# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2003

data_global

_journal_coden_Cambridge         182

_publ_contact_author_name        'Prof James D. Wuest'

_publ_contact_author_address     
;
Departement de Chimie
Universite de Montreal
Montreal
Quebec
H3C 3J7
CANADA
;

_publ_contact_author_email       WUEST@CHIMIE.UMONTREAL.CA

_publ_requested_journal          'Chemical Communication'
_publ_requested_category         ?

_publ_section_title              
;
Excavations in molecular crystals
;

loop_
_publ_author_name
_publ_author_address
'Le Fur, Erwan'
;
Universite de Montreal
Departement de Chimie
Montreal, Quebec
Canada, H3C 3J7
;
'Demers, Eric'
;
Universite de Montreal
Departement de Chimie
Montreal, Quebec
Canada, H3C 3J7
;
'Maris, Thierry'
;
Universite de Montreal
Departement de Chimie
Montreal, Quebec
Canada, H3C 3J7
;
'Wuest,James D.'
;
Universite de Montreal
Departement de Chimie
Montreal, Quebec
Canada, H3C 3J7
;

_publ_section_abstract           
;
Single crystals built from porous molecular networks can be excavated by agents
that penetrate the crystals, cleave fragments from the network, and thereby
increase the volume available for guests, all without substantial loss of
crystallinity.
;

_publ_section_exptl_refinement   
;
The structure was solved by direct method with ShelxS-97.
All non-H atoms were refined by full-matrix least-squares
with anisotropic displacement parameters while hydrogen atoms
were placed in idealized position.
;

_publ_section_references         
;
SAINT Release 6.06 (1999). Integration Software for Single Crystal Data.
Bruker AXS Inc., Madison, WI 53719-1173.

Sheldrick, G. M. (1996). SADABS, Bruker Area Detector Absorption Corrections.
Bruker AXS Inc., Madison, WI 53719-1173.

Sheldrick, G. M. (1997). SHELXS97. Program for Crystal Structure
solution. University of Gottingen, Germany.

Sheldrick, G. M. (1997). SHELXL97. Program for crystal structure
refinement. University of Gottingen, Germany.

SHELXTL (1997). Release 5.10; The Complete Software Package for Single
Crystal Structure Determination.  Bruker AXS Inc.,
Madison, WI 53719-1173.

SMART (1999). Release 5.059; Bruker Molecular Analysis Research Tool.
Bruker AXS Inc., Madison, WI 53719-1173.

Spek, A. L. (1994). Am. Crystallogr. Assoc.-Abstracts, 22, 66.

Spek, A. L. (2000). PLATON, Molecular Geometry Program, 2000 version.
University of Utrecht, Utrecht, Holland.

P. v.d. Sluis & A.L. Spek, (1990), Acta Cryst. A46, 194.

XPREP (1997). Release 5.10. X-ray data Preparation and Reciprocal space
Exploration Program.  Bruker AXS Inc., Madison, WI 53719-1173.

;

# ========================================================
#                     STRUCTURAL DATA
# ========================================================

data_jiw249
_database_code_depnum_ccdc_archive 'CCDC 222274'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C53 H60 N24 O8'
_chemical_formula_sum            'C53 H60 N24 O8'
_chemical_formula_weight         1161.25
_chemical_compound_source        'Synthesized by the authors. See text'

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I41/a
_symmetry_space_group_name_hall  '-I 4ad'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   25.6644(3)
_cell_length_b                   25.6644(3)
_cell_length_c                   12.2028(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8037.5(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7775
_cell_measurement_theta_min      3.44
_cell_measurement_theta_max      71.79

_exptl_crystal_description       block
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.960
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2440
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_Type   multi-scan
_exptl_absorpt_correction_T_min  0.3300
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'Sadabs (Sheldrick,1996)'

_exptl_special_details           
;
X-ray crystallographic data for I were collected from a single crystal
sample, which was mounted on a glass fiber. Data were collected using
a Bruker Platform diffractometer, equipped with a Bruker SMART 2K
Charged-Coupled Device (CCD) Area Detector using the program SMART and
normal focus sealed tube source graphite monochromated Cu-K\a radiation.
The crystal-to-detector distance was 4.908 cm, and the data collection
was carried out in 512 x 512 pixel mode, utilizing 4 x 4 pixel binning.
The initial unit cell parameters were determined by a least-squares fit
of the angular setting of strong reflections, collected by a 9.0 degree
scan in 30 frames over four different parts of the reciprocal space
(120 frames total).  One complete sphere of data was collected, to
better than 0.8\%A resolution.  Upon completion of the data collection,
the first 101 frames were recollected in order to improve the decay
correction analysis.
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Sealed Tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AXS Smart 2K/Platform'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 5.5
_diffrn_standards_number         264
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.04
_diffrn_reflns_number            32725
_diffrn_reflns_av_R_equivalents  0.055
_diffrn_reflns_av_sigmaI/netI    0.0810
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.44
_diffrn_reflns_theta_max         72.95
_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        72.95
_diffrn_measured_fraction_theta_full 0.991

_reflns_number_total             3976
_reflns_number_gt                2230
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'SMART (Bruker, 1999)'
_computing_cell_refinement       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP (Bruker, 1999)'
_computing_publication_material  'UdMX (local program)'

_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.

