# Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2000
# CCDC Number: 186/2040

# CIF files for the two structures contained in ms B003249M follow.
#    Vickie McKee
#
#
# Protonated Azacryptand Hosts for Nitrate
# MJ Hynes, B Maubert, V McKee, RM Town and J Nelson
 
data_complex1
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C36 H66 Cl6 N8 O27' 
_chemical_formula_weight          1255.67 
  
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' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Cubic 
_symmetry_space_group_name_H-M    P2(1)3 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, -y, z+1/2' 
 '-x, y+1/2, -z+1/2' 
 'x+1/2, -y+1/2, -z' 
 'z, x, y' 
 'z+1/2, -x+1/2, -y' 
 '-z+1/2, -x, y+1/2' 
 '-z, x+1/2, -y+1/2' 
 'y, z, x' 
 '-y, z+1/2, -x+1/2' 
 'y+1/2, -z+1/2, -x' 
 '-y+1/2, -z, x+1/2' 
  
_cell_length_a                    17.443(2) 
_cell_length_b                    17.443(2) 
_cell_length_c                    17.443(2) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      5307.5(12) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     153(2) 
_cell_measurement_reflns_used     27 
_cell_measurement_theta_min       4.81 
_cell_measurement_theta_max       11.51 
  
_exptl_crystal_description        'trigonal prism' 
_exptl_crystal_colour             colourless 
_exptl_crystal_size_max           0.65 
_exptl_crystal_size_mid           0.60 
_exptl_crystal_size_min           0.42 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.571 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2624 
_exptl_absorpt_coefficient_mu     0.419 
_exptl_absorpt_correction_type    none 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       153(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   ? 
_diffrn_measurement_method        '\w scans' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  97 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         0 
_diffrn_reflns_number             6903 
_diffrn_reflns_av_R_equivalents   0.0487 
_diffrn_reflns_av_sigmaI/netI     0.0631 
_diffrn_reflns_limit_h_min        -12 
_diffrn_reflns_limit_h_max        17 
_diffrn_reflns_limit_k_min        -20 
_diffrn_reflns_limit_k_max        9 
_diffrn_reflns_limit_l_min        -9 
_diffrn_reflns_limit_l_max        20 
_diffrn_reflns_theta_min          2.02 
_diffrn_reflns_theta_max          24.99 
_reflns_number_total              3141 
_reflns_number_gt                 2464 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Siemens XSCANS' 
_computing_cell_refinement        'Siemens XSCANS' 
_computing_data_reduction         'Siemens SHELXTL' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'Siemens SHELXTL' 
_computing_publication_material   'Siemens SHELXTL' 
  
_refine_special_details 
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR 
and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and 
is 
 not relevant to the choice of reflections for refinement.  R-factors 
based 
 on F^2^ are statistically about twice as large as those based on F, and 
R- 
 factors based on ALL data will be even larger. 
; 
  
