
N1 C5 C6 O6B -2.1(4) . . . . ?
C4 C5 C6 O6B 178.3(3) . . . . ?
N1 C5 C6 O6A 178.0(2) . . . . ?
C4 C5 C6 O6A -1.6(4) . . . . ?
C10 O7A C7 O7B 3.2(4) . . . . ?
C10 O7A C7 C3 -177.1(2) . . . . ?
N2 C3 C7 O7B 2.2(4) . . . . ?
C4 C3 C7 O7B -177.6(3) . . . . ?
N2 C3 C7 O7A -177.5(2) . . . . ?
C4 C3 C7 O7A 2.7(4) . . . . ?
C6 O6A C8 C9 -172.2(3) . . . . ?
C7 O7A C10 C11 173.1(3) . . . . ?
C20 C12 C13 N3 -177.0(2) . . . . ?
C13 C12 C20 C21 -69.1(4) . . . . ?
C13 C12 C20 C25 109.1(3) . . . . ?
C25 C20 C21 C22 2.5(5) . . . . ?
C12 C20 C21 C22 -179.4(3) . . . . ?
C20 C21 C22 C23 -1.6(5) . . . . ?
C21 C22 C23 O15 179.2(3) . . . . ?
C21 C22 C23 C24 -0.9(5) . . . . ?
C15 O15 C23 C22 -1.2(5) . . . . ?
C15 O15 C23 C24 178.9(3) . . . . ?
C16 O16 C24 C25 -4.4(5) . . . . ?
C16 O16 C24 C23 176.6(3) . . . . ?
C22 C23 C24 O16 -178.5(3) . . . . ?
O15 C23 C24 O16 1.3(4) . . . . ?
C22 C23 C24 C25 2.5(4) . . . . ?
O15 C23 C24 C25 -177.7(3) . . . . ?
O16 C24 C25 C20 179.6(3) . . . . ?
C23 C24 C25 C20 -1.6(4) . . . . ?
C21 C20 C25 C24 -0.9(4) . . . . ?
C12 C20 C25 C24 -179.1(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        25.36
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.049