The host network can be easily found and refined but no resolved solvent
(DMSO/acetone) molecules could be found within the cavities. Most solvent
molecules were disordered to such extent that few significant difference
peaks were found by Fourier difference. Refining the structure with
isolated solvent peaks for modeling the disordered solvent gave a
residual R1 close to 20% at this point even though what appeared to
be a correct solution was found. The data were treated with the
Squeeze option of the program Platon to remove as much of the
effects of the solvent disorder as possible.

Platon found a potential solvent void of 3166 cubic angstrom in the
unit-cell volume of 8037.5 cubic angstrom, or 39%. The Squeeze option
found 760 electrons of diffuse scattering, values giving 18 DMSO
solvent molecules per unit-cell or 4.5 per molecules. This figures
is close to the 3.5 DMSO per molecules found by NMR, but water maybe
also included in the cavities in the unit cell (see text).

Note that the use of the Squeeze option from Platon has some
consequences in the values of the standard uncertainties of the
geometric data.

Ref : P. v.d. Sluis & A.L. Spek, Acta Cryst. A46, (1990), 194

;

_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^)+(0.0995P)^2^] 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         3976
_refine_ls_number_parameters     193
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1568
_refine_ls_R_factor_gt           0.0824
_refine_ls_wR_factor_ref         0.2306
_refine_ls_wR_factor_gt          0.1885
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.202
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.045

