# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Gerhard Laus'
_publ_contact_author_email       GERHARD.LAUS@UIBK.AC.AT

_publ_section_title              
;
Hydrogen Bonding in the Perhydrate and Hydrates of
1,4-Diazabicyclo[2.2.2]octane (DABCO)
;
_publ_requested_category         FO
loop_
_publ_author_name
'Gerhard Laus'
'Volker Kahlenberg'
'Thomas Lorting'
'Herwig Schottenberger'

# Attachment 'LAUS_CCDC634612-4_revised.cif'

data_bisperhydrate_CCDC634612
_database_code_depnum_ccdc_archive 'CCDC 634612'

_audit_creation_date             2005-10-06T16:43:51-00:00
_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            'C6 H16 N2 O3.70 '
_chemical_formula_moiety         'C6 H12 N2, 1.7(H2O2), 0.3(H2O)'
_chemical_formula_weight         176.2

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

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

_symmetry_space_group_name_H-M   'I 41/a'
_cell_length_a                   12.0860(17)
_cell_length_b                   12.0860(17)
_cell_length_c                   12.0361(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1758.1(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    173
_cell_measurement_reflns_used    5485
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      27.23

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

_exptl_crystal_description       lath-shaped
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.33
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             768
_exptl_special_details           
;
?
;

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

_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.160
_exptl_absorpt_process_details   
;
SADABS - Bruker Nonius area detector scaling and absorption correction - V2.06
R.H. Blessing, Acta Cryst. (1995) A51 33-38
;

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

_diffrn_source                   
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_ambient_temperature      173
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_number            6709
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.38
_diffrn_reflns_theta_max         26.96
_diffrn_reflns_theta_full        26.95
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_reflns_number_total             948
_reflns_number_gt                789
_reflns_threshold_expression     >2sigma(I)

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

_computing_data_collection       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

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

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0759P)²+1.0460P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_coef       0.055(11)
_refine_ls_number_reflns         948
_refine_ls_number_parameters     66
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0563
_refine_ls_wR_factor_ref         0.1534
_refine_ls_wR_factor_gt          0.1378
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.1
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.199
_refine_diff_density_min         -0.151
_refine_diff_density_rms         0.042

#----------------------------------------------------------------------------#
# 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'
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'
H H 0 0 '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
O1 O 0.7031(2) -0.0040(2) 0.6244(2) 0.0544(8) Uani 0.851(9) 1 d PD . .
H1 H 0.655(3) 0.054(3) 0.622(4) 0.082(10) Uiso 0.851(9) 1 d PD . .
O2 O 0.7876(2) 0.0556(2) 0.6844(3) 0.0644(10) Uani 0.851(9) 1 d PD . .
H2 H 0.775(4) 0.014(3) 0.746(2) 0.082(10) Uiso 0.851(9) 1 d PD . .
N1 N 0.56373(17) 0.16601(16) 0.61668(16) 0.0425(6) Uani 1 1 d . . .
C1 C 0.5353(3) 0.1974(2) 0.7309(2) 0.0600(8) Uani 1 1 d . . .
H1A H 0.6038 0.2103 0.774 0.072 Uiso 1 1 calc R . .
H1B H 0.4938 0.1365 0.7668 0.072 Uiso 1 1 calc R . .
C2 C 0.4620(2) 0.1411(2) 0.5562(3) 0.0603(8) Uani 1 1 d . . .
H2A H 0.4265 0.0746 0.5885 0.072 Uiso 1 1 calc R . .
H2B H 0.4795 0.1253 0.4775 0.072 Uiso 1 1 calc R . .
C3 C 0.6180(2) 0.2598(3) 0.5633(3) 0.0598(8) Uani 1 1 d . . .
H3A H 0.6421 0.2386 0.4877 0.072 Uiso 1 1 calc R . .
H3B H 0.6844 0.2811 0.6065 0.072 Uiso 1 1 calc R . .
OW O 0.7503(2) 0.0297(3) 0.6311(3) 0.082(7) Uiso 0.149(9) 1 d PR . .


#----------------------------------------------------------------------------#
# 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
O1 O2 1.443(4) . ?
O1 H1 0.912(10) . ?
O2 H2 0.908(10) . ?
N1 C3 1.459(4) . ?
N1 C2 1.460(3) . ?
N1 C1 1.467(3) . ?
C1 C1 1.531(6) 2_655 ?
C1 H1A 0.99 . ?
C1 H1B 0.99 . ?
C2 C3 1.541(4) 2_655 ?
C2 H2A 0.99 . ?
C2 H2B 0.99 . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?

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
O2 O1 H1 95(3) . . ?
O1 O2 H2 90(3) . . ?
C3 N1 C2 108.6(2) . . ?
C3 N1 C1 108.5(2) . . ?
C2 N1 C1 108.8(2) . . ?
N1 C1 C1 110.21(13) . 2_655 ?
N1 C1 H1A 109.6 . . ?
C1 C1 H1A 109.6 2_655 . ?
N1 C1 H1B 109.6 . . ?
C1 C1 H1B 109.6 2_655 . ?
H1A C1 H1B 108.1 . . ?
N1 C2 C3 109.9(2) . 2_655 ?
N1 C2 H2A 109.7 . . ?
C3 C2 H2A 109.7 2_655 . ?
N1 C2 H2B 109.7 . . ?
C3 C2 H2B 109.7 2_655 . ?
H2A C2 H2B 108.2 . . ?
N1 C3 C2 110.3(2) . 2_655 ?
N1 C3 H3A 109.6 . . ?
C2 C3 H3A 109.6 2_655 . ?
N1 C3 H3B 109.6 . . ?
C2 C3 H3B 109.6 2_655 . ?
H3A C3 H3B 108.1 . . ?
#===END

data_monohydrate_CCDC634613
_database_code_depnum_ccdc_archive 'CCDC 634613'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H12 N2, 2(C3 H6 N), 2(H2 O)'
_chemical_formula_sum            'C12 H28 N4 O2'
_chemical_formula_weight         260.38

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/c
_symmetry_space_group_name_Hall  -C2yc

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

_cell_length_a                   21.822(4)
_cell_length_b                   6.2155(16)
_cell_length_c                   10.7703(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.225(13)
_cell_angle_gamma                90.00
_cell_volume                     1437.6(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2544
_cell_measurement_theta_min      1.90
_cell_measurement_theta_max      24.97

_exptl_crystal_description       'fragment of a plate'
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             576
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.935
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_process_details   
;
SADABS - Bruker Nonius area detector scaling and absorption correction - V2.06
R.H. Blessing, Acta Cryst. (1995) A51 33-38
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(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  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_detector_area_resol_mean 6.67
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4063
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         24.75
_reflns_number_total             1209
_reflns_number_gt                936
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
STOE X-Area data collection software, WinXpose version 1.6.8
;
_computing_cell_refinement       
;
STOE X-Area version 1.25
;
_computing_data_reduction        
;
STOE X-Area data evaluation software, X-RED 32
;
_computing_structure_solution    
;
BRUKER AXS SHELXTL Vers.6.12, DOS/WIN95/NT/2000/ME
;
_computing_structure_refinement  
;
BRUKER AXS SHELXTL Vers.6.12, DOS/WIN95/NT/2000/ME
;
_computing_molecular_graphics    
;
BRUKER AXS SHELXTL Vers.6.12, DOS/WIN95/NT/2000/ME
;
_computing_publication_material  
;
BRUKER AXS SHELXTL Vers.6.12, DOS/WIN95/NT/2000/ME
;

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0576P)²+1.2563P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1209
_refine_ls_number_parameters     109
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0599
_refine_ls_wR_factor_ref         0.1380
_refine_ls_wR_factor_gt          0.1293
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.088
_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
N1 N 0.28370(8) 0.3983(3) 0.46190(17) 0.0353(5) Uani 1 1 d . . .
C1A C 0.2731(3) 0.4482(9) 0.5891(5) 0.0584(15) Uani 0.50 1 d P . .
H1A1 H 0.2511 0.5876 0.5885 0.070 Uiso 0.50 1 d PR . .
H1A2 H 0.3135 0.4605 0.6473 0.070 Uiso 0.50 1 d PR . .
C2A C 0.3170(2) 0.1897(8) 0.4698(7) 0.0569(15) Uani 0.50 1 d P . .
H2A1 H 0.3565 0.2010 0.5309 0.068 Uiso 0.50 1 d PR . .
H2A2 H 0.3271 0.1531 0.3863 0.068 Uiso 0.50 1 d PR . .
C3A C 0.2263(3) 0.3813(12) 0.3806(7) 0.074(2) Uani 0.50 1 d P . .
H3A1 H 0.2333 0.3474 0.2944 0.089 Uiso 0.50 1 d PR . .
H3A2 H 0.2041 0.5206 0.3775 0.089 Uiso 0.50 1 d PR . .
C1B C 0.3142(3) 0.2975(12) 0.5739(6) 0.069(2) Uani 0.50 1 d P . .
H1B1 H 0.3243 0.4072 0.6410 0.083 Uiso 0.50 1 d PR . .
H1B2 H 0.3538 0.2340 0.5588 0.083 Uiso 0.50 1 d PR . .
C2B C 0.2664(3) 0.2314(10) 0.3650(6) 0.0656(17) Uani 0.50 1 d P . .
H2B1 H 0.3047 0.1678 0.3429 0.079 Uiso 0.50 1 d PR . .
H2B2 H 0.2425 0.2981 0.2879 0.079 Uiso 0.50 1 d PR . .
C3B C 0.2239(3) 0.4890(9) 0.4881(7) 0.0610(16) Uani 0.50 1 d P . .
H3B1 H 0.2011 0.5591 0.4110 0.073 Uiso 0.50 1 d PR . .
H3B2 H 0.2328 0.5995 0.5551 0.073 Uiso 0.50 1 d PR . .
O1 O 0.37594(8) 0.7070(3) 0.39820(15) 0.0504(5) Uani 1 1 d . . .
H2A H 0.4026 0.7180 0.4670 0.076 Uiso 1 1 d R . .
H2B H 0.3477 0.6230 0.4170 0.076 Uiso 1 1 d R . .
N2 N 0.53239(8) 0.2675(3) 0.36252(17) 0.0357(5) Uani 1 1 d . . .
C4 C 0.51910(11) 0.4886(4) 0.3171(2) 0.0437(6) Uani 1 1 d . . .
H4A H 0.5588 0.5663 0.3176 0.052 Uiso 1 1 d R . .
H4B H 0.4957 0.5649 0.3744 0.052 Uiso 1 1 d R . .
C5 C 0.43372(12) 0.1608(4) 0.2258(2) 0.0502(7) Uani 1 1 d . . .
H5A H 0.4238 0.0113 0.1975 0.060 Uiso 1 1 d R . .
H5B H 0.3940 0.2373 0.2268 0.060 Uiso 1 1 d R . .
C6 C 0.47252(12) 0.1582(5) 0.3595(2) 0.0547(8) Uani 1 1 d . . .
H6A H 0.4491 0.2308 0.4182 0.066 Uiso 1 1 d R . .
H6B H 0.4800 0.0075 0.3879 0.066 Uiso 1 1 d R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C3A 1.399(5) . ?
N1 C1B 1.416(6) . ?
N1 C1A 1.463(6) . ?
N1 C2B 1.473(6) . ?
N1 C2A 1.482(5) . ?
N1 C3B 1.494(6) . ?
C1A C1B 1.327(10) . ?
C1A C3B 1.409(9) . ?
C1A C2B 1.544(7) 7_556 ?
C1A H1A1 0.9900 . ?
C1A H1A2 0.9898 . ?
C2A C1B 1.317(10) . ?
C2A C2B 1.456(10) . ?
C2A C3B 1.542(7) 7_556 ?
C2A H2A1 0.9897 . ?
C2A H2A2 0.9897 . ?
C3A C2B 1.309(10) . ?
C3A C3B 1.347(10) . ?
C3A C1B 1.553(8) 7_556 ?
C3A H3A1 0.9900 . ?
C3A H3A2 0.9898 . ?
C1B H1B1 0.9896 . ?
C1B H1B2 0.9894 . ?
C2B H2B1 0.9910 . ?
C2B H2B2 0.9898 . ?
C3B H3B1 0.9901 . ?
C3B H3B2 0.9901 . ?
O1 H2A 0.8600 . ?
O1 H2B 0.8590 . ?
N2 C5 1.463(3) 2_655 ?
N2 C6 1.468(3) . ?
N2 C4 1.470(3) . ?
C4 C4 1.534(5) 2_655 ?
C4 H4A 0.9910 . ?
C4 H4B 0.9892 . ?
C5 C6 1.536(3) . ?
C5 H5A 0.9899 . ?
C5 H5B 0.9905 . ?
C6 H6A 0.9897 . ?
C6 H6B 0.9898 . ?