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
 'calc w=1/[\s^2^(Fo^2^)+(0.0603P)^2^+4.7820P] 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     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.07(10) 
_refine_ls_number_reflns          3141 
_refine_ls_number_parameters      232 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0795 
_refine_ls_R_factor_gt            0.0554 
_refine_ls_wR_factor_ref          0.1307 
_refine_ls_wR_factor_gt           0.1196 
_refine_ls_goodness_of_fit_ref    1.026 
_refine_ls_restrained_S_all       1.026 
_refine_ls_shift/su_max           0.002 
_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_multiplicit 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
N1 N 0.6320(2) 0.8680(2) 0.1320(2) 0.0177(13) Uani 1 3 d S . . 
C1 C 0.6090(3) 0.7868(3) 0.1246(3) 0.0250(11) Uani 1 1 d . . . 
H1A H 0.6380 0.7565 0.1629 0.030 Uiso 1 1 calc R . . 
H1B H 0.6244 0.7685 0.0732 0.030 Uiso 1 1 calc R . . 
C2 C 0.5247(3) 0.7702(3) 0.1352(3) 0.0252(11) Uani 1 1 d . . . 
H2A H 0.5169 0.7140 0.1363 0.030 Uiso 1 1 calc R . . 
H2B H 0.5079 0.7910 0.1852 0.030 Uiso 1 1 calc R . . 
N3 N 0.4764(2) 0.8037(2) 0.0735(2) 0.0239(9) Uani 1 1 d . . . 
H3A H 0.4986 0.7938 0.0267 0.029 Uiso 1 1 calc R . . 
H3B H 0.4742 0.8561 0.0796 0.029 Uiso 1 1 calc R . . 
C3 C 0.3961(3) 0.7716(3) 0.0743(3) 0.0298(12) Uani 1 1 d . . . 
H3C H 0.3984 0.7150 0.0716 0.036 Uiso 1 1 calc R . . 
H3D H 0.3706 0.7858 0.1230 0.036 Uiso 1 1 calc R . . 
C4 C 0.3494(3) 0.8015(3) 0.0079(3) 0.0284(11) Uani 1 1 d . . . 
C5 C 0.3650(3) 0.7769(3) -0.0650(3) 0.0334(12) Uani 1 1 d . . . 
H5 H 0.4053 0.7413 -0.0737 0.040 Uiso 1 1 calc R . . 
C6 C 0.3226(3) 0.8035(3) -0.1253(3) 0.0343(12) Uani 1 1 d . . . 
H6 H 0.3341 0.7868 -0.1758 0.041 Uiso 1 1 calc R . . 
C7 C 0.2633(3) 0.8543(3) -0.1137(3) 0.0349(13) Uani 1 1 d . . . 
H7 H 0.2343 0.8723 -0.1562 0.042 Uiso 1 1 calc R . . 
C8 C 0.2454(3) 0.8795(3) -0.0403(3) 0.0290(11) Uani 1 1 d . . . 
C9 C 0.2892(3) 0.8527(3) 0.0212(3) 0.0296(11) Uani 1 1 d . . . 
H9 H 0.2780 0.8692 0.0719 0.036 Uiso 1 1 calc R . . 
C10 C 0.1840(3) 0.9387(3) -0.0290(4) 0.0380(14) Uani 1 1 d . . . 
H10A H 0.1558 0.9280 0.0190 0.046 Uiso 1 1 calc R . . 
H10B H 0.1471 0.9362 -0.0721 0.046 Uiso 1 1 calc R . . 
N4 N 0.2189(2) 1.0185(2) -0.0251(2) 0.0298(10) Uani 1 1 d . . . 
H4A H 0.1802 1.0543 -0.0281 0.036 Uiso 1 1 calc R . . 
H4B H 0.2428 1.0245 0.0215 0.036 Uiso 1 1 calc R . . 
C11 C 0.2747(3) 1.0332(3) -0.0868(3) 0.0290(11) Uani 1 1 d . . . 
H11A H 0.2524 1.0172 -0.1365 0.035 Uiso 1 1 calc R . . 
H11B H 0.3213 1.0022 -0.0777 0.035 Uiso 1 1 calc R . . 
C12 C 0.2965(3) 1.1177(3) -0.0909(3) 0.0285(11) Uani 1 1 d . . . 
H12A H 0.2601 1.1456 -0.1243 0.034 Uiso 1 1 calc R . . 
H12B H 0.2947 1.1409 -0.0391 0.034 Uiso 1 1 calc R . . 
N2 N 0.3768(2) 1.1232(2) -0.1232(2) 0.0235(14) Uani 1 3 d S . . 
Cl1 Cl 0.50929(6) 0.99071(6) 0.00929(6) 0.0259(5) Uani 1 3 d S . . 
O11 O 0.4615(2) 1.0385(2) -0.0385(2) 0.0504(19) Uani 1 3 d S . . 
O12 O 0.46436(19) 0.96324(19) 0.07552(19) 0.0283(8) Uani 1 1 d . . . 
Cl2 Cl 0.45951(7) 0.54049(7) 0.04049(7) 0.0325(5) Uani 1 3 d S . . 
O21 O 0.5061(3) 0.5827(3) 0.0936(3) 0.0590(12) Uani 1 1 d . . . 
O22 O 0.5070(2) 0.4930(2) -0.0070(2) 0.0474(18) Uani 1 3 d S . . 
Cl3 Cl 0.12948(8) 1.12948(8) 0.12948(8) 0.0376(5) Uani 1 3 d S . . 
O31 O 0.1756(3) 1.1756(3) 0.1756(3) 0.067(2) Uani 1 3 d S . . 
O32 O 0.1395(2) 1.1491(2) 0.0506(2) 0..0477(11) Uani 1 1 d . . . 
Cl4 Cl 0.08676(8) 0.77652(8) 0.12597(8) 0.0404(3) Uani 1 1 d . . . 
O41 O 0.0981(3) 0.8563(2) 0.1238(2) 0.0612(13) Uani 1 1 d . . . 
O42 O 0.0755(4) 0.7484(4) 0.0535(3) 0.127(3) Uani 1 1 d . . . 
O43 O 0.0214(3) 0.7593(3) 0.1729(3) 0.0788(17) Uani 1 1 d . . . 
O44 O 0.1516(5) 0.7459(4) 0.1600(6) 0.158(4) Uani 1 1 d . . . 
O1W O 0.3203(2) 1.0296(2) 0.0922(2) 0.0445(10) Uani 1 1 d . . . 
H1WA H 0.3773 1.0070 0.0988 0.050 Uiso 1 1 d . . . 
H1WB H 0.3057 1.0322 0.1431 0.050 Uiso 1 1 d . . . 
  