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 0.85878(12) 0.22014(12) 0.1352(3) 0.0892(10) Uani 1 1 d . . .
O2 O 0.82823(13) 0.26353(13) 0.2815(3) 0.0971(11) Uani 1 1 d . . .
N1 N 0.87681(10) 0.37814(10) -0.0836(2) 0.0501(8) Uani 1 1 d . . .
H1 H 0.8864 0.4102 -0.0849 0.060 Uiso 1 1 calc R . .
N2 N 0.81835(10) 0.40947(10) 0.0382(2) 0.0490(8) Uani 1 1 d . . .
N3 N 0.75206(10) 0.35411(10) 0.1108(2) 0.0487(7) Uani 1 1 d . . .
N4 N 0.81804(10) 0.31966(10) -0.0072(2) 0.0475(7) Uani 1 1 d . . .
N5 N 0.75695(12) 0.44037(11) 0.1577(3) 0.0775(11) Uani 1 1 d . . .
H5A H 0.7298 0.4364 0.1982 0.093 Uiso 1 1 calc R . .
H5B H 0.7717 0.4704 0.1532 0.093 Uiso 1 1 calc R . .
N6 N 0.75452(11) 0.26760(10) 0.0695(3) 0.0597(9) Uani 1 1 d . . .
H6 H 0.7245 0.2658 0.1006 0.072 Uiso 1 1 calc R . .
C1 C 1.0000 0.2500 -0.3750 0.0337(13) Uani 1 4 d S . .
C2 C 0.96713(11) 0.28536(11) -0.2986(3) 0.0369(7) Uani 1 1 d . . .
C3 C 0.96571(12) 0.33904(11) -0.3033(3) 0.0443(8) Uani 1 1 d . . .
H3 H 0.9856 0.3560 -0.3562 0.053 Uiso 1 1 calc R . .
C4 C 0.93572(12) 0.36869(12) -0.2323(3) 0.0482(9) Uani 1 1 d . . .
H4 H 0.9359 0.4048 -0.2383 0.058 Uiso 1 1 calc R . .
C5 C 0.90557(11) 0.34509(11) -0.1525(3) 0.0403(8) Uani 1 1 d . . .
C6 C 0.90785(12) 0.29133(12) -0.1431(3) 0.0461(8) Uani 1 1 d . . .
H6' H 0.8891 0.2746 -0.0882 0.055 Uiso 1 1 calc R . .
C7 C 0.93794(12) 0.26243(12) -0.2149(3) 0.0429(8) Uani 1 1 d . . .
H7 H 0.9387 0.2264 -0.2071 0.051 Uiso 1 1 calc R . .
C8 C 0.83618(12) 0.36778(12) -0.0152(3) 0.0432(8) Uani 1 1 d . . .
C9 C 0.77626(12) 0.39976(12) 0.1013(3) 0.0492(9) Uani 1 1 d . . .
C10 C 0.77580(12) 0.31517(12) 0.0576(3) 0.0471(9) Uani 1 1 d . . .
C11 C 0.77811(16) 0.21943(13) 0.0343(4) 0.0657(11) Uani 1 1 d . . .
H11A H 0.8003 0.2265 -0.0284 0.079 Uiso 1 1 calc R . .
H11B H 0.7508 0.1959 0.0102 0.079 Uiso 1 1 calc R . .
C12 C 0.80954(17) 0.19286(16) 0.1193(4) 0.0849(14) Uani 1 1 d . . .
H12A H 0.7903 0.1921 0.1877 0.102 Uiso 1 1 calc R . .
H12B H 0.8163 0.1572 0.0971 0.102 Uiso 1 1 calc R . .
C13 C 0.86285(19) 0.25534(19) 0.2188(5) 0.0796(13) Uani 1 1 d . . .
C14 C 0.91451(18) 0.2804(2) 0.2188(5) 0.1083(18) Uani 1 1 d . . .
H14A H 0.9138 0.3104 0.2658 0.162 Uiso 1 1 calc R . .
H14B H 0.9233 0.2909 0.1457 0.162 Uiso 1 1 calc R . .
H14C H 0.9401 0.2561 0.2451 0.162 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
O1 0.073(2) 0.079(2) 0.116(3) 0.008(2) 0.0097(19) 0.0080(16)
O2 0.075(2) 0.118(3) 0.099(3) 0.005(2) 0.0226(19) -0.009(2)
N1 0.0480(16) 0.0314(14) 0.071(2) -0.0068(14) 0.0189(14) -0.0038(12)
N2 0.0422(15) 0.0355(15) 0.069(2) -0.0039(14) 0.0156(14) -0.0004(12)
N3 0.0381(15) 0.0407(15) 0.067(2) -0.0049(14) 0.0053(13) -0.0013(12)
N4 0.0394(15) 0.0378(15) 0.065(2) 0.0007(13) 0.0122(13) 0.0004(11)
N5 0.070(2) 0.0442(17) 0.119(3) -0.0192(18) 0.045(2) -0.0076(15)
N6 0.0493(17) 0.0372(15) 0.093(3) 0.0022(15) 0.0116(17) -0.0048(13)
C1 0.0312(18) 0.0312(18) 0.039(4) 0.000 0.000 0.000
C2 0.0298(15) 0.0310(15) 0.050(2) -0.0013(14) -0.0001(14) 0.0020(12)
C3 0.0423(18) 0.0340(16) 0.057(2) 0.0016(15) 0.0109(16) -0.0050(13)
C4 0.0450(19) 0.0299(16) 0.070(3) -0.0001(16) 0.0129(17) -0.0032(13)
C5 0.0342(16) 0.0335(16) 0.053(2) -0.0051(15) 0.0025(15) 0.0020(13)
C6 0.0455(19) 0.0416(18) 0.051(2) 0.0035(15) 0.0116(16) -0.0030(14)
C7 0.0430(18) 0.0297(15) 0.056(2) 0.0024(14) 0.0085(16) 0.0017(13)
C8 0.0338(16) 0.0354(17) 0.060(2) 0.0002(15) 0.0029(15) 0.0007(13)
C9 0.0409(18) 0.0405(18) 0.066(3) -0.0078(17) 0.0101(17) 0.0008(14)
C10 0.0369(17) 0.0384(18) 0.066(3) 0.0006(16) 0.0005(17) 0.0011(13)
C11 0.069(3) 0.039(2) 0.090(3) -0.004(2) 0.007(2) -0.0066(18)
C12 0.076(3) 0.050(2) 0.128(4) 0.005(3) 0.013(3) 0.000(2)
C13 0.069(3) 0.072(3) 0.098(4) 0.015(3) 0.004(3) 0.001(2)
C14 0.070(3) 0.122(5) 0.133(5) 0.004(4) 0.001(3) -0.019(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_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C13 . . 1.367(6) Y
O1 C12 . . 1.458(5) Y