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
C3A N1 C1B 137.1(3) . . ?
C3A N1 C1A 109.2(5) . . ?
C1B N1 C1A 54.9(4) . . ?
C3A N1 C2B 54.1(5) . . ?
C1B N1 C2B 108.3(5) . . ?
C1A N1 C2B 138.6(3) . . ?
C3A N1 C2A 110.2(5) . . ?
C1B N1 C2A 54.0(4) . . ?
C1A N1 C2A 106.8(4) . . ?
C2B N1 C2A 59.0(4) . . ?
C3A N1 C3B 55.4(4) . . ?
C1B N1 C3B 107.5(4) . . ?
C1A N1 C3B 56.9(4) . . ?
C2B N1 C3B 106.1(4) . . ?
C2A N1 C3B 139.1(3) . . ?
C1B C1A C3B 118.1(5) . . ?
C1B C1A N1 60.8(4) . . ?
C3B C1A N1 62.7(4) . . ?
C1B C1A C2B 87.5(5) . 7_556 ?
C3B C1A C2B 89.2(5) . 7_556 ?
N1 C1A C2B 109.7(4) . 7_556 ?
C1B C1A H1A1 162.7 . . ?
C3B C1A H1A1 62.3 . . ?
N1 C1A H1A1 109.7 . . ?
C2B C1A H1A1 109.7 7_556 . ?
C1B C1A H1A2 65.6 . . ?
C3B C1A H1A2 161.1 . . ?
N1 C1A H1A2 109.8 . . ?
C2B C1A H1A2 109.7 7_556 . ?
H1A1 C1A H1A2 108.2 . . ?
C1B C1A H1B1 46.0 . . ?
C3B C1A H1B1 158.2 . . ?
N1 C1A H1B1 95.9 . . ?
C2B C1A H1B1 103.1 7_556 . ?
H1A1 C1A H1B1 127.4 . . ?
C1B C1A H3B2 156.6 . . ?
N1 C1A H3B2 95.8 . . ?
C2B C1A H3B2 103.0 7_556 . ?
H1A2 C1A H3B2 127.4 . . ?
H1B1 C1A H3B2 145.7 . . ?
C1B C2A C2B 115.2(5) . . ?
C1B C2A N1 60.5(4) . . ?
C2B C2A N1 60.2(3) . . ?
C1B C2A C3B 89.9(5) . 7_556 ?
C2B C2A C3B 87.6(5) . 7_556 ?
N1 C2A C3B 110.1(4) . 7_556 ?
C1B C2A H2A1 64.2 . . ?
C2B C2A H2A1 162.6 . . ?
N1 C2A H2A1 109.7 . . ?
C3B C2A H2A1 109.7 7_556 . ?
C1B C2A H2A2 160.4 . . ?
C2B C2A H2A2 66.2 . . ?
N1 C2A H2A2 109.6 . . ?
C3B C2A H2A2 109.6 7_556 . ?
H2A1 C2A H2A2 108.2 . . ?
C1B C2A H1B2 46.4 . . ?
C2B C2A H1B2 155.5 . . ?
N1 C2A H1B2 95.7 . . ?
C3B C2A H1B2 106.1 7_556 . ?
H2A2 C2A H1B2 124.6 . . ?
C1B C2A H2B1 151.7 . . ?
N1 C2A H2B1 91.3 . . ?
C3B C2A H2B1 101.7 7_556 . ?
H2A1 C2A H2B1 132.3 . . ?
H1B2 C2A H2B1 146.8 . . ?
C2B C3A C3B 126.4(6) . . ?
C2B C3A N1 65.8(4) . . ?
C3B C3A N1 65.9(4) . . ?
C2B C3A C1B 87.8(6) . 7_556 ?
C3B C3A C1B 88.4(6) . 7_556 ?
N1 C3A C1B 110.7(4) . 7_556 ?
C2B C3A H3A1 60.7 . . ?
C3B C3A H3A1 161.5 . . ?
N1 C3A H3A1 109.5 . . ?
C1B C3A H3A1 109.6 7_556 . ?
C2B C3A H3A2 162.3 . . ?
C3B C3A H3A2 60.0 . . ?
N1 C3A H3A2 109.5 . . ?
C1B C3A H3A2 109.5 7_556 . ?
H3A1 C3A H3A2 108.1 . . ?
C2B C3A H2B2 45.8 . . ?
C3B C3A H2B2 165.4 . . ?
N1 C3A H2B2 100.7 . . ?
C1B C3A H2B2 102.5 7_556 . ?
H3A2 C3A H2B2 123.3 . . ?
C2B C3A H3B1 163.4 . . ?
N1 C3A H3B1 98.6 . . ?
C1B C3A H3B1 103.7 7_556 . ?
H3A1 C3A H3B1 124.0 . . ?
H2B2 C3A H3B1 139.1 . . ?
C1A C1B C2A 126.8(6) . . ?
C1A C1B N1 64.3(4) . . ?
C2A C1B N1 65.5(4) . . ?
C1A C1B C3A 91.8(6) . 7_556 ?
C2A C1B C3A 91.2(6) . 7_556 ?
N1 C1B C3A 112.2(4) . 7_556 ?
C1A C1B C2B 50.8(4) . 7_556 ?
C2A C1B C2B 114.4(4) . 7_556 ?
N1 C1B C2B 90.7(4) . 7_556 ?
C1A C1B C3B 114.5(4) . 7_556 ?
C2A C1B C3B 49.5(4) . 7_556 ?
N1 C1B C3B 90.3(4) . 7_556 ?
C2B C1B C3B 72.3(3) 7_556 7_556 ?
C2A C1B H1A2 158.6 . . ?
N1 C1B H1A2 96.9 . . ?
C3A C1B H1A2 107.4 7_556 . ?
C2B C1B H1A2 76.1 7_556 . ?
C3B C1B H1A2 147.7 7_556 . ?
C1A C1B H2A1 160.0 . . ?
C2A C1B H2A1 45.2 . . ?
N1 C1B H2A1 99.3 . . ?
C3A C1B H2A1 105.8 7_556 . ?
C2B C1B H2A1 145.9 7_556 . ?
C3B C1B H2A1 75.2 7_556 . ?
H1A2 C1B H2A1 133.8 . . ?
C1A C1B H1B1 59.4 . . ?
C2A C1B H1B1 159.1 . . ?
N1 C1B H1B1 109.1 . . ?
C3A C1B H1B1 109.1 7_556 . ?
C2B C1B H1B1 85.2 7_556 . ?
C3B C1B H1B1 150.6 7_556 . ?
H2A1 C1B H1B1 121.0 . . ?
C1A C1B H1B2 158.6 . . ?
C2A C1B H1B2 58.9 . . ?
N1 C1B H1B2 109.2 . . ?
C3A C1B H1B2 109.2 7_556 . ?
C2B C1B H1B2 150.0 7_556 . ?
C3B C1B H1B2 85.1 7_556 . ?
H1A2 C1B H1B2 121.4 . . ?
H1B1 C1B H1B2 107.9 . . ?
C3A C2B C2A 117.3(5) . . ?
C3A C2B N1 60.0(4) . . ?
C2A C2B N1 60.8(3) . . ?
C3A C2B C1A 92.9(5) . 7_556 ?
C2A C2B C1A 90.7(5) . 7_556 ?
N1 C2B C1A 111.7(4) . 7_556 ?
C3A C2B C1B 51.1(4) . 7_556 ?
C2A C2B C1B 108.7(4) . 7_556 ?
N1 C2B C1B 87.7(4) . 7_556 ?
C3A C2B H2A2 150.0 . . ?
N1 C2B H2A2 90.7 . . ?
C1A C2B H2A2 105.3 7_556 . ?
C1B C2B H2A2 141.6 7_556 . ?
C3A C2B H3A1 46.3 . . ?
C2A C2B H3A1 153.1 . . ?
N1 C2B H3A1 94.4 . . ?
C1A C2B H3A1 109.4 7_556 . ?
C1B C2B H3A1 78.2 7_556 . ?
H2A2 C2B H3A1 140.1 . . ?
C3A C2B H2B1 157.8 . . ?
C2A C2B H2B1 63.8 . . ?
N1 C2B H2B1 109.3 . . ?
C1A C2B H2B1 109.3 7_556 . ?
C1B C2B H2B1 151.0 7_556 . ?
H3A1 C2B H2B1 121.9 . . ?
C3A C2B H2B2 63.0 . . ?
C2A C2B H2B2 160.0 . . ?
N1 C2B H2B2 109.3 . . ?
C1A C2B H2B2 109.3 7_556 . ?
C1B C2B H2B2 87.2 7_556 . ?
H2A2 C2B H2B2 129.0 . . ?
H2B1 C2B H2B2 107.9 . . ?
C3A C3B C1A 115.7(5) . . ?
C3A C3B N1 58.7(3) . . ?
C1A C3B N1 60.4(3) . . ?
C3A C3B C2A 90.5(5) . 7_556 ?
C1A C3B C2A 92.6(5) . 7_556 ?
N1 C3B C2A 110.8(4) . 7_556 ?
C3A C3B C1B 50.0(4) . 7_556 ?
C1A C3B C1B 107.9(4) . 7_556 ?
N1 C3B C1B 85.8(4) . 7_556 ?
C3A C3B H1A1 150.8 . . ?
N1 C3B H1A1 92.8 . . ?
C2A C3B H1A1 107.4 7_556 . ?
C1B C3B H1A1 142.5 7_556 . ?
C3A C3B H3A2 45.2 . . ?
C1A C3B H3A2 151.6 . . ?
N1 C3B H3A2 92.6 . . ?
C2A C3B H3A2 106.5 7_556 . ?
C1B C3B H3A2 76.4 7_556 . ?
H1A1 C3B H3A2 141.1 . . ?
C3A C3B H3B1 65.7 . . ?
C1A C3B H3B1 158.0 . . ?
N1 C3B H3B1 109.5 . . ?
C2A C3B H3B1 109.4 7_556 . ?
C1B C3B H3B1 89.7 7_556 . ?
H1A1 C3B H3B1 125.5 . . ?
C3A C3B H3B2 159.8 . . ?
C1A C3B H3B2 62.5 . . ?
N1 C3B H3B2 109.5 . . ?
C2A C3B H3B2 109.5 7_556 . ?
C1B C3B H3B2 149.9 7_556 . ?
H3A2 C3B H3B2 126.5 . . ?
H3B1 C3B H3B2 108.1 . . ?
H2A O1 H2B 104.4 . . ?
C5 N2 C6 109.1(2) 2_655 . ?
C5 N2 C4 107.44(19) 2_655 . ?
C6 N2 C4 107.63(19) . . ?
N2 C4 C4 110.83(11) . 2_655 ?
N2 C4 H4A 109.5 . . ?
C4 C4 H4A 109.5 2_655 . ?
N2 C4 H4B 109.5 . . ?
C4 C4 H4B 109.4 2_655 . ?
H4A C4 H4B 108.1 . . ?
N2 C5 C6 110.86(19) 2_655 . ?
N2 C5 H5A 109.5 2_655 . ?
C6 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 2_655 . ?
C6 C5 H5B 109.4 . . ?
H5A C5 H5B 108.0 . . ?
N2 C6 C5 110.88(19) . . ?
N2 C6 H6A 109.5 . . ?
C5 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?