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 
N1 0.0177(13) 0.0177(13) 0.0177(13) 0.0005(16) -0.0005(16) 0.0005(16) 
C1 0.029(3) 0.020(2) 0.026(3) 0.004(2) -0.005(2) 0.003(2) 
C2 0.028(3) 0.025(3) 0.023(3) 0.008(2) -0.001(2) 0.002(2) 
N3 0.020(2) 0.024(2) 0.028(2) 0.0018(18) -0.0007(17) -0.0040(17) 
C3 0.029(3) 0.020(3) 0.041(3) 0.007(2) -0.006(2) -0.007(2) 
C4 0.024(3) 0.017(2) 0.044(3) 0.002(2) -0.007(2) -0.011(2) 
C5 0.036(3) 0.023(3) 0.041(3) -0.006(2) 0.000(3) -0.005(2) 
C6 0.041(3) 0.025(3) 0.037(3) -0.007(2) -0.001(3) -0.013(2) 
C7 0.038(3) 0.032(3) 0.034(3) 0.006(2) -0.013(2) -0.007(2) 
C8 0.019(2) 0.031(3) 0.037(3) 0.007(2) -0.005(2) -0.005(2) 
C9 0.032(3) 0.026(3) 0.031(3) 0.000(2) 0.001(2) -0.008(2) 
C10 0.020(3) 0.042(3) 0.051(4) 0.006(3) 0.005(2) -0.006(2) 
N4 0.026(2) 0.032(2) 0.031(2) -0.0005(19) 0.0026(19) 0.0060(19) 
C11 0.024(3) 0.030(3) 0.034(3) 0.004(2) 0.001(2) 0.003(2) 
C12 0.025(3) 0.029(3) 0.031(3) -0.001(2) 0.002(2) 0.002(2) 
N2 0.0235(14) 0.0235(14) 0.0235(14) -0.0048(18) 0.0048(18) -0.0048(18) 
Cl1 0.0259(5) 0.0259(5) 0.0259(5) 0.0031(5) -0.0031(5) 0.0031(5) 
O11 0.0504(19) 0.0504(19) 0.0504(19) 0.0168(18) -0.0168(18) 0.0168(18) 
O12 0.0255(18) 0.0287(18) 0.0306(19) 0.0005(15) 0.0063(16) -0.0004(15) 
Cl2 0.0325(5) 0.0325(5) 0.0325(5) -0.0049(5) 0.0049(5) 0.0049(5) 
O21 0.054(3) 0.062(3) 0.061(3) -0.027(2) -0..013(2) 0.001(2) 
O22 0.0474(18) 0.0474(18) 0.0474(18) -0.0101(19) 0.0101(19) 0.0101(19) 
Cl3 0.0376(5) 0.0376(5) 0.0376(5) 0.0007(6) 0.0007(6) 0.0007(6) 
O31 0.067(2) 0.067(2) 0.067(2) -0.008(2) -0.008(2) -0.008(2) 
O32 0.058(3) 0.043(2) 0.043(2) 0.0123(19) 0.019(2) 0.010(2) 
Cl4 0.0469(8) 0.0334(7) 0.0410(8) -0.0112(6) 0.0013(7) -0.0004(6) 
O41 0.104(4) 0.036(2) 0.044(2) 0.002(2) 0.031(2) -0.001(2) 
O42 0.103(5) 0.205(7) 0.074(4) -0.092(4) 0.037(3) -0.087(5) 
O43 0.108(4) 0.064(3) 0.064(3) -0.030(3) 0.041(3) -0.042(3) 
O44 0.134(7) 0.117(6) 0.222(10) 0.032(6) -0.048(7) 0.065(5) 
O1W 0.032(2) 0.064(3) 0.037(2) -0.016(2) -0.0015(17) 0.0103(19) 
  