O2 C13 . . 1.192(5) Y
N1 C8 . . 1.362(4) Y
N1 C5 . . 1.404(4) Y
N1 H1 . . 0.86 ?
N2 C8 . . 1.334(4) Y
N2 C9 . . 1.349(4) Y
N3 C9 . . 1.331(4) Y
N3 C10 . . 1.338(4) Y
N4 C8 . . 1.323(4) Y
N4 C10 . . 1.347(4) Y
N5 C9 . . 1.343(4) Y
N5 H5a . . 0.86 ?
N5 H5b . . 0.86 ?
N6 C10 . . 1.345(4) Y
N6 C11 . . 1.442(4) Y
N6 H6 . . 0.86 ?
C1 C2 . 12_755 1.551(3) Y
C1 C2 . 15_664 1.551(3) Y
C1 C2 . 6_654 1.551(3) Y
C1 C2 . . 1.551(3) Y
C2 C3 . . 1.379(4) Y
C2 C7 . . 1.397(4) Y
C3 C4 . . 1.387(4) Y
C3 H3 . . 0.93 ?
C4 C5 . . 1.383(4) Y
C4 H4 . . 0.93 ?
C5 C6 . . 1.386(4) Y
C6 C7 . . 1.384(4) Y
C6 H6 . . 0.93 ?
C7 H7 . . 0.93 ?
C11 C12 . . 1.480(6) Y
C11 H11a . . 0.97 ?
C11 H11b . . 0.97 ?
C12 H12a . . 0.97 ?
C12 H12b . . 0.97 ?
C13 C14 . . 1.473(6) Y
C14 H14a . . 0.96 ?
C14 H14b . . 0.96 ?
C14 H14c . . 0.96 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C13 O1 C12 . . . 118.9(4) Y
C8 N1 C5 . . . 130.6(3) Y
C8 N1 H1 . . . 114.7 ?
C5 N1 H1 . . . 114.7 ?
C8 N2 C9 . . . 113.9(3) Y
C9 N3 C10 . . . 113.7(3) Y
C8 N4 C10 . . . 114.0(3) Y
C9 N5 H5A . . . 120 ?
C9 N5 H5B . . . 120 ?
H5A N5 H5B . . . 120 ?
C10 N6 C11 . . . 125.1(3) Y
C10 N6 H6 . . . 117.4 ?
C11 N6 H6 . . . 117.4 ?
C2 C1 C2 12_755 . 15_664 106.1(2) Y
C2 C1 C2 12_755 . 6_654 111.20(12) Y
C2 C1 C2 15_664 . 6_654 111.20(12) Y
C2 C1 C2 12_755 . . 111.20(12) Y
C2 C1 C2 15_664 . . 111.20(12) Y
C2 C1 C2 6_654 . . 106.1(2) Y
C3 C2 C7 . . . 116.0(3) Y
C3 C2 C1 . . . 125.0(3) Y
C7 C2 C1 . . . 119.0(2) Y
C2 C3 C4 . . . 122.4(3) Y
C2 C3 H3 . . . 118.8 ?
C4 C3 H3 . . . 118.8 ?
C5 C4 C3 . . . 120.7(3) Y
C5 C4 H4 . . . 119.7 ?
C3 C4 H4 . . . 119.7 ?
C4 C5 C6 . . . 118.1(3) Y
C4 C5 N1 . . . 116.8(3) Y
C6 C5 N1 . . . 125.1(3) Y
C7 C6 C5 . . . 120.3(3) Y
C7 C6 H6 . . . 119.8 ?
C5 C6 H6 . . . 119.8 ?
C6 C7 C2 . . . 122.5(3) Y
C6 C7 H7 . . . 118.8 ?
C2 C7 H7 . . . 118.8 ?
N4 C8 N2 . . . 126.3(3) Y
N4 C8 N1 . . . 119.8(3) Y
N2 C8 N1 . . . 113.9(3) Y
N3 C9 N5 . . . 117.8(3) Y
N3 C9 N2 . . . 125.9(3) Y
N5 C9 N2 . . . 116.4(3) Y
N3 C10 N6 . . . 116.1(3) Y
N3 C10 N4 . . . 126.0(3) Y
N6 C10 N4 . . . 117.9(3) Y
N6 C11 C12 . . . 114.5(4) Y
N6 C11 H11A . . . 108.6 ?
C12 C11 H11A . . . 108.6 ?
N6 C11 H11B . . . 108.6 ?
C12 C11 H11B . . . 108.6 ?
H11A C11 H11B . . . 107.6 ?
O1 C12 C11 . . . 110.1(3) Y
O1 C12 H12A . . . 109.6 ?
C11 C12 H12A . . . 109.6 ?
O1 C12 H12B . . . 109.6 ?
C11 C12 H12B . . . 109.6 ?
H12A C12 H12B . . . 108.1 ?
O2 C13 O1 . . . 122.6(5) Y
O2 C13 C14 . . . 126.4(6) Y
O1 C13 C14 . . . 110.9(5) Y
C13 C14 H14A . . . 109.5 ?
C13 C14 H14B . . . 109.5 ?
H14A C14 H14B . . . 109.5 ?
C13 C14 H14C . . . 109.5 ?
H14A C14 H14C . . . 109.5 ?
H14B C14 H14C . . . 109.5 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C2 C1 C2 C3 12_755 . . . -112.7(4) Y
C2 C1 C2 C3 15_664 . . . 5.2(3) Y
C2 C1 C2 C3 6_654 . . . 126.3(3) Y
C2 C1 C2 C7 12_755 . . . 70.00(18) Y
C2 C1 C2 C7 15_664 . . . -172.0(3) Y
C2 C1 C2 C7 6_654 . . . -51.0(2) Y
C7 C2 C3 C4 . . . . -2.3(5) Y
C1 C2 C3 C4 . . . . -179.6(3) Y
C2 C3 C4 C5 . . . . 0.0(5) Y
C3 C4 C5 C6 . . . . 2.5(5) Y
C3 C4 C5 N1 . . . . 179.5(3) Y
C8 N1 C5 C4 . . . . 164.2(3) Y
C8 N1 C5 C6 . . . . -19.1(5) Y
C4 C5 C6 C7 . . . . -2.6(5) Y
N1 C5 C6 C7 . . . . -179.3(3) Y
C5 C6 C7 C2 . . . . 0.3(5) Y
C3 C2 C7 C6 . . . . 2.2(5) Y
C1 C2 C7 C6 . . . . 179.7(3) Y
C10 N4 C8 N2 . . . . 3.8(5) Y
C10 N4 C8 N1 . . . . -175.9(3) Y
C9 N2 C8 N4 . . . . -3.3(5) Y
C9 N2 C8 N1 . . . . 176.5(3) Y
C5 N1 C8 N4 . . . . -0.2(5) Y
C5 N1 C8 N2 . . . . 180.0(3) Y
C10 N3 C9 N5 . . . . -175.9(3) Y
C10 N3 C9 N2 . . . . 5.2(5) Y
C8 N2 C9 N3 . . . . -1.7(5) Y
C8 N2 C9 N5 . . . . 179.5(3) Y
C9 N3 C10 N6 . . . . 176.5(3) Y
C9 N3 C10 N4 . . . . -4.6(5) Y
C11 N6 C10 N3 . . . . -169.7(3) Y
C11 N6 C10 N4 . . . . 11.3(6) Y
C8 N4 C10 N3 . . . . 0.5(5) Y
C8 N4 C10 N6 . . . . 179.4(3) Y
C10 N6 C11 C12 . . . . 92.6(5) Y
C13 O1 C12 C11 . . . . 96.6(5) Y
N6 C11 C12 O1 . . . . -74.4(5) Y
C12 O1 C13 O2 . . . . 2.4(7) Y
C12 O1 C13 C14 . . . . -177.6(4) Y