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 N1 C1A C1B 134.7(4) . . . . ?
C2B N1 C1A C1B 77.5(7) . . . . ?
C2A N1 C1A C1B 15.5(4) . . . . ?
C3B N1 C1A C1B 153.7(5) . . . . ?
C3A N1 C1A C3B -19.0(5) . . . . ?
C1B N1 C1A C3B -153.7(5) . . . . ?
C2B N1 C1A C3B -76.1(7) . . . . ?
C2A N1 C1A C3B -138.1(4) . . . . ?
C3A N1 C1A C2B 59.3(7) . . . 7_556 ?
C1B N1 C1A C2B -75.4(6) . . . 7_556 ?
C2B N1 C1A C2B 2.2(11) . . . 7_556 ?
C2A N1 C1A C2B -59.8(6) . . . 7_556 ?
C3B N1 C1A C2B 78.3(6) . . . 7_556 ?
C3A N1 C2A C1B -134.3(4) . . . . ?
C1A N1 C2A C1B -15.7(4) . . . . ?
C2B N1 C2A C1B -152.8(5) . . . . ?
C3B N1 C2A C1B -74.3(7) . . . . ?
C3A N1 C2A C2B 18.5(4) . . . . ?
C1B N1 C2A C2B 152.8(5) . . . . ?
C1A N1 C2A C2B 137.1(4) . . . . ?
C3B N1 C2A C2B 78.5(7) . . . . ?
C3A N1 C2A C3B -56.3(7) . . . 7_556 ?
C1B N1 C2A C3B 77.9(5) . . . 7_556 ?
C1A N1 C2A C3B 62.2(6) . . . 7_556 ?
C2B N1 C2A C3B -74.8(5) . . . 7_556 ?
C3B N1 C2A C3B 3.7(11) . . . 7_556 ?
C1B N1 C3A C2B -78.0(8) . . . . ?
C1A N1 C3A C2B -136.7(4) . . . . ?
C2A N1 C3A C2B -19.6(5) . . . . ?
C3B N1 C3A C2B -156.1(5) . . . . ?
C1B N1 C3A C3B 78.0(8) . . . . ?
C1A N1 C3A C3B 19.3(5) . . . . ?
C2B N1 C3A C3B 156.1(5) . . . . ?
C2A N1 C3A C3B 136.4(4) . . . . ?
C1B N1 C3A C1B -0.4(14) . . . 7_556 ?
C1A N1 C3A C1B -59.1(8) . . . 7_556 ?
C2B N1 C3A C1B 77.7(7) . . . 7_556 ?
C2A N1 C3A C1B 58.0(8) . . . 7_556 ?
C3B N1 C3A C1B -78.4(7) . . . 7_556 ?
C3B C1A C1B C2A 5.4(9) . . . . ?
N1 C1A C1B C2A -21.1(5) . . . . ?
C2B C1A C1B C2A 93.1(7) 7_556 . . . ?
C3B C1A C1B N1 26.5(5) . . . . ?
C2B C1A C1B N1 114.2(4) 7_556 . . . ?
C3B C1A C1B C3A -87.3(6) . . . 7_556 ?
N1 C1A C1B C3A -113.9(4) . . . 7_556 ?
C2B C1A C1B C3A 0.4(5) 7_556 . . 7_556 ?
C3B C1A C1B C2B -87.7(6) . . . 7_556 ?
N1 C1A C1B C2B -114.2(4) . . . 7_556 ?
C3B C1A C1B C3B -51.2(7) . . . 7_556 ?
N1 C1A C1B C3B -77.7(4) . . . 7_556 ?
C2B C1A C1B C3B 36.5(5) 7_556 . . 7_556 ?
C2B C2A C1B C1A -5.1(9) . . . . ?
N1 C2A C1B C1A 20.9(5) . . . . ?
C3B C2A C1B C1A -92.4(7) 7_556 . . . ?
C2B C2A C1B N1 -26.0(4) . . . . ?
C3B C2A C1B N1 -113.3(4) 7_556 . . . ?
C2B C2A C1B C3A 87.9(6) . . . 7_556 ?
N1 C2A C1B C3A 114.0(4) . . . 7_556 ?
C3B C2A C1B C3A 0.7(5) 7_556 . . 7_556 ?
C2B C2A C1B C2B 53.0(7) . . . 7_556 ?
N1 C2A C1B C2B 79.0(5) . . . 7_556 ?
C3B C2A C1B C2B -34.3(6) 7_556 . . 7_556 ?
C2B C2A C1B C3B 87.3(5) . . . 7_556 ?
N1 C2A C1B C3B 113.3(4) . . . 7_556 ?
C3A N1 C1B C1A -80.5(8) . . . . ?
C2B N1 C1B C1A -137.1(4) . . . . ?
C2A N1 C1B C1A -161.5(5) . . . . ?
C3B N1 C1B C1A -22.9(4) . . . . ?
C3A N1 C1B C2A 81.1(8) . . . . ?
C1A N1 C1B C2A 161.5(5) . . . . ?
C2B N1 C1B C2A 24.4(4) . . . . ?
C3B N1 C1B C2A 138.6(4) . . . . ?
C3A N1 C1B C3A 0.4(14) . . . 7_556 ?
C1A N1 C1B C3A 80.8(7) . . . 7_556 ?
C2B N1 C1B C3A -56.3(8) . . . 7_556 ?
C2A N1 C1B C3A -80.7(7) . . . 7_556 ?
C3B N1 C1B C3A 57.9(8) . . . 7_556 ?
C3A N1 C1B C2B -35.6(9) . . . 7_556 ?
C1A N1 C1B C2B 44.9(4) . . . 7_556 ?
C2B N1 C1B C2B -92.2(4) . . . 7_556 ?
C2A N1 C1B C2B -116.6(4) . . . 7_556 ?
C3B N1 C1B C2B 22.0(4) . . . 7_556 ?
C3A N1 C1B C3B 36.7(9) . . . 7_556 ?
C1A N1 C1B C3B 117.2(4) . . . 7_556 ?
C2B N1 C1B C3B -19.9(5) . . . 7_556 ?
C2A N1 C1B C3B -44.3(3) . . . 7_556 ?
C3B N1 C1B C3B 94.3(4) . . . 7_556 ?
C3B C3A C2B C2A -6.2(9) . . . . ?
N1 C3A C2B C2A 21.2(5) . . . . ?
C1B C3A C2B C2A -92.7(5) 7_556 . . . ?
C3B C3A C2B N1 -27.4(5) . . . . ?
C1B C3A C2B N1 -113.8(4) 7_556 . . . ?
C3B C3A C2B C1A 86.0(7) . . . 7_556 ?
N1 C3A C2B C1A 113.5(4) . . . 7_556 ?
C1B C3A C2B C1A -0.4(5) 7_556 . . 7_556 ?
C3B C3A C2B C1B 86.4(7) . . . 7_556 ?
N1 C3A C2B C1B 113.8(4) . . . 7_556 ?
C1B C2A C2B C3A 5.1(8) . . . . ?
N1 C2A C2B C3A -21.0(5) . . . . ?
C3B C2A C2B C3A 93.9(6) 7_556 . . . ?
C1B C2A C2B N1 26.1(4) . . . . ?
C3B C2A C2B N1 114.9(4) 7_556 . . . ?
C1B C2A C2B C1A -88.5(5) . . . 7_556 ?
N1 C2A C2B C1A -114.6(4) . . . 7_556 ?
C3B C2A C2B C1A 0.3(4) 7_556 . . 7_556 ?
C1B C2A C2B C1B -50.1(7) . . . 7_556 ?
N1 C2A C2B C1B -76.2(4) . . . 7_556 ?
C3B C2A C2B C1B 38.7(5) 7_556 . . 7_556 ?
C1B N1 C2B C3A 135.5(5) . . . . ?
C1A N1 C2B C3A 78.2(7) . . . . ?
C2A N1 C2B C3A 158.4(5) . . . . ?
C3B N1 C2B C3A 20.3(5) . . . . ?
C3A N1 C2B C2A -158.4(5) . . . . ?
C1B N1 C2B C2A -23.0(4) . . . . ?
C1A N1 C2B C2A -80.2(7) . . . . ?
C3B N1 C2B C2A -138.1(4) . . . . ?
C3A N1 C2B C1A -80.4(6) . . . 7_556 ?
C1B N1 C2B C1A 55.1(7) . . . 7_556 ?
C1A N1 C2B C1A -2.2(11) . . . 7_556 ?
C2A N1 C2B C1A 78.0(6) . . . 7_556 ?
C3B N1 C2B C1A -60.0(7) . . . 7_556 ?
C3A N1 C2B C1B -45.5(4) . . . 7_556 ?
C1B N1 C2B C1B 90.0(4) . . . 7_556 ?
C1A N1 C2B C1B 32.7(8) . . . 7_556 ?
C2A N1 C2B C1B 113.0(4) . . . 7_556 ?
C3B N1 C2B C1B -25.1(4) . . . 7_556 ?
C2B C3A C3B C1A 6.3(9) . . . . ?
N1 C3A C3B C1A -21.1(4) . . . . ?
C1B C3A C3B C1A 92.4(5) 7_556 . . . ?
C2B C3A C3B N1 27.4(5) . . . . ?
C1B C3A C3B N1 113.5(4) 7_556 . . . ?
C2B C3A C3B C2A -86.8(7) . . . 7_556 ?
N1 C3A C3B C2A -114.2(4) . . . 7_556 ?
C1B C3A C3B C2A -0.6(5) 7_556 . . 7_556 ?
C2B C3A C3B C1B -86.1(7) . . . 7_556 ?
N1 C3A C3B C1B -113.5(4) . . . 7_556 ?
C1B C1A C3B C3A -5.3(8) . . . . ?
N1 C1A C3B C3A 20.7(4) . . . . ?
C2B C1A C3B C3A -92.0(5) 7_556 . . . ?
C1B C1A C3B N1 -26.0(4) . . . . ?
C2B C1A C3B N1 -112.8(4) 7_556 . . . ?
C1B C1A C3B C2A 86.5(6) . . . 7_556 ?
N1 C1A C3B C2A 112.5(4) . . . 7_556 ?
C2B C1A C3B C2A -0.3(4) 7_556 . . 7_556 ?
C1B C1A C3B C1B 48.2(7) . . . 7_556 ?
N1 C1A C3B C1B 74.2(4) . . . 7_556 ?
C2B C1A C3B C1B -38.5(5) 7_556 . . 7_556 ?
C1B N1 C3B C3A -135.7(4) . . . . ?
C1A N1 C3B C3A -158.1(5) . . . . ?
C2B N1 C3B C3A -20.0(5) . . . . ?
C2A N1 C3B C3A -81.0(7) . . . . ?
C3A N1 C3B C1A 158.1(5) . . . . ?
C1B N1 C3B C1A 22.4(4) . . . . ?
C2B N1 C3B C1A 138.1(4) . . . . ?
C2A N1 C3B C1A 77.1(7) . . . . ?
C3A N1 C3B C2A 77.3(6) . . . 7_556 ?
C1B N1 C3B C2A -58.4(6) . . . 7_556 ?
C1A N1 C3B C2A -80.8(6) . . . 7_556 ?
C2B N1 C3B C2A 57.3(6) . . . 7_556 ?
C2A N1 C3B C2A -3.7(11) . . . 7_556 ?
C3A N1 C3B C1B 44.7(3) . . . 7_556 ?
C1B N1 C3B C1B -91.0(4) . . . 7_556 ?
C1A N1 C3B C1B -113.4(4) . . . 7_556 ?
C2B N1 C3B C1B 24.7(4) . . . 7_556 ?
C2A N1 C3B C1B -36.3(7) . . . 7_556 ?
C5 N2 C4 C4 58.5(3) 2_655 . . 2_655 ?
C6 N2 C4 C4 -58.8(3) . . . 2_655 ?
C5 N2 C6 C5 -58.4(3) 2_655 . . . ?
C4 N2 C6 C5 57.9(3) . . . . ?
N2 C5 C6 N2 1.2(3) 2_655 . . . ?

_diffrn_measured_fraction_theta_max 0.970
_diffrn_reflns_theta_full        24.75
_diffrn_measured_fraction_theta_full 0.970
_refine_diff_density_max         0.151
_refine_diff_density_min         -0.127
_refine_diff_density_rms         0.033
#===END

data_CCDC634614
_database_code_depnum_ccdc_archive 'CCDC 634614'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H12 N2, 6(H2 O)'
_chemical_formula_sum            'C6 H24 N2 O6'
_chemical_formula_weight         220.27

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           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.5426(10)
_cell_length_b                   12.6014(9)
_cell_length_c                   17.2689(13)
_cell_angle_alpha                99.590(6)
_cell_angle_beta                 108.320(6)
_cell_angle_gamma                99.448(6)
_cell_volume                     2485.6(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    18481
_cell_measurement_theta_min      1.28
_cell_measurement_theta_max      23.22

_exptl_crystal_description       Fragment
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             976
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9515
_exptl_absorpt_correction_T_max  0.9871

_exptl_absorpt_process_details   '(R.H. Blessing, Acta Cryst. (1995) A51 33-38)'