_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 C1 1.479(5) 6_566 ? 
N1 C1 1.479(5) . ? 
N1 C1 1.479(5) 12_664 ? 
C1 C2 1.510(6) . ? 
C2 N3 1.487(6) . ? 
N3 C3 1.509(6) . ? 
C3 C4 1.508(7) . ? 
C4 C5 1.370(7) . ? 
C4 C9 1.398(7) . ? 
C5 C6 1.367(8) . ? 
C6 C7 1.377(8) . ? 
C7 C8 1.389(7) . ? 
C8 C9 1.397(7) . ? 
C8 C10 1.501(7) . ? 
C10 N4 1.521(6) . ? 
N4 C11 1.473(6) . ? 
C11 C12 1.524(7) . ? 
C12 N2 1.513(5) . ? 
N2 C12 1.513(5) 12_664 ? 
N2 C12 1.513(5) 6_566 ? 
Cl1 O11 1.444(7) . ? 
Cl1 O12 1.476(3) 12_664 ? 
Cl1 O12 1.476(3) . ? 
Cl1 O12 1.476(3) 6_566 ? 
Cl2 O22 1.434(7) . ? 
Cl2 O21 1.436(4) . ? 
Cl2 O21 1.436(4) 7_564 ? 
Cl2 O21 1.436(4) 10_655 ? 
Cl3 O31 1.392(8) . ? 
Cl3 O32 1.429(4) 9_465 ? 
Cl3 O32 1.429(4) 5_564 ? 
Cl3 O32 1.429(4) . ? 
Cl4 O42 1.370(5) . ? 
Cl4 O44 1.385(7) . ? 
Cl4 O41 1.406(4) . ? 
Cl4 O43 1.436(5) . ? 
  