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 N3 0.86 2.46 3.288(4) 161.9 7_544
N5 H5A N2 0.86 2.12 2.975(4) 174.6 8_454
N6 H6 O2 0.86 2.11 2.907(4) 153.3 13_655

# ===========================================================================

data_jiw489
_database_code_depnum_ccdc_archive 'CCDC 222275'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C50.60 H60.40 N24 O6.80'
_chemical_formula_weight         1113.63
_chemical_compound_source        'Synthesized by the authors. See text'

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I41/a
_symmetry_space_group_name_hall  '-I 4ad'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   25.6490(6)
_cell_length_b                   25.6490(6)
_cell_length_c                   11.9420(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7856.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    223(2)
_cell_measurement_reflns_used    3567
_cell_measurement_theta_min      3.49
_cell_measurement_theta_max      38.61

_exptl_crystal_description       block
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.942
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2346
_exptl_absorpt_coefficient_mu    0.550
_exptl_absorpt_correction_Type   multi-scan
_exptl_absorpt_correction_T_min  0.6400
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'Sadabs (Sheldrick,1996)'

_exptl_special_details           
;
X-ray crystallographic data for I were collected from a single crystal
sample, which was mounted on a loop fiber. Data were collected using
a Bruker Platform diffractometer, equipped with a Bruker SMART 2K
Charged-Coupled Device (CCD) Area Detector using the program SMART and
normal focus sealed tube source graphite monochromated Cu-K\a radiation.
The crystal-to-detector distance was 4.908 cm, and the data collection
was carried out in 512 x 512 pixel mode, utilizing 4 x 4 pixel binning.
The initial unit cell parameters were determined by a least-squares fit
of the angular setting of strong reflections, collected by a 9.0 degree
scan in 30 frames over four different parts of the reciprocal space
(120 frames total).  This sample despite the specimen size did not
diffract well as the result of the strain subsequent of the reaction.
The data appear truncated at low resolution and one complete sphere
of data was collected up to 59 degrees. Upon completion of the data
collection, the first 101 frames were recollected in order to
improve the decay correction analysis. Upon completion of the
data collection, the first 101 frames were recollected in order
to improve the decay correction analysis.
;

_diffrn_ambient_temperature      223(2)
_diffrn_radiation_wavelength     1.54180
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Sealed Tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker AXS Smart 2K/Platform'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 5.5
_diffrn_standards_number         5
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.00
_diffrn_reflns_number            18629
_diffrn_reflns_av_R_equivalents  0.046
_diffrn_reflns_av_sigmaI/netI    0.2982
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.45
_diffrn_reflns_theta_max         59.19
_diffrn_measured_fraction_theta_max 0.937
_diffrn_reflns_theta_full        59.19
_diffrn_measured_fraction_theta_full 0.937

_computing_data_collection       'SMART (Bruker, 1999)'
_computing_cell_refinement       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'XP (Bruker, 1999)'
_computing_publication_material  'UdMX (local program)'

_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.