_exptl_special_details           
;
?
;
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16189
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.28
_diffrn_reflns_theta_max         22.75
_reflns_number_total             4779
_reflns_number_gt                3680
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Carbon atoms at DABCO N4--N44 were 1:1 disordered.Hydrogen atoms at O1,
O2, O4, O6, O7, O12, O16 and O17 were found and refined with bond
restraints (d=0.85 angs.). The positions of the other hydrogen atoms at
water molecules O1-O24 were disordered over three to four positions with
occupancy factors between 0.25 and 1.0. This disorder is caused by
the water molecules O10 and O18, which are each connected by an inversion
centre, leading to a completely disordered hydrogen bond network between
the water molecules. This disorder could not be reliably refined and
these hydrogen atoms were omitted (an attempt to refine the disordered
positions failed after several days).
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0521P)²+1.2831P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4779
_refine_ls_number_parameters     591
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0519
_refine_ls_wR_factor_ref         0.1302
_refine_ls_wR_factor_gt          0.1201
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.5968(2) 0.2617(2) 0.05170(16) 0.0385(6) Uani 1 1 d D . .
O2 O 0.39935(19) 0.2576(2) -0.08149(14) 0.0394(6) Uani 1 1 d D . .
O3 O 0.2157(6) 0.3350(4) -0.0536(3) 0.0463(11) Uani 1 1 d . . .
O4 O 0.2294(2) 0.55145(19) -0.07231(15) 0.0387(6) Uani 1 1 d D . .
O5 O 0.1006(5) 0.3160(6) 0.0618(4) 0.0691(14) Uani 1 1 d . . .
O6 O 0.1483(2) 0.1847(2) 0.17232(16) 0.0392(6) Uani 1 1 d D . .
O7 O 0.34980(19) 0.3054(2) 0.30498(14) 0.0410(6) Uani 1 1 d D . .
O8 O 0.5288(6) 0.1958(4) 0.3184(3) 0.0506(11) Uani 1 1 d . . .
O9 O 0.6442(6) 0.2134(6) 0.2052(4) 0.0828(17) Uani 1 1 d . . .
O10 O 0.0845(8) 0.5959(10) 0.0185(7) 0.0497(18) Uani 1 1 d . . .
O11 O 0.1706(2) 0.7444(2) 0.17308(16) 0.0558(7) Uani 1 1 d . . .
O12 O 0.3609(2) 0.8217(2) 0.32311(16) 0.0419(6) Uani 1 1 d D A .
O13 O 0.5366(3) 0.9675(2) 0.30280(17) 0.0566(8) Uani 1 1 d . . .
O14 O 0.6915(8) 0.8968(10) 0.2351(7) 0.0444(15) Uani 1 1 d . . .
O15 O 0.8714(5) 0.7930(6) 0.3035(4) 0.0679(13) Uani 1 1 d . . .
O16 O 0.8981(2) 0.7358(2) 0.45188(17) 0.0410(6) Uani 1 1 d D . .
O17 O 0.77460(19) 0.55179(17) 0.48503(14) 0.0414(5) Uani 1 1 d D . .
O18 O 0.5844(8) 0.5970(10) 0.5254(6) 0.0446(15) Uani 1 1 d . . .
O19 O 0.4164(5) 0.7007(6) 0.4397(4) 0.0740(14) Uani 1 1 d . . .
O20 O 0.0288(6) 0.1840(5) -0.1800(3) 0.0512(11) Uani 1 1 d . . .
O21 O 0.0309(3) -0.0371(2) -0.1873(2) 0.0590(8) Uani 1 1 d . . .
O22 O 0.1802(9) -0.1069(11) -0.2676(7) 0.0493(15) Uani 1 1 d . . .
O23 O 0.1218(2) -0.2152(2) -0.43238(18) 0.0628(8) Uani 1 1 d . . .
O24 O 0.2884(6) -0.3211(5) -0.4534(3) 0.0511(11) Uani 1 1 d . . .
N1 N 0.6789(2) 0.09234(19) -0.00972(14) 0.0337(6) Uani 1 1 d . . .
N11 N 0.7720(2) -0.0411(2) -0.08101(15) 0.0368(6) Uani 1 1 d . . .
N2 N 0.4867(2) 0.3975(2) -0.16336(14) 0.0345(6) Uani 1 1 d . . .
N22 N 0.5723(2) 0.5343(2) -0.23434(17) 0.0375(7) Uani 1 1 d . . .
N3 N 0.0793(2) 0.5376(2) -0.22769(15) 0.0380(7) Uani 1 1 d . . .
N33 N -0.0736(2) 0.5360(2) -0.36725(15) 0.0353(6) Uani 1 1 d . . .
N4 N 0.2780(2) 0.9705(2) 0.40670(16) 0.0394(7) Uani 1 1 d . . .
N44 N 0.1821(2) 1.1029(2) 0.47520(16) 0.0380(6) Uani 1 1 d . . .
C1 C 0.6242(4) 0.0689(3) -0.1010(2) 0.0502(10) Uani 1 1 d . . .
H1A H 0.6324 0.1388 -0.1199 0.060 Uiso 1 1 calc R . .
H1B H 0.5408 0.0358 -0.1173 0.060 Uiso 1 1 calc R . .
C2 C 0.6795(3) -0.0106(3) -0.1438(2) 0.0516(11) Uani 1 1 d . . .
H2A H 0.6200 -0.0780 -0.1786 0.062 Uiso 1 1 calc R . .
H2B H 0.7117 0.0249 -0.1811 0.062 Uiso 1 1 calc R . .
C3 C 0.6668(3) -0.0118(3) 0.0173(2) 0.0459(9) Uani 1 1 d . . .
H3A H 0.5839 -0.0460 0.0025 0.055 Uiso 1 1 calc R . .
H3B H 0.7042 0.0030 0.0790 0.055 Uiso 1 1 calc R . .
C4 C 0.7232(3) -0.0921(3) -0.0254(2) 0.0528(10) Uani 1 1 d . . .
H4A H 0.7851 -0.1116 0.0179 0.063 Uiso 1 1 calc R . .
H4B H 0.6647 -0.1611 -0.0583 0.063 Uiso 1 1 calc R . .
C5 C 0.8031(5) 0.1402(4) 0.0128(3) 0.0472(14) Uani 1 1 d . . .
H5A H 0.8419 0.1555 0.0744 0.057 Uiso 1 1 calc R . .
H5B H 0.8138 0.2110 -0.0046 0.057 Uiso 1 1 calc R . .
C6 C 0.8576(3) 0.0599(3) -0.0304(2) 0.0475(9) Uani 1 1 d . . .
H6A H 0.8916 0.0960 -0.0667 0.057 Uiso 1 1 calc R . .
H6B H 0.9205 0.0411 0.0125 0.057 Uiso 1 1 calc R . .
C7 C 0.5986(3) 0.3796(3) -0.1648(3) 0.0511(11) Uani 1 1 d . . .
H7A H 0.5892 0.3022 -0.1940 0.061 Uiso 1 1 calc R . .
H7B H 0.6528 0.3919 -0.1066 0.061 Uiso 1 1 calc R . .
C8 C 0.6487(3) 0.4593(3) -0.2102(2) 0.0491(9) Uani 1 1 d . . .
H8A H 0.7264 0.5030 -0.1728 0.059 Uiso 1 1 calc R . .
H8B H 0.6563 0.4164 -0.2609 0.059 Uiso 1 1 calc R . .
C9 C 0.4104(4) 0.3824(4) -0.2498(3) 0.0644(16) Uani 1 1 d . . .
H9A H 0.3331 0.3912 -0.2506 0.077 Uiso 1 1 calc R . .
H9B H 0.4019 0.3067 -0.2817 0.077 Uiso 1 1 calc R . .
C10 C 0.4598(3) 0.4677(3) -0.2914(2) 0.0559(10) Uani 1 1 d . . .
H10A H 0.4676 0.4289 -0.3434 0.067 Uiso 1 1 calc R . .
H10B H 0.4061 0.5165 -0.3068 0.067 Uiso 1 1 calc R . .
C11 C 0.5041(4) 0.5105(3) -0.1170(3) 0.0583(12) Uani 1 1 d . . .
H11A H 0.5553 0.5204 -0.0583 0.070 Uiso 1 1 calc R . .
H11B H 0.4291 0.5251 -0.1166 0.070 Uiso 1 1 calc R . .
C12 C 0.5591(3) 0.5929(3) -0.1586(2) 0.0487(9) Uani 1 1 d . . .
H12A H 0.5097 0.6456 -0.1732 0.058 Uiso 1 1 calc R . .
H12B H 0.6356 0.6358 -0.1184 0.058 Uiso 1 1 calc R . .
C13 C -0.0240(3) 0.4498(3) -0.2460(2) 0.0582(11) Uani 1 1 d . . .
H13A H -0.0563 0.4627 -0.2007 0.070 Uiso 1 1 calc R . .
H13B H -0.0030 0.3772 -0.2484 0.070 Uiso 1 1 calc R . .
C14 C -0.1153(3) 0.4487(3) -0.3306(2) 0.0588(11) Uani 1 1 d . . .
H14A H -0.1328 0.3759 -0.3697 0.071 Uiso 1 1 calc R . .
H14B H -0.1874 0.4597 -0.3219 0.071 Uiso 1 1 calc R . .
C15 C 0.1247(3) 0.5167(3) -0.2966(2) 0.0481(9) Uani 1 1 d . . .
H15A H 0.1458 0.4442 -0.3004 0.058 Uiso 1 1 calc R . .
H15B H 0.1951 0.5746 -0.2851 0.058 Uiso 1 1 calc R . .
C16 C 0.0330(3) 0.5173(3) -0.3805(2) 0.0477(9) Uani 1 1 d . . .
H16A H 0.0632 0.5766 -0.4045 0.057 Uiso 1 1 calc R . .
H16B H 0.0158 0.4457 -0.4209 0.057 Uiso 1 1 calc R . .
C17 C 0.0472(4) 0.6444(4) -0.2240(3) 0.0421(11) Uani 1 1 d . . .
H17A H 0.1162 0.7040 -0.2126 0.051 Uiso 1 1 calc R . .