The space group I41/a was determined based on systematic absences and
intensity statistics. A successful direct-methods solution was
calculated which provided most non-hydrogen atoms from the E-map.
Several full-matrix least squares / difference Fourier cycles
were performed which located the remainder of the non-hydrogen
atoms. By this way, the host network can be easily found and
refined but no resolved solvent molecules could be found
within the cavities. Refinement of the acetyl group with
an occupancy factor equals to unity does not converge and
give large anisotropic thermal parameters converging to
unreasonable values. Refinement with a variable occupancy
factor and using restraints on some distances yielded
acceptable value for the thermal parameters.  The solvent
molecules were refined as pseudo atoms from the few
significant difference peaks found by Fourier difference.
;

_reflns_number_total             2675
_reflns_number_gt                559
_reflns_threshold_expression     'I > 2\s(I)'
_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^)+(0.0950P)^2^+17.5400P] 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         2675
_refine_ls_number_parameters     210
_refine_ls_number_restraints     75
_refine_ls_R_factor_all          0.3808
_refine_ls_R_factor_gt           0.1196
_refine_ls_wR_factor_ref         0.3579
_refine_ls_wR_factor_gt          0.3102
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.066

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 0.5000 0.2500 0.3750 0.099(6) Uani 1 4 d SU . 1
N1 N 0.3774(4) 0.3793(3) 0.0755(8) 0.108(3) Uani 1 1 d U A 1
H1 H 0.3882 0.4114 0.0739 0.130 Uiso 1 1 calc . B 1
C2 C 0.4665(4) 0.2854(5) 0.2993(9) 0.087(3) Uani 1 1 d U A 1
N2 N 0.3206(4) 0.4116(4) -0.0506(8) 0.113(3) Uani 1 1 d U A 1
C3 C 0.4642(5) 0.3390(5) 0.3044(9) 0.100(4) Uani 1 1 d U A 1
H3 H 0.4840 0.3559 0.3599 0.120 Uiso 1 1 calc . C 1
N3 N 0.2527(4) 0.3553(4) -0.1240(8) 0.110(3) Uani 1 1 d U A 1
C4 C 0.4344(5) 0.3700(4) 0.2323(10) 0.112(4) Uani 1 1 d U A 1
H4 H 0.4339 0.4065 0.2403 0.134 Uiso 1 1 calc . D 1
N4 N 0.3181(4) 0.3192(4) -0.0006(8) 0.104(3) Uani 1 1 d U A 1
C5 C 0.4058(5) 0.3461(5) 0.1497(10) 0.097(4) Uani 1 1 d U A 1
N5 N 0.2577(4) 0.4413(4) -0.1764(8) 0.135(4) Uani 1 1 d U A 1
H5A H 0.2721 0.4720 -0.1746 0.162 Uiso 1 1 calc . E 1
H5B H 0.2303 0.4359 -0.2178 0.162 Uiso 1 1 calc . F 1
C6 C 0.4060(4) 0.2912(5) 0.1392(9) 0.099(4) Uani 1 1 d U A 1
H6 H 0.3862 0.2741 0.0840 0.118 Uiso 1 1 calc . G 1
N6 N 0.2532(4) 0.2677(4) -0.0780(8) 0.132(4) Uani 1 1 d DU A 1
H6A H 0.2254 0.2655 -0.1196 0.158 Uiso 1 1 calc . H 1
C7 C 0.4373(5) 0.2633(4) 0.2155(9) 0.103(4) Uani 1 1 d U A 1
H7 H 0.4383 0.2268 0.2084 0.123 Uiso 1 1 calc . I 1
C8 C 0.3348(5) 0.3688(6) 0.0044(11) 0.099(4) Uani 1 1 d U A 1
C9 C 0.2781(6) 0.4014(6) -0.1139(12) 0.115(4) Uani 1 1 d U A 1
C10 C 0.2762(5) 0.3148(6) -0.0670(12) 0.109(4) Uani 1 1 d U A 1
C11 C 0.2721(5) 0.2208(4) -0.0241(10) 0.157(5) Uani 1 1 d DU A 1
H11A H 0.2426 0.1998 0.0023 0.189 Uiso 1 1 calc R A 1
H11B H 0.2937 0.2300 0.0406 0.189 Uiso 1 1 calc R A 1
C12 C 0.3044(5) 0.1893(5) -0.1082(12) 0.210(7) Uani 1 1 d DU A 1
H12A H 0.2862 0.1873 -0.1803 0.252 Uiso 1 1 calc R A 1
H12B H 0.3100 0.1538 -0.0804 0.252 Uiso 1 1 calc R A 1
O1 O 0.3597(5) 0.2194(4) -0.1225(10) 0.232(5) Uani 1 1 d DU A 1
C13 C 0.3648(5) 0.2508(6) -0.2163(12) 0.141(7) Uani 0.70 1 d PDU A 1
O2 O 0.3286(4) 0.2600(4) -0.2726(9) 0.154(4) Uani 0.70 1 d PDU A 1
C14 C 0.4174(5) 0.2787(6) -0.2109(13) 0.147(6) Uani 0.70 1 d PDU A 1
H14A H 0.4381 0.2641 -0.1505 0.221 Uiso 0.70 1 calc PR A 1
H14B H 0.4118 0.3155 -0.1974 0.221 Uiso 0.70 1 calc PR A 1
H14C H 0.4357 0.2741 -0.2813 0.221 Uiso 0.70 1 calc PR A 1
O20 O 0.2941(8) 0.4217(8) 0.5142(19) 0.450 Uiso 1 1 d . J 2
C21 C 0.4710(12) 0.4689(11) 0.474(3) 0.450 Uiso 1 1 d . K 2
C22 C 0.3687(12) 0.3603(12) 0.598(3) 0.450 Uiso 1 1 d . L 2
C23 C 0.3483(13) 0.5856(13) 0.782(3) 0.450 Uiso 1 1 d . M 2
C24 C 0.3434(12) 0.5435(12) 0.559(2) 0.450 Uiso 1 1 d . N 2
C25 C 0.4014(13) 0.4988(12) 0.491(3) 0.450 Uiso 1 1 d . K 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
C1 0.105(11) 0.105(11) 0.087(18) 0.000 0.000 0.000
N1 0.115(9) 0.105(8) 0.104(8) 0.005(6) -0.017(5) -0.004(6)
C2 0.100(9) 0.093(8) 0.068(8) -0.006(7) 0.011(6) 0.002(8)
N2 0.130(9) 0.097(7) 0.114(9) 0.018(6) -0.033(6) -0.002(7)
C3 0.122(10) 0.096(7) 0.081(8) -0.007(7) -0.010(6) -0.009(8)
N3 0.094(8) 0.120(9) 0.116(8) 0.015(7) -0.006(6) -0.010(6)
C4 0.146(13) 0.086(8) 0.103(11) -0.015(7) -0.022(7) 0.003(7)
N4 0.119(9) 0.096(7) 0.096(8) 0.010(6) -0.014(6) -0.008(7)
C5 0.108(10) 0.099(8) 0.085(9) -0.003(7) -0.004(6) 0.003(8)
N5 0.144(9) 0.120(8) 0.141(9) 0.028(6) -0.044(7) -0.006(7)
C6 0.115(10) 0.098(8) 0.083(8) -0.009(7) -0.007(6) -0.013(8)
N6 0.133(9) 0.111(9) 0.152(9) 0.017(8) -0.044(7) -0.011(7)
C7 0.142(12) 0.090(8) 0.077(9) -0.002(6) -0.001(6) 0.000(7)
C8 0.090(10) 0.107(9) 0.099(10) 0.015(8) 0.005(6) 0.000(8)
C9 0.126(13) 0.108(9) 0.112(11) 0.021(9) -0.018(7) -0.009(8)
C10 0.100(12) 0.104(9) 0.123(13) 0.007(9) -0.001(7) -0.001(7)
C11 0.158(7) 0.158(7) 0.156(7) -0.002(5) -0.004(5) 0.004(5)
C12 0.207(8) 0.213(8) 0.210(8) -0.004(5) -0.005(5) -0.001(5)
O1 0.238(6) 0.228(6) 0.230(6) -0.016(5) 0.004(5) 0.007(5)
C13 0.146(8) 0.138(8) 0.140(8) -0.008(5) 0.006(5) 0.011(5)
O2 0.153(6) 0.162(6) 0.148(6) -0.012(4) -0.013(5) 0.013(5)
C14 0.143(8) 0.149(8) 0.150(8) -0.005(5) 0.007(5) -0.001(5)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.542(11) 6_554 Y
C1 C2 1.542(11) 16_656 Y
C1 C2 1.542(11) 11_666 Y
C1 C2 1.542(11) . Y
N1 C8 1.409(12) . Y
N1 C5 1.428(12) . Y
C2 C7 1.373(13) . Y
C2 C3 1.377(12) . Y
N2 C8 1.328(13) . Y
N2 C9 1.353(14) . Y
C3 C4 1.401(13) . Y
N3 C9 1.355(13) . Y
N3 C10 1.382(13) . Y
C4 C5 1.374(13) . Y
N4 C10 1.340(13) . Y
N4 C8 1.344(13) . Y
C5 C6 1.415(13) . Y
N5 C9 1.369(13) . Y
C6 C7 1.409(12) . Y
N6 C10 1.349(13) . Y
N6 C11 1.449(5) . Y
C11 C12 1.531(5) . Y
C12 O1 1.624(14) . Y
O1 C13 1.386(5) . Y
C13 O2 1.170(5) . Y
C13 C14 1.529(5) . Y
O20 C23 1.20(3) 4_454 Y
C21 C25 1.95(4) . Y
C22 C23 1.57(3) 4_454 Y
C23 O20 1.20(3) 3 Y
C23 C22 1.57(3) 3 Y