H17B H 0.0169 0.6598 -0.1779 0.051 Uiso 1 1 calc R . .
C18 C -0.0456(3) 0.6428(3) -0.3081(2) 0.0470(9) Uani 1 1 d . . .
H18A H -0.1162 0.6567 -0.2982 0.056 Uiso 1 1 calc R . .
H18B H -0.0170 0.7024 -0.3324 0.056 Uiso 1 1 calc R . .
C19 C 0.1551(9) 0.9128(10) 0.3937(7) 0.049(3) Uani 0.50 1 d P A 1
H19A H 0.1108 0.8849 0.3330 0.059 Uiso 0.50 1 calc PR A 1
H19B H 0.1564 0.8488 0.4200 0.059 Uiso 0.50 1 calc PR A 1
C20 C 0.0967(8) 0.9919(8) 0.4320(5) 0.047(2) Uani 0.50 1 d P A 1
H20A H 0.0691 0.9611 0.4732 0.057 Uiso 0.50 1 calc PR A 1
H20B H 0.0292 1.0020 0.3876 0.057 Uiso 0.50 1 calc PR A 1
C21 C 0.2652(16) 1.0594(15) 0.3687(10) 0.075(6) Uani 0.50 1 d P A 1
H21A H 0.2191 1.0302 0.3083 0.090 Uiso 0.50 1 calc PR A 1
H21B H 0.3424 1.0998 0.3731 0.090 Uiso 0.50 1 calc PR A 1
C22 C 0.2081(17) 1.1394(16) 0.4058(13) 0.065(6) Uani 0.50 1 d P A 1
H22A H 0.2599 1.2142 0.4264 0.079 Uiso 0.50 1 calc PR A 1
H22B H 0.1359 1.1430 0.3625 0.079 Uiso 0.50 1 calc PR A 1
C23 C 0.3378(8) 1.0033(8) 0.4968(5) 0.058(2) Uani 0.50 1 d P A 1
H23A H 0.4195 1.0398 0.5095 0.070 Uiso 0.50 1 calc PR A 1
H23B H 0.3360 0.9372 0.5207 0.070 Uiso 0.50 1 calc PR A 1
C24 C 0.2788(8) 1.0835(8) 0.5362(5) 0.055(2) Uani 0.50 1 d P A 1
H24A H 0.2532 1.0524 0.5781 0.066 Uiso 0.50 1 calc PR A 1
H24B H 0.3353 1.1547 0.5658 0.066 Uiso 0.50 1 calc PR A 1
C19A C 0.2010(12) 0.9141(10) 0.4372(9) 0.076(4) Uani 0.50 1 d P A 2
H19C H 0.2425 0.8748 0.4778 0.092 Uiso 0.50 1 calc PR A 2
H19D H 0.1403 0.8581 0.3902 0.092 Uiso 0.50 1 calc PR A 2
C20A C 0.1432(11) 0.9936(8) 0.4809(8) 0.074(4) Uani 0.50 1 d P A 2
H20C H 0.0583 0.9701 0.4536 0.088 Uiso 0.50 1 calc PR A 2
H20D H 0.1632 0.9905 0.5406 0.088 Uiso 0.50 1 calc PR A 2
C21A C 0.2241(17) 1.0329(16) 0.3468(11) 0.084(7) Uani 0.50 1 d P A 2
H21C H 0.1648 0.9819 0.2961 0.101 Uiso 0.50 1 calc PR A 2
H21D H 0.2829 1.0755 0.3296 0.101 Uiso 0.50 1 calc PR A 2
C22A C 0.1663(19) 1.115(2) 0.3929(15) 0.085(8) Uani 0.50 1 d P A 2
H22C H 0.2010 1.1922 0.3948 0.102 Uiso 0.50 1 calc PR A 2
H22D H 0.0827 1.0994 0.3603 0.102 Uiso 0.50 1 calc PR A 2
C23A C 0.3673(9) 1.0567(9) 0.4769(7) 0.064(3) Uani 0.50 1 d P A 2
H23C H 0.4207 1.0985 0.4550 0.076 Uiso 0.50 1 calc PR A 2
H23D H 0.4128 1.0206 0.5183 0.076 Uiso 0.50 1 calc PR A 2
C24A C 0.3124(10) 1.1383(11) 0.5212(8) 0.050(3) Uani 0.50 1 d P A 2
H24C H 0.3314 1.1352 0.5808 0.060 Uiso 0.50 1 calc PR A 2
H24D H 0.3422 1.2149 0.5187 0.060 Uiso 0.50 1 calc PR A 2
H11 H 0.624(3) 0.209(2) 0.033(2) 0.063(12) Uiso 1 1 d D . .
H21 H 0.424(3) 0.303(3) -0.109(2) 0.095(14) Uiso 1 1 d D . .
H41 H 0.188(3) 0.547(3) -0.1241(13) 0.071(12) Uiso 1 1 d D . .
H61 H 0.175(3) 0.137(3) 0.146(2) 0.071(13) Uiso 1 1 d D . .
H71 H 0.375(3) 0.358(2) 0.282(2) 0.079(13) Uiso 1 1 d D . .
H121 H 0.337(3) 0.871(3) 0.349(2) 0.074(13) Uiso 1 1 d D . .
H161 H 0.870(3) 0.787(2) 0.473(2) 0.064(12) Uiso 1 1 d D . .
H171 H 0.824(3) 0.554(3) 0.5343(15) 0.080(13) Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 N1 2.719(4) . ?
O1 O9 2.724(7) . ?
O1 O2 2.786(3) . ?
O1 O4 2.823(3) 2_665 ?
O1 H11 0.859(19) . ?
O2 N2 2.735(3) . ?
O2 O3 2.787(6) . ?
O2 O14 2.788(12) 2_665 ?
O2 H21 0.88(4) . ?
O3 O4 2.784(5) . ?
O3 O20 2.795(13) . ?
O3 O5 2.821(7) . ?
O4 N3 2.708(3) . ?
O4 O10 2.813(11) . ?
O4 O1 2.823(3) 2_665 ?
O4 H41 0.871(18) . ?
O5 O6 2.720(7) . ?
O5 O10 2.808(11) 2_565 ?
O6 N11 2.719(4) 2_655 ?
O6 O21 2.780(4) 2 ?
O6 O7 2.809(3) . ?
O6 H61 0.87(4) . ?
O7 N22 2.729(3) 2_665 ?
O7 O18 2.779(11) 2_666 ?
O7 O8 2.793(6) . ?
O7 H71 0.894(19) . ?
O8 O24 2.722(12) 2_655 ?
O8 O9 2.789(7) . ?
O8 O13 2.865(6) 1_545 ?
O9 O22 2.788(12) 2_655 ?
O10 O11 2.766(12) . ?
O10 O10 2.77(2) 2_565 ?
O10 O5 2.808(11) 2_565 ?
O11 O12 2.805(4) . ?
O11 O20 2.824(7) 2_565 ?
O12 O19 2.713(7) . ?
O12 N4 2.714(4) . ?
O12 O13 2.779(4) . ?
O12 H121 0.85(4) . ?
O13 O14 2.754(11) . ?
O13 O8 2.865(6) 1_565 ?
O14 O22 2.73(2) 2_665 ?
O14 O2 2.788(12) 2_665 ?
O14 O15 2.829(10) . ?
O15 O16 2.713(6) . ?
O15 O20 2.822(7) 2_665 ?
O16 N44 2.710(4) 2_676 ?
O16 O23 2.783(4) 1_666 ?
O16 O17 2.815(3) . ?
O16 H161 0.867(19) . ?
O17 N33 2.723(3) 1_656 ?
O17 O24 2.796(6) 2_655 ?
O17 O18 2.804(11) . ?
O17 H171 0.874(19) . ?
O18 O18 2.77(2) 2_666 ?
O18 O7 2.779(11) 2_666 ?
O18 O19 2.815(10) . ?
O19 O24 2.819(6) 1_566 ?
O20 O21 2.774(6) . ?
O20 O15 2.822(7) 2_665 ?
O20 O11 2.824(7) 2_565 ?
O21 O6 2.780(4) 2 ?
O21 O22 2.823(12) . ?
O22 O14 2.73(2) 2_665 ?
O22 O23 2.751(12) . ?
O22 O9 2.788(12) 2_655 ?
O23 O24 2.740(6) . ?
O23 O16 2.783(4) 1_444 ?
O24 O8 2.722(12) 2_655 ?
O24 O17 2.796(6) 2_655 ?
O24 O19 2.819(6) 1_544 ?
N1 C1 1.464(4) . ?
N1 C3 1.466(4) . ?
N1 C5 1.475(6) . ?
N11 C6 1.459(4) . ?
N11 C4 1.469(4) . ?
N11 C2 1.472(4) . ?
N11 O6 2.719(4) 2_655 ?
N2 C11 1.457(4) . ?
N2 C9 1.458(5) . ?
N2 C7 1.464(5) . ?
N22 C10 1.459(4) . ?
N22 C12 1.463(4) . ?
N22 C8 1.469(4) . ?
N22 O7 2.729(3) 2_665 ?
N3 C17 1.465(5) . ?
N3 C13 1.469(4) . ?
N3 C15 1.477(4) . ?
N33 C14 1.461(4) . ?
N33 C18 1.462(4) . ?
N33 C16 1.473(5) . ?
N33 O17 2.723(3) 1_454 ?
N4 C19A 1.391(13) . ?
N4 C21 1.396(16) . ?
N4 C23 1.450(9) . ?
N4 C21A 1.467(18) . ?
N4 C23A 1.488(11) . ?
N4 C19 1.522(12) . ?
N44 C22A 1.41(2) . ?
N44 C20A 1.414(10) . ?
N44 C24 1.421(9) . ?
N44 C22 1.46(2) . ?
N44 C20 1.522(10) . ?
N44 C24A 1.526(13) . ?
N44 O16 2.710(4) 2_676 ?
C1 C2 1.527(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.544(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.530(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.545(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.542(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.547(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.544(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.543(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.544(6) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.513(16) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.50(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.538(13) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C19A C20A 1.558(16) . ?
C19A H19C 0.9900 . ?
C19A H19D 0.9900 . ?
C20A H20C 0.9900 . ?
C20A H20D 0.9900 . ?
C21A C22A 1.60(4) . ?
C21A H21C 0.9900 . ?
C21A H21D 0.9900 . ?
C22A H22C 0.9900 . ?
C22A H22D 0.9900 . ?
C23A C24A 1.555(15) . ?
C23A H23C 0.9900 . ?
C23A H23D 0.9900 . ?
C24A H24C 0.9900 . ?
C24A H24D 0.9900 . ?

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
N1 O1 O9 93.20(16) . . ?
N1 O1 O2 103.48(11) . . ?
O9 O1 O2 136.42(17) . . ?
N1 O1 O4 102.31(11) . 2_665 ?
O9 O1 O4 105.80(19) . 2_665 ?
O2 O1 O4 109.35(11) . 2_665 ?
O9 O1 H11 93(2) . . ?
O2 O1 H11 105(2) . . ?
O4 O1 H11 101(2) 2_665 . ?
N2 O2 O1 101.57(10) . . ?
N2 O2 O3 105.95(14) . . ?
O1 O2 O3 121.08(16) . . ?
N2 O2 O14 86.4(3) . 2_665 ?
O1 O2 O14 126.0(2) . 2_665 ?
O3 O2 O14 106.9(2) . 2_665 ?
O1 O2 H21 104(3) . . ?
O3 O2 H21 104(3) . . ?
O14 O2 H21 85(3) 2_665 . ?
O4 O3 O2 110.2(2) . . ?
O4 O3 O20 112.8(3) . . ?
O2 O3 O20 100.6(2) . . ?
O4 O3 O5 105.2(2) . . ?
O2 O3 O5 134.9(2) . . ?
O20 O3 O5 90.2(3) . . ?
N3 O4 O3 106.00(16) . . ?
N3 O4 O10 98.1(2) . . ?
O3 O4 O10 94.0(3) . . ?
N3 O4 O1 101.85(10) . 2_665 ?
O3 O4 O1 137.64(17) . 2_665 ?
O10 O4 O1 113.0(3) . 2_665 ?
O3 O4 H41 107(2) . . ?
O10 O4 H41 104(2) . . ?
O1 O4 H41 98(2) 2_665 . ?
O6 O5 O10 138.2(3) . 2_565 ?
O6 O5 O3 122.2(2) . . ?
O10 O5 O3 96.5(3) 2_565 . ?
N11 O6 O5 96.72(15) 2_655 . ?
N11 O6 O21 99.59(12) 2_655 2 ?
O5 O6 O21 119.83(18) . 2 ?
N11 O6 O7 102.95(11) 2_655 . ?
O5 O6 O7 105.99(18) . . ?
O21 O6 O7 125.45(12) 2 . ?
O5 O6 H61 100(2) . . ?
O21 O6 H61 98(2) 2 . ?
O7 O6 H61 101(2) . . ?
N22 O7 O18 105.9(3) 2_665 2_666 ?
N22 O7 O8 97.34(15) 2_665 . ?
O18 O7 O8 96.9(2) 2_666 . ?
N22 O7 O6 101.05(10) 2_665 . ?
O18 O7 O6 138.2(2) 2_666 . ?
O8 O7 O6 110.81(15) . . ?
O18 O7 H71 106(2) 2_666 . ?
O8 O7 H71 97(2) . . ?
O6 O7 H71 101(2) . . ?
O24 O8 O9 94.3(3) 2_655 . ?
O24 O8 O7 106.1(2) 2_655 . ?
O9 O8 O7 117.1(3) . . ?
O24 O8 O13 109.3(3) 2_655 1_545 ?
O9 O8 O13 90.2(2) . 1_545 ?
O7 O8 O13 132.9(2) . 1_545 ?
O1 O9 O22 121.8(3) . 2_655 ?
O1 O9 O8 136.1(3) . . ?
O22 O9 O8 100.5(4) 2_655 . ?
O11 O10 O10 122.9(6) . 2_565 ?
O11 O10 O5 99.3(4) . 2_565 ?
O10 O10 O5 84.4(4) 2_565 2_565 ?
O11 O10 O4 120.8(4) . . ?
O10 O10 O4 107.5(6) 2_565 . ?
O5 O10 O4 115.5(4) 2_565 . ?
O10 O11 O12 144.1(2) . . ?
O10 O11 O20 101.3(2) . 2_565 ?
O12 O11 O20 113.81(16) . 2_565 ?
O19 O12 N4 98.37(15) . . ?
O19 O12 O13 119.00(17) . . ?
N4 O12 O13 98.89(12) . . ?
O19 O12 O11 122.89(19) . . ?
N4 O12 O11 99.35(12) . . ?
O13 O12 O11 111.08(12) . . ?
O19 O12 H121 100(3) . . ?
O13 O12 H121 97(3) . . ?
O11 O12 H121 100(3) . . ?
O14 O13 O12 122.6(3) . . ?
O14 O13 O8 117.1(3) . 1_565 ?
O12 O13 O8 118.91(17) . 1_565 ?
O22 O14 O13 92.7(6) 2_665 . ?
O22 O14 O2 126.9(7) 2_665 2_665 ?
O13 O14 O2 117.1(3) . 2_665 ?
O22 O14 O15 98.9(5) 2_665 . ?
O13 O14 O15 129.4(4) . . ?
O2 O14 O15 94.2(4) 2_665 . ?
O16 O15 O20 145.2(2) . 2_665 ?
O16 O15 O14 119.9(3) . . ?
O20 O15 O14 94.4(3) 2_665 . ?
N44 O16 O15 99.03(15) 2_676 . ?
N44 O16 O23 98.93(12) 2_676 1_666 ?
O15 O16 O23 116.94(16) . 1_666 ?
N44 O16 O17 99.16(11) 2_676 . ?
O15 O16 O17 129.07(18) . . ?
O23 O16 O17 106.52(11) 1_666 . ?
O15 O16 H161 98(2) . . ?
O23 O16 H161 101(2) 1_666 . ?
O17 O16 H161 99(2) . . ?
N33 O17 O24 84.41(15) 1_656 2_655 ?
N33 O17 O18 104.1(2) 1_656 . ?
O24 O17 O18 97.8(3) 2_655 . ?
N33 O17 O16 101.67(10) 1_656 . ?
O24 O17 O16 146.38(14) 2_655 . ?
O18 O17 O16 112.3(3) . . ?
O24 O17 H171 90(3) 2_655 . ?
O18 O17 H171 102(3) . . ?
O16 O17 H171 98(3) . . ?
O18 O18 O7 113.1(6) 2_666 2_666 ?
O18 O18 O17 108.5(6) 2_666 . ?
O7 O18 O17 110.9(3) 2_666 . ?
O18 O18 O19 88.6(4) 2_666 . ?
O7 O18 O19 106.5(4) 2_666 . ?
O17 O18 O19 127.4(4) . . ?
O12 O19 O18 145.2(3) . . ?
O12 O19 O24 120.0(2) . 1_566 ?
O18 O19 O24 94.0(3) . 1_566 ?
O21 O20 O3 115.4(3) . . ?
O21 O20 O15 96.2(2) . 2_665 ?
O3 O20 O15 92.8(3) . 2_665 ?
O21 O20 O11 118.8(2) . 2_565 ?
O3 O20 O11 106.1(2) . 2_565 ?
O15 O20 O11 125.2(3) 2_665 2_565 ?
O20 O21 O6 121.76(18) . 2 ?
O20 O21 O22 112.2(3) . . ?
O6 O21 O22 122.4(3) 2 . ?
O14 O22 O23 111.5(6) 2_665 . ?
O14 O22 O9 99.7(5) 2_665 2_655 ?
O23 O22 O9 95.1(4) . 2_655 ?
O14 O22 O21 92.9(6) 2_665 . ?
O23 O22 O21 127.4(4) . . ?
O9 O22 O21 126.8(5) 2_655 . ?
O24 O23 O22 111.0(3) . . ?
O24 O23 O16 123.48(18) . 1_444 ?
O22 O23 O16 123.0(3) . 1_444 ?
O8 O24 O23 98.8(2) 2_655 . ?
O8 O24 O17 122.9(3) 2_655 2_655 ?
O23 O24 O17 114.9(2) . 2_655 ?
O8 O24 O19 91.3(3) 2_655 1_544 ?
O23 O24 O19 129.5(3) . 1_544 ?
O17 O24 O19 99.6(2) 2_655 1_544 ?
C1 N1 C3 108.9(3) . . ?
C1 N1 C5 108.4(3) . . ?
C3 N1 C5 108.0(3) . . ?
C1 N1 O1 105.67(19) . . ?
C3 N1 O1 121.0(2) . . ?
C5 N1 O1 104.3(2) . . ?
C6 N11 C4 108.0(3) . . ?
C6 N11 C2 108.2(3) . . ?
C4 N11 C2 108.8(3) . . ?
C6 N11 O6 114.46(19) . 2_655 ?
C4 N11 O6 112.5(2) . 2_655 ?
C2 N11 O6 104.70(19) . 2_655 ?
C11 N2 C9 109.8(3) . . ?
C11 N2 C7 108.3(3) . . ?
C9 N2 C7 108.0(3) . . ?
C11 N2 O2 107.9(2) . . ?
C9 N2 O2 112.4(2) . . ?
C7 N2 O2 110.39(19) . . ?
C10 N22 C12 109.0(3) . . ?
C10 N22 C8 108.3(3) . . ?
C12 N22 C8 108.2(3) . . ?
C10 N22 O7 109.73(19) . 2_665 ?
C12 N22 O7 105.75(19) . 2_665 ?
C8 N22 O7 115.7(2) . 2_665 ?
C17 N3 C13 109.2(3) . . ?
C17 N3 C15 108.7(3) . . ?
C13 N3 C15 108.4(3) . . ?
C17 N3 O4 105.5(2) . . ?
C13 N3 O4 109.35(18) . . ?
C15 N3 O4 115.57(19) . . ?
C14 N33 C18 109.0(3) . . ?
C14 N33 C16 108.6(3) . . ?
C18 N33 C16 108.3(3) . . ?
C14 N33 O17 115.19(18) . 1_454 ?
C18 N33 O17 107.00(19) . 1_454 ?
C16 N33 O17 108.65(19) . 1_454 ?
C19A N4 C21 127.3(9) . . ?
C19A N4 C23 77.1(7) . . ?
C21 N4 C23 113.8(8) . . ?
C19A N4 C21A 113.1(10) . . ?
C23 N4 C21A 131.2(8) . . ?
C19A N4 C23A 109.2(7) . . ?
C21 N4 C23A 83.2(9) . . ?
C21A N4 C23A 104.1(9) . . ?
C21 N4 C19 104.3(9) . . ?
C23 N4 C19 105.8(6) . . ?
C21A N4 C19 85.5(9) . . ?
C23A N4 C19 132.4(6) . . ?
C19A N4 O12 108.9(5) . . ?
C21 N4 O12 110.9(7) . . ?
C23 N4 O12 115.0(4) . . ?
C21A N4 O12 106.5(8) . . ?
C23A N4 O12 115.1(4) . . ?
C19 N4 O12 106.0(5) . . ?
C22A N44 C20A 114.4(11) . . ?
C22A N44 C24 130.1(11) . . ?
C20A N44 C24 76.4(7) . . ?
C20A N44 C22 128.2(10) . . ?
C24 N44 C22 113.8(9) . . ?
C22A N44 C20 84.5(10) . . ?
C24 N44 C20 107.6(6) . . ?
C22 N44 C20 102.8(9) . . ?
C22A N44 C24A 104.7(10) . . ?
C20A N44 C24A 108.4(8) . . ?
C22 N44 C24A 84.8(9) . . ?
C20 N44 C24A 134.3(6) . . ?
C22A N44 O16 107.0(11) . 2_676 ?
C20A N44 O16 117.5(4) . 2_676 ?
C24 N44 O16 109.5(4) . 2_676 ?
C22 N44 O16 106.6(9) . 2_676 ?
C20 N44 O16 116.6(4) . 2_676 ?
C24A N44 O16 103.5(4) . 2_676 ?
N1 C1 C2 110.7(3) . . ?
N1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
N11 C2 C1 110.6(3) . . ?
N11 C2 H2A 109.5 . . ?
C1 C2 H2A 109.5 . . ?
N11 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
N1 C3 C4 110.2(3) . . ?
N1 C3 H3A 109.6 . . ?
C4 C3 H3A 109.6 . . ?
N1 C3 H3B 109.6 . . ?
C4 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
N11 C4 C3 110.4(3) . . ?
N11 C4 H4A 109.6 . . ?
C3 C4 H4A 109.6 . . ?
N11 C4 H4B 109.6 . . ?
C3 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
N1 C5 C6 110.2(4) . . ?
N1 C5 H5A 109.6 . . ?
C6 C5 H5A 109.6 . . ?
N1 C5 H5B 109.6 . . ?
C6 C5 H5B 109.6 . . ?
H5A C5 H5B 108.1 . . ?
N11 C6 C5 111.0(3) . . ?
N11 C6 H6A 109.4 . . ?
C5 C6 H6A 109.4 . . ?
N11 C6 H6B 109.4 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
N2 C7 C8 110.5(3) . . ?
N2 C7 H7A 109.6 . . ?
C8 C7 H7A 109.6 . . ?
N2 C7 H7B 109.6 . . ?
C8 C7 H7B 109.6 . . ?
H7A C7 H7B 108.1 . . ?
N22 C8 C7 109.9(3) . . ?
N22 C8 H8A 109.7 . . ?
C7 C8 H8A 109.7 . . ?
N22 C8 H8B 109.7 . . ?
C7 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
N2 C9 C10 110.4(3) . . ?
N2 C9 H9A 109.6 . . ?
C10 C9 H9A 109.6 . . ?
N2 C9 H9B 109.6 . . ?
C10 C9 H9B 109.6 . . ?
H9A C9 H9B 108.1 . . ?
N22 C10 C9 110.4(3) . . ?
N22 C10 H10A 109.6 . . ?
C9 C10 H10A 109.6 . . ?
N22 C10 H10B 109.6 . . ?
C9 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
N2 C11 C12 109.8(3) . . ?
N2 C11 H11A 109.7 . . ?
C12 C11 H11A 109.7 . . ?
N2 C11 H11B 109.7 . . ?
C12 C11 H11B 109.7 . . ?
H11A C11 H11B 108.2 . . ?
N22 C12 C11 110.7(3) . . ?
N22 C12 H12A 109.5 . . ?
C11 C12 H12A 109.5 . . ?
N22 C12 H12B 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
N3 C13 C14 109.9(3) . . ?
N3 C13 H13A 109.7 . . ?
C14 C13 H13A 109.7 . . ?
N3 C13 H13B 109.7 . . ?
C14 C13 H13B 109.7 . . ?
H13A C13 H13B 108.2 . . ?
N33 C14 C13 110.7(3) . . ?
N33 C14 H14A 109.5 . . ?
C13 C14 H14A 109.5 . . ?
N33 C14 H14B 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
N3 C15 C16 110.1(3) . . ?
N3 C15 H15A 109.6 . . ?
C16 C15 H15A 109.6 . . ?
N3 C15 H15B 109.6 . . ?
C16 C15 H15B 109.6 . . ?
H15A C15 H15B 108.2 . . ?
N33 C16 C15 110.2(3) . . ?
N33 C16 H16A 109.6 . . ?
C15 C16 H16A 109.6 . . ?
N33 C16 H16B 109.6 . . ?
C15 C16 H16B 109.6 . . ?
H16A C16 H16B 108.1 . . ?
N3 C17 C18 109.9(3) . . ?
N3 C17 H17A 109.7 . . ?
C18 C17 H17A 109.7 . . ?
N3 C17 H17B 109.7 . . ?
C18 C17 H17B 109.7 . . ?
H17A C17 H17B 108.2 . . ?
N33 C18 C17 110.7(3) . . ?
N33 C18 H18A 109.5 . . ?
C17 C18 H18A 109.5 . . ?
N33 C18 H18B 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
C20 C19 N4 110.5(8) . . ?
C20 C19 H19A 109.6 . . ?
N4 C19 H19A 109.6 . . ?
C20 C19 H19B 109.6 . . ?
N4 C19 H19B 109.6 . . ?
H19A C19 H19B 108.1 . . ?
C19 C20 N44 109.4(7) . . ?
C19 C20 H20A 109.8 . . ?
N44 C20 H20A 109.8 . . ?
C19 C20 H20B 109.8 . . ?
N44 C20 H20B 109.8 . . ?
H20A C20 H20B 108.2 . . ?
N4 C21 C22 114.1(12) . . ?
N4 C21 H21A 108.7 . . ?
C22 C21 H21A 108.7 . . ?
N4 C21 H21B 108.7 . . ?
C22 C21 H21B 108.7 . . ?
H21A C21 H21B 107.6 . . ?
N44 C22 C21 109.2(13) . . ?
N44 C22 H22A 109.8 . . ?
C21 C22 H22A 109.8 . . ?
N44 C22 H22B 109.8 . . ?
C21 C22 H22B 109.8 . . ?
H22A C22 H22B 108.3 . . ?
N4 C23 C24 109.4(6) . . ?
N4 C23 H23A 109.8 . . ?
C24 C23 H23A 109.8 . . ?
N4 C23 H23B 109.8 . . ?
C24 C23 H23B 109.8 . . ?
H23A C23 H23B 108.2 . . ?
N44 C24 C23 112.1(6) . . ?
N44 C24 H24A 109.2 . . ?
C23 C24 H24A 109.2 . . ?
N44 C24 H24B 109.2 . . ?
C23 C24 H24B 109.2 . . ?
H24A C24 H24B 107.9 . . ?
N4 C19A C20A 111.9(9) . . ?
N4 C19A H19C 109.2 . . ?
C20A C19A H19C 109.2 . . ?
N4 C19A H19D 109.2 . . ?
C20A C19A H19D 109.2 . . ?
H19C C19A H19D 107.9 . . ?
N44 C20A C19A 109.6(8) . . ?
N44 C20A H20C 109.7 . . ?
C19A C20A H20C 109.7 . . ?
N44 C20A H20D 109.7 . . ?
C19A C20A H20D 109.7 . . ?
H20C C20A H20D 108.2 . . ?
N4 C21A C22A 107.2(14) . . ?
N4 C21A H21C 110.3 . . ?
C22A C21A H21C 110.3 . . ?
N4 C21A H21D 110.3 . . ?
C22A C21A H21D 110.3 . . ?
H21C C21A H21D 108.5 . . ?
N44 C22A C21A 111.6(17) . . ?
N44 C22A H22C 109.3 . . ?
C21A C22A H22C 109.3 . . ?
N44 C22A H22D 109.3 . . ?
C21A C22A H22D 109.3 . . ?
H22C C22A H22D 108.0 . . ?
N4 C23A C24A 111.6(8) . . ?
N4 C23A H23C 109.3 . . ?
C24A C23A H23C 109.3 . . ?
N4 C23A H23D 109.3 . . ?
C24A C23A H23D 109.3 . . ?
H23C C23A H23D 108.0 . . ?
N44 C24A C23A 107.1(9) . . ?
N44 C24A H24C 110.3 . . ?
C23A C24A H24C 110.3 . . ?
N44 C24A H24D 110.3 . . ?
C23A C24A H24D 110.3 . . ?
H24C C24A H24D 108.5 . . ?