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C2 110.1(4) 6_554 16_656 Y
C2 C1 C2 110.1(4) 6_554 11_666 Y
C2 C1 C2 108.3(8) 16_656 11_666 Y
C2 C1 C2 108.3(8) 6_554 . Y
C2 C1 C2 110.1(4) 16_656 . Y
C2 C1 C2 110.1(4) 11_666 . Y
C8 N1 C5 131.0(11) . . Y
C7 C2 C3 114.9(11) . . Y
C7 C2 C1 119.2(11) . . Y
C3 C2 C1 125.9(11) . . Y
C8 N2 C9 109.8(12) . . Y
C2 C3 C4 124.3(11) . . Y
C9 N3 C10 113.8(13) . . Y
C5 C4 C3 118.6(12) . . Y
C10 N4 C8 111.2(13) . . Y
C4 C5 C6 120.4(12) . . Y
C4 C5 N1 116.9(13) . . Y
C6 C5 N1 122.7(12) . . Y
C7 C6 C5 116.8(11) . . Y
C10 N6 C11 123.5(12) . . Y
C2 C7 C6 124.9(12) . . Y
N2 C8 N4 132.3(14) . . Y
N2 C8 N1 110.7(13) . . Y
N4 C8 N1 116.9(13) . . Y
N2 C9 N3 127.2(14) . . Y
N2 C9 N5 118.0(14) . . Y
N3 C9 N5 114.8(14) . . Y
N4 C10 N6 119.0(14) . . Y
N4 C10 N3 125.3(14) . . Y
N6 C10 N3 115.7(14) . . Y
N6 C11 C12 109.2(10) . . Y
C11 C12 O1 106.9(11) . . Y
C13 O1 C12 116.3(12) . . Y
O2 C13 O1 120.5(14) . . Y
O2 C13 C14 129.1(14) . . Y
O1 C13 C14 108.7(11) . . Y
O20 C23 C22 149(4) 3 3 Y

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
C2 C1 C2 C7 51.2(8) 6_554 . . . Y
C2 C1 C2 C7 -69.2(7) 16_656 . . . Y
C2 C1 C2 C7 171.5(10) 11_666 . . . Y
C2 C1 C2 C3 -126.2(12) 6_554 . . . Y
C2 C1 C2 C3 113.5(13) 16_656 . . . Y
C2 C1 C2 C3 -5.8(11) 11_666 . . . Y
C7 C2 C3 C4 0.9(18) . . . . Y
C1 C2 C3 C4 178.3(9) . . . . Y
C2 C3 C4 C5 -0.9(19) . . . . Y
C3 C4 C5 C6 1.0(18) . . . . Y
C3 C4 C5 N1 -177.8(10) . . . . Y
C8 N1 C5 C4 -160.6(12) . . . . Y
C8 N1 C5 C6 20.7(18) . . . . Y
C4 C5 C6 C7 -1.1(17) . . . . Y
N1 C5 C6 C7 177.6(10) . . . . Y
C3 C2 C7 C6 -1.0(17) . . . . Y
C1 C2 C7 C6 -178.6(9) . . . . Y
C5 C6 C7 C2 1.2(17) . . . . Y
C9 N2 C8 N4 7.2(19) . . . . Y
C9 N2 C8 N1 -176.8(10) . . . . Y
C10 N4 C8 N2 -6.9(19) . . . . Y
C10 N4 C8 N1 177.3(10) . . . . Y
C5 N1 C8 N2 -179.8(11) . . . . Y
C5 N1 C8 N4 -3.2(17) . . . . Y
C8 N2 C9 N3 -0.9(19) . . . . Y
C8 N2 C9 N5 179.7(11) . . . . Y
C10 N3 C9 N2 -4.0(19) . . . . Y
C10 N3 C9 N5 175.4(11) . . . . Y
C8 N4 C10 N6 -177.5(11) . . . . Y
C8 N4 C10 N3 0.2(17) . . . . Y
C11 N6 C10 N4 -1.9(19) . . . . Y
C11 N6 C10 N3 -179.8(10) . . . . Y
C9 N3 C10 N4 4.4(18) . . . . Y
C9 N3 C10 N6 -177.9(11) . . . . Y
C10 N6 C11 C12 -98.5(14) . . . . Y
N6 C11 C12 O1 74.4(13) . . . . Y
C11 C12 O1 C13 -99.8(14) . . . . Y
C12 O1 C13 O2 10(2) . . . . Y
C12 O1 C13 C14 175.9(11) . . . . Y

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 N3 0.87 2.43 3.253(12) 158.4 3
N5 H5A O20 0.87 2.46 3.28(2) 157.4 3_554
N5 H5B N2 0.87 2.03 2.893(12) 172.6 4_454
N6 H6A O2 0.87 2.00 2.844(14) 162.9 13_554

#============================================================================
#===END