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
N1 O1 O2 N2 -90.57(12) . . . . ?
O9 O1 O2 N2 159.8(3) . . . . ?
O4 O1 O2 N2 17.89(14) 2_665 . . . ?
N1 O1 O2 O3 152.63(16) . . . . ?
O9 O1 O2 O3 43.0(3) . . . . ?
O4 O1 O2 O3 -98.91(18) 2_665 . . . ?
N1 O1 O2 O14 3.4(3) . . . 2_665 ?
O9 O1 O2 O14 -106.2(4) . . . 2_665 ?
O4 O1 O2 O14 111.9(3) 2_665 . . 2_665 ?
N2 O2 O3 O4 -17.1(2) . . . . ?
O1 O2 O3 O4 97.5(2) . . . . ?
O14 O2 O3 O4 -108.1(3) 2_665 . . . ?
N2 O2 O3 O20 102.2(2) . . . . ?
O1 O2 O3 O20 -143.2(2) . . . . ?
O14 O2 O3 O20 11.1(4) 2_665 . . . ?
N2 O2 O3 O5 -156.8(3) . . . . ?
O1 O2 O3 O5 -42.2(4) . . . . ?
O14 O2 O3 O5 112.2(4) 2_665 . . . ?
O2 O3 O4 N3 100.0(2) . . . . ?
O20 O3 O4 N3 -11.6(3) . . . . ?
O5 O3 O4 N3 -108.4(2) . . . . ?
O2 O3 O4 O10 -160.4(3) . . . . ?
O20 O3 O4 O10 88.1(3) . . . . ?
O5 O3 O4 O10 -8.8(3) . . . . ?
O2 O3 O4 O1 -29.2(3) . . . 2_665 ?
O20 O3 O4 O1 -140.7(3) . . . 2_665 ?
O5 O3 O4 O1 122.5(3) . . . 2_665 ?
O4 O3 O5 O6 -147.0(3) . . . . ?
O2 O3 O5 O6 -6.0(6) . . . . ?
O20 O3 O5 O6 99.2(4) . . . . ?
O4 O3 O5 O10 49.7(4) . . . 2_565 ?
O2 O3 O5 O10 -169.3(4) . . . 2_565 ?
O20 O3 O5 O10 -64.1(4) . . . 2_565 ?
O10 O5 O6 N11 129.2(5) 2_565 . . 2_655 ?
O3 O5 O6 N11 -25.5(3) . . . 2_655 ?
O10 O5 O6 O21 24.0(6) 2_565 . . 2 ?
O3 O5 O6 O21 -130.6(3) . . . 2 ?
O10 O5 O6 O7 -125.3(5) 2_565 . . . ?
O3 O5 O6 O7 80.1(3) . . . . ?
N11 O6 O7 N22 85.53(12) 2_655 . . 2_665 ?
O5 O6 O7 N22 -15.47(17) . . . 2_665 ?
O21 O6 O7 N22 -162.53(15) 2 . . 2_665 ?
N11 O6 O7 O18 -145.0(4) 2_655 . . 2_666 ?
O5 O6 O7 O18 114.0(4) . . . 2_666 ?
O21 O6 O7 O18 -33.0(4) 2 . . 2_666 ?
N11 O6 O7 O8 -16.79(18) 2_655 . . . ?
O5 O6 O7 O8 -117.79(19) . . . . ?
O21 O6 O7 O8 95.15(19) 2 . . . ?
N22 O7 O8 O24 77.5(3) 2_665 . . 2_655 ?
O18 O7 O8 O24 -29.6(4) 2_666 . . 2_655 ?
O6 O7 O8 O24 -177.7(2) . . . 2_655 ?
N22 O7 O8 O9 -26.2(3) 2_665 . . . ?
O18 O7 O8 O9 -133.2(4) 2_666 . . . ?
O6 O7 O8 O9 78.6(3) . . . . ?
N22 O7 O8 O13 -145.0(2) 2_665 . . 1_545 ?
O18 O7 O8 O13 108.0(4) 2_666 . . 1_545 ?
O6 O7 O8 O13 -40.2(3) . . . 1_545 ?
N1 O1 O9 O22 26.8(4) . . . 2_655 ?
O2 O1 O9 O22 140.3(4) . . . 2_655 ?
O4 O1 O9 O22 -76.9(4) 2_665 . . 2_655 ?
N1 O1 O9 O8 -135.0(4) . . . . ?
O2 O1 O9 O8 -21.6(6) . . . . ?
O4 O1 O9 O8 121.3(4) 2_665 . . . ?
O24 O8 O9 O1 -132.2(5) 2_655 . . . ?
O7 O8 O9 O1 -21.7(6) . . . . ?
O13 O8 O9 O1 118.4(4) 1_545 . . . ?
O24 O8 O9 O22 63.4(4) 2_655 . . 2_655 ?
O7 O8 O9 O22 174.0(3) . . . 2_655 ?
O13 O8 O9 O22 -46.0(4) 1_545 . . 2_655 ?
N3 O4 O10 O11 -141.2(4) . . . . ?
O3 O4 O10 O11 111.9(4) . . . . ?
O1 O4 O10 O11 -34.6(5) 2_665 . . . ?
N3 O4 O10 O10 70.4(5) . . . 2_565 ?
O3 O4 O10 O10 -36.4(5) . . . 2_565 ?
O1 O4 O10 O10 177.0(4) 2_665 . . 2_565 ?
N3 O4 O10 O5 -21.7(5) . . . 2_565 ?
O3 O4 O10 O5 -128.5(4) . . . 2_565 ?
O1 O4 O10 O5 84.9(4) 2_665 . . 2_565 ?
O10 O10 O11 O12 105.3(6) 2_565 . . . ?
O5 O10 O11 O12 -165.4(3) 2_565 . . . ?
O4 O10 O11 O12 -38.1(8) . . . . ?
O10 O10 O11 O20 -63.0(7) 2_565 . . 2_565 ?
O5 O10 O11 O20 26.3(4) 2_565 . . 2_565 ?
O4 O10 O11 O20 153.6(4) . . . 2_565 ?
O10 O11 O12 O19 -71.2(5) . . . . ?
O20 O11 O12 O19 96.3(2) 2_565 . . . ?
O10 O11 O12 N4 -177.6(5) . . . . ?
O20 O11 O12 N4 -10.11(19) 2_565 . . . ?
O10 O11 O12 O13 79.0(5) . . . . ?
O20 O11 O12 O13 -113.49(19) 2_565 . . . ?
O19 O12 O13 O14 69.6(3) . . . . ?
N4 O12 O13 O14 174.3(3) . . . . ?
O11 O12 O13 O14 -82.0(3) . . . . ?
O19 O12 O13 O8 -124.1(2) . . . 1_565 ?
N4 O12 O13 O8 -19.3(2) . . . 1_565 ?
O11 O12 O13 O8 84.3(2) . . . 1_565 ?
O12 O13 O14 O22 -173.9(3) . . . 2_665 ?
O8 O13 O14 O22 19.5(5) 1_565 . . 2_665 ?
O12 O13 O14 O2 51.7(5) . . . 2_665 ?
O8 O13 O14 O2 -114.8(4) 1_565 . . 2_665 ?
O12 O13 O14 O15 -70.1(6) . . . . ?
O8 O13 O14 O15 123.4(5) 1_565 . . . ?
O22 O14 O15 O16 105.9(6) 2_665 . . . ?
O13 O14 O15 O16 4.9(7) . . . . ?
O2 O14 O15 O16 -125.8(3) 2_665 . . . ?
O22 O14 O15 O20 -68.1(6) 2_665 . . 2_665 ?
O13 O14 O15 O20 -169.1(5) . . . 2_665 ?
O2 O14 O15 O20 60.2(3) 2_665 . . 2_665 ?
O20 O15 O16 N44 138.9(5) 2_665 . . 2_676 ?
O14 O15 O16 N44 -30.5(4) . . . 2_676 ?
O20 O15 O16 O23 34.0(6) 2_665 . . 1_666 ?
O14 O15 O16 O23 -135.4(3) . . . 1_666 ?
O20 O15 O16 O17 -111.4(5) 2_665 . . . ?
O14 O15 O16 O17 79.1(4) . . . . ?
N44 O16 O17 N33 -92.48(12) 2_676 . . 1_656 ?
O15 O16 O17 N33 157.90(19) . . . 1_656 ?
O23 O16 O17 N33 9.74(14) 1_666 . . 1_656 ?
N44 O16 O17 O24 170.0(3) 2_676 . . 2_655 ?
O15 O16 O17 O24 60.4(4) . . . 2_655 ?
O23 O16 O17 O24 -87.8(3) 1_666 . . 2_655 ?
N44 O16 O17 O18 18.2(2) 2_676 . . . ?
O15 O16 O17 O18 -91.4(3) . . . . ?
O23 O16 O17 O18 120.4(2) 1_666 . . . ?
N33 O17 O18 O18 -100.6(5) 1_656 . . 2_666 ?
O24 O17 O18 O18 -14.4(5) 2_655 . . 2_666 ?
O16 O17 O18 O18 150.2(4) . . . 2_666 ?
N33 O17 O18 O7 24.2(4) 1_656 . . 2_666 ?
O24 O17 O18 O7 110.3(4) 2_655 . . 2_666 ?
O16 O17 O18 O7 -85.0(4) . . . 2_666 ?
N33 O17 O18 O19 156.6(5) 1_656 . . . ?
O24 O17 O18 O19 -117.3(5) 2_655 . . . ?
O16 O17 O18 O19 47.4(6) . . . . ?
N4 O12 O19 O18 -135.7(6) . . . . ?
O13 O12 O19 O18 -30.6(7) . . . . ?
O11 O12 O19 O18 117.4(6) . . . . ?
N4 O12 O19 O24 30.6(3) . . . 1_566 ?
O13 O12 O19 O24 135.7(3) . . . 1_566 ?
O11 O12 O19 O24 -76.3(3) . . . 1_566 ?
O18 O18 O19 O12 -126.2(6) 2_666 . . . ?
O7 O18 O19 O12 120.1(6) 2_666 . . . ?
O17 O18 O19 O12 -13.8(10) . . . . ?
O18 O18 O19 O24 65.7(5) 2_666 . . 1_566 ?
O7 O18 O19 O24 -48.0(4) 2_666 . . 1_566 ?
O17 O18 O19 O24 178.1(5) . . . 1_566 ?
O4 O3 O20 O21 168.00(12) . . . . ?
O2 O3 O20 O21 50.6(3) . . . . ?
O5 O3 O20 O21 -85.3(3) . . . . ?
O4 O3 O20 O15 69.8(3) . . . 2_665 ?
O2 O3 O20 O15 -47.7(3) . . . 2_665 ?
O5 O3 O20 O15 176.43(11) . . . 2_665 ?
O4 O3 O20 O11 -58.2(3) . . . 2_565 ?
O2 O3 O20 O11 -175.64(9) . . . 2_565 ?
O5 O3 O20 O11 48.4(3) . . . 2_565 ?
O3 O20 O21 O6 121.6(3) . . . 2 ?
O15 O20 O21 O6 -142.3(2) 2_665 . . 2 ?
O11 O20 O21 O6 -6.1(3) 2_565 . . 2 ?
O3 O20 O21 O22 -79.4(4) . . . . ?
O15 O20 O21 O22 16.7(4) 2_665 . . . ?
O11 O20 O21 O22 153.0(3) 2_565 . . . ?
O20 O21 O22 O14 22.8(5) . . . 2_665 ?
O6 O21 O22 O14 -178.3(3) 2 . . 2_665 ?
O20 O21 O22 O23 -97.2(6) . . . . ?
O6 O21 O22 O23 61.7(6) 2 . . . ?
O20 O21 O22 O9 127.3(5) . . . 2_655 ?
O6 O21 O22 O9 -73.8(6) 2 . . 2_655 ?
O14 O22 O23 O24 88.6(5) 2_665 . . . ?
O9 O22 O23 O24 -14.0(5) 2_655 . . . ?
O21 O22 O23 O24 -159.6(5) . . . . ?
O14 O22 O23 O16 -109.0(5) 2_665 . . 1_444 ?
O9 O22 O23 O16 148.5(2) 2_655 . . 1_444 ?
O21 O22 O23 O16 2.8(7) . . . 1_444 ?
O22 O23 O24 O8 -24.0(4) . . . 2_655 ?
O16 O23 O24 O8 173.7(2) 1_444 . . 2_655 ?
O22 O23 O24 O17 108.6(4) . . . 2_655 ?
O16 O23 O24 O17 -53.7(3) 1_444 . . 2_655 ?
O22 O23 O24 O19 -123.1(4) . . . 1_544 ?
O16 O23 O24 O19 74.6(4) 1_444 . . 1_544 ?
O9 O1 N1 C1 157.9(3) . . . . ?
O2 O1 N1 C1 18.5(2) . . . . ?
O4 O1 N1 C1 -95.2(2) 2_665 . . . ?
O9 O1 N1 C3 33.7(3) . . . . ?
O2 O1 N1 C3 -105.7(2) . . . . ?
O4 O1 N1 C3 140.7(2) 2_665 . . . ?
O9 O1 N1 C5 -87.9(3) . . . . ?
O2 O1 N1 C5 132.7(3) . . . . ?
O4 O1 N1 C5 19.1(3) 2_665 . . . ?
O1 O2 N2 C11 -77.9(3) . . . . ?
O3 O2 N2 C11 49.4(3) . . . . ?
O14 O2 N2 C11 156.0(3) 2_665 . . . ?
O1 O2 N2 C9 160.9(3) . . . . ?
O3 O2 N2 C9 -71.8(3) . . . . ?
O14 O2 N2 C9 34.8(3) 2_665 . . . ?
O1 O2 N2 C7 40.2(2) . . . . ?
O3 O2 N2 C7 167.5(2) . . . . ?
O14 O2 N2 C7 -85.9(3) 2_665 . . . ?
O3 O4 N3 C17 155.1(3) . . . . ?
O10 O4 N3 C17 58.5(4) . . . . ?
O1 O4 N3 C17 -57.2(3) 2_665 . . . ?
O3 O4 N3 C13 37.8(3) . . . . ?
O10 O4 N3 C13 -58.8(4) . . . . ?
O1 O4 N3 C13 -174.5(3) 2_665 . . . ?
O3 O4 N3 C15 -84.9(3) . . . . ?
O10 O4 N3 C15 178.6(3) . . . . ?
O1 O4 N3 C15 62.9(2) 2_665 . . . ?
O19 O12 N4 C19A -48.1(7) . . . . ?
O13 O12 N4 C19A -169.4(6) . . . . ?
O11 O12 N4 C19A 77.4(7) . . . . ?
O19 O12 N4 C21 167.1(8) . . . . ?
O13 O12 N4 C21 45.8(8) . . . . ?
O11 O12 N4 C21 -67.4(8) . . . . ?
O19 O12 N4 C23 36.2(5) . . . . ?
O13 O12 N4 C23 -85.1(5) . . . . ?
O11 O12 N4 C23 161.6(5) . . . . ?
O19 O12 N4 C21A -170.3(8) . . . . ?
O13 O12 N4 C21A 68.4(8) . . . . ?
O11 O12 N4 C21A -44.8(8) . . . . ?
O19 O12 N4 C23A 74.9(5) . . . . ?
O13 O12 N4 C23A -46.3(5) . . . . ?
O11 O12 N4 C23A -159.6(5) . . . . ?
O19 O12 N4 C19 -80.3(5) . . . . ?
O13 O12 N4 C19 158.4(4) . . . . ?
O11 O12 N4 C19 45.2(5) . . . . ?
C3 N1 C1 C2 -58.8(4) . . . . ?
C5 N1 C1 C2 58.5(4) . . . . ?
O1 N1 C1 C2 169.8(3) . . . . ?
C6 N11 C2 C1 -58.7(4) . . . . ?
C4 N11 C2 C1 58.3(4) . . . . ?
O6 N11 C2 C1 178.8(3) 2_655 . . . ?
N1 C1 C2 N11 0.1(5) . . . . ?
C1 N1 C3 C4 58.8(4) . . . . ?
C5 N1 C3 C4 -58.8(4) . . . . ?
O1 N1 C3 C4 -178.6(2) . . . . ?
C6 N11 C4 C3 59.2(4) . . . . ?
C2 N11 C4 C3 -58.0(4) . . . . ?
O6 N11 C4 C3 -173.5(2) 2_655 . . . ?
N1 C3 C4 N11 -0.3(4) . . . . ?
C1 N1 C5 C6 -58.4(5) . . . . ?
C3 N1 C5 C6 59.5(4) . . . . ?
O1 N1 C5 C6 -170.6(3) . . . . ?
C4 N11 C6 C5 -58.9(4) . . . . ?
C2 N11 C6 C5 58.8(4) . . . . ?
O6 N11 C6 C5 175.0(3) 2_655 . . . ?
N1 C5 C6 N11 -0.4(5) . . . . ?
C11 N2 C7 C8 -61.6(4) . . . . ?
C9 N2 C7 C8 57.3(4) . . . . ?
O2 N2 C7 C8 -179.5(2) . . . . ?
C10 N22 C8 C7 -61.0(4) . . . . ?
C12 N22 C8 C7 57.0(4) . . . . ?
O7 N22 C8 C7 175.4(2) 2_665 . . . ?
N2 C7 C8 N22 3.3(4) . . . . ?
C11 N2 C9 C10 56.5(5) . . . . ?
C7 N2 C9 C10 -61.4(5) . . . . ?
O2 N2 C9 C10 176.5(3) . . . . ?
C12 N22 C10 C9 -60.4(4) . . . . ?
C8 N22 C10 C9 57.1(4) . . . . ?
O7 N22 C10 C9 -175.7(3) 2_665 . . . ?
N2 C9 C10 N22 3.8(6) . . . . ?
C9 N2 C11 C12 -59.9(4) . . . . ?
C7 N2 C11 C12 57.8(4) . . . . ?
O2 N2 C11 C12 177.3(3) . . . . ?
C10 N22 C12 C11 56.7(4) . . . . ?
C8 N22 C12 C11 -60.8(4) . . . . ?
O7 N22 C12 C11 174.6(3) 2_665 . . . ?
N2 C11 C12 N22 2.8(5) . . . . ?
C17 N3 C13 C14 59.5(4) . . . . ?
C15 N3 C13 C14 -58.8(4) . . . . ?
O4 N3 C13 C14 174.4(3) . . . . ?
C18 N33 C14 C13 -58.0(4) . . . . ?
C16 N33 C14 C13 59.7(4) . . . . ?
O17 N33 C14 C13 -178.2(3) 1_454 . . . ?
N3 C13 C14 N33 -0.9(5) . . . . ?
C17 N3 C15 C16 -58.5(4) . . . . ?
C13 N3 C15 C16 60.0(4) . . . . ?
O4 N3 C15 C16 -176.8(2) . . . . ?
C14 N33 C16 C15 -58.3(3) . . . . ?
C18 N33 C16 C15 59.9(3) . . . . ?
O17 N33 C16 C15 175.7(2) 1_454 . . . ?
N3 C15 C16 N33 -1.3(4) . . . . ?
C13 N3 C17 C18 -58.5(4) . . . . ?
C15 N3 C17 C18 59.6(4) . . . . ?
O4 N3 C17 C18 -175.9(3) . . . . ?
C14 N33 C18 C17 59.0(4) . . . . ?
C16 N33 C18 C17 -59.0(4) . . . . ?
O17 N33 C18 C17 -175.9(3) 1_454 . . . ?
N3 C17 C18 N33 -0.7(5) . . . . ?
C19A N4 C19 C20 84.4(17) . . . . ?
C21 N4 C19 C20 -58.2(11) . . . . ?
C23 N4 C19 C20 62.1(9) . . . . ?
C21A N4 C19 C20 -69.5(10) . . . . ?
C23A N4 C19 C20 35.6(12) . . . . ?
O12 N4 C19 C20 -175.3(6) . . . . ?
N4 C19 C20 N44 -2.8(10) . . . . ?
C22A N44 C20 C19 72.8(13) . . . . ?
C20A N44 C20 C19 -80.5(12) . . . . ?
C24 N44 C20 C19 -57.6(8) . . . . ?
C22 N44 C20 C19 62.9(11) . . . . ?
C24A N44 C20 C19 -32.4(11) . . . . ?
O16 N44 C20 C19 179.0(6) 2_676 . . . ?
C19A N4 C21 C22 37.2(19) . . . . ?
C23 N4 C21 C22 -54.5(16) . . . . ?
C21A N4 C21 C22 92(4) . . . . ?
C23A N4 C21 C22 -71.8(14) . . . . ?
C19 N4 C21 C22 60.2(15) . . . . ?
O12 N4 C21 C22 173.9(12) . . . . ?
C22A N44 C22 C21 -92(6) . . . . ?
C20A N44 C22 C21 -38.2(19) . . . . ?
C24 N44 C22 C21 52.9(16) . . . . ?
C20 N44 C22 C21 -63.1(14) . . . . ?
C24A N44 C22 C21 71.2(14) . . . . ?
O16 N44 C22 C21 173.8(11) 2_676 . . . ?
N4 C21 C22 N44 1(2) . . . . ?
C19A N4 C23 C24 -72.5(9) . . . . ?
C21 N4 C23 C24 52.9(12) . . . . ?
C21A N4 C23 C24 37.0(16) . . . . ?
C23A N4 C23 C24 83.8(12) . . . . ?
C19 N4 C23 C24 -61.0(9) . . . . ?
O12 N4 C23 C24 -177.6(6) . . . . ?
C22A N44 C24 C23 -38.2(17) . . . . ?
C20A N44 C24 C23 72.5(9) . . . . ?
C22 N44 C24 C23 -53.6(13) . . . . ?
C20 N44 C24 C23 59.6(9) . . . . ?
C24A N44 C24 C23 -87.5(12) . . . . ?
O16 N44 C24 C23 -172.8(7) 2_676 . . . ?
N4 C23 C24 N44 0.7(11) . . . . ?
C21 N4 C19A C20A -38.8(17) . . . . ?
C23 N4 C19A C20A 71.5(11) . . . . ?
C21A N4 C19A C20A -58.0(14) . . . . ?
C23A N4 C19A C20A 57.4(12) . . . . ?
C19 N4 C19A C20A -86.5(19) . . . . ?
O12 N4 C19A C20A -176.2(9) . . . . ?
C22A N44 C20A C19A 54.6(16) . . . . ?
C24 N44 C20A C19A -73.6(10) . . . . ?
C22 N44 C20A C19A 36.2(17) . . . . ?
C20 N44 C20A C19A 84.0(14) . . . . ?
C24A N44 C20A C19A -61.9(12) . . . . ?
O16 N44 C20A C19A -178.7(8) 2_676 . . . ?
N4 C19A C20A N44 2.1(16) . . . . ?
C19A N4 C21A C22A 56.2(15) . . . . ?
C21 N4 C21A C22A -79(4) . . . . ?
C23 N4 C21A C22A -37(2) . . . . ?
C23A N4 C21A C22A -62.2(15) . . . . ?
C19 N4 C21A C22A 70.4(14) . . . . ?
O12 N4 C21A C22A 175.8(11) . . . . ?
C20A N44 C22A C21A -54.7(17) . . . . ?
C24 N44 C22A C21A 38(2) . . . . ?
C22 N44 C22A C21A 81(5) . . . . ?
C20 N44 C22A C21A -70.6(14) . . . . ?
C24A N44 C22A C21A 63.8(16) . . . . ?
O16 N44 C22A C21A 173.3(12) 2_676 . . . ?
N4 C21A C22A N44 -1(2) . . . . ?
C19A N4 C23A C24A -57.2(11) . . . . ?
C21 N4 C23A C24A 70.1(11) . . . . ?
C23 N4 C23A C24A -81.6(12) . . . . ?
C21A N4 C23A C24A 63.9(12) . . . . ?
C19 N4 C23A C24A -33.0(13) . . . . ?
O12 N4 C23A C24A 180.0(7) . . . . ?
C22A N44 C24A C23A -62.2(14) . . . . ?
C20A N44 C24A C23A 60.4(10) . . . . ?
C24 N44 C24A C23A 81.0(12) . . . . ?
C22 N44 C24A C23A -68.2(12) . . . . ?
C20 N44 C24A C23A 34.6(13) . . . . ?
O16 N44 C24A C23A -174.1(7) 2_676 . . . ?
N4 C23A C24A N44 -1.3(12) . . . . ?

_diffrn_measured_fraction_theta_max 0.711
_diffrn_reflns_theta_full        22.75
_diffrn_measured_fraction_theta_full 0.711
_refine_diff_density_max         0.175
_refine_diff_density_min         -0.180
_refine_diff_density_rms         0.027
#===END