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 
C1 N1 C1 108.6(3) 6_566 . ? 
C1 N1 C1 108.6(3) 6_566 12_664 ? 
C1 N1 C1 108.6(3) . 12_664 ? 
N1 C1 C2 115.9(4) . . ? 
N3 C2 C1 112.8(4) . . ? 
C2 N3 C3 111.9(4) . . ? 
C4 C3 N3 111.5(4) . . ? 
C5 C4 C9 120.2(5) . . ? 
C5 C4 C3 119.8(5) . . ? 
C9 C4 C3 119.9(5) . . ? 
C6 C5 C4 120.0(5) . . ? 
C5 C6 C7 120.8(5) . . ? 
C6 C7 C8 120.5(5) . . ? 
C7 C8 C9 118.7(5) . . ? 
C7 C8 C10 119.8(5) . . ? 
C9 C8 C10 121.3(5) . . ? 
C8 C9 C4 119.8(5) . . ? 
C8 C10 N4 110.5(4) . . ? 
C11 N4 C10 113.0(4) . . ? 
N4 C11 C12 111.6(4) . . ? 
N2 C12 C11 108.1(4) . . ? 
C12 N2 C12 112.3(3) 12_664 6_566 ? 
C12 N2 C12 112.3(3) 12_664 . ? 
C12 N2 C12 112.3(3) 6_566 . ? 
O11 Cl1 O12 109.44(15) . 12_664 ? 
O11 Cl1 O12 109.44(15) . . ? 
O12 Cl1 O12 109.51(15) 12_664 . ? 
O11 Cl1 O12 109.44(15) . 6_566 ? 
O12 Cl1 O12 109.51(15) 12_664 6_566 ? 
O12 Cl1 O12 109.51(15) . 6_566 ? 
O22 Cl2 O21 110.02(19) . . ? 
O22 Cl2 O21 110.02(19) . 7_564 ? 
O21 Cl2 O21 108.92(19) . 7_564 ? 
O22 Cl2 O21 110.02(19) . 10_655 ? 
O21 Cl2 O21 108.92(19) . 10_655 ? 
O21 Cl2 O21 108.92(19) 7_564 10_655 ? 
O31 Cl3 O32 110.3(2) . 9_465 ? 
O31 Cl3 O32 110.3(2) . 5_564 ? 
O32 Cl3 O32 108.6(2) 9_465 5_564 ? 
O31 Cl3 O32 110.3(2) . . ? 
O32 Cl3 O32 108.6(2) 9_465 . ? 
O32 Cl3 O32 108.6(2) 5_564 . ? 
O42 Cl4 O44 112.0(5) . . ? 
O42 Cl4 O41 110.5(4) . . ? 
O44 Cl4 O41 106.2(4) . . ? 
O42 Cl4 O43 109.7(3) . . ? 
O44 Cl4 O43 108.9(5) . . ? 
O41 Cl4 O43 109.5(3) . . ? 
  
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
C1 N1 C1 C2 70.2(7) 6_566 . . . ? 
C1 N1 C1 C2 -171.8(4) 12_664 . . . ? 
N1 C1 C2 N3 66.5(5) . . . . ? 
C1 C2 N3 C3 166.6(4) . . . . ? 
C2 N3 C3 C4 -175.7(4) . . . . ? 
N3 C3 C4 C5 71.3(5) . . . . ? 
N3 C3 C4 C9 -110.3(5) . . . . ? 
C9 C4 C5 C6 1.2(7) . . . . ? 
C3 C4 C5 C6 179.7(4) . . . . ? 
C4 C5 C6 C7 -0.9(7) . . . . ? 
C5 C6 C7 C8 0.0(8) . . . . ? 
C6 C7 C8 C9 0.4(8) . . . . ? 
C6 C7 C8 C10 176.1(5) . . . . ? 
C7 C8 C9 C4 -0.1(7) . . . . ? 
C10 C8 C9 C4 -175.6(4) . . . . ? 
C5 C4 C9 C8 -0.8(7) . . . . ? 
C3 C4 C9 C8 -179.2(4) . . . . ? 
C7 C8 C10 N4 -94.7(6) . . . . ? 
C9 C8 C10 N4 80.8(6) . . . . ? 
C8 C10 N4 C11 47.4(6) . . . . ? 
C10 N4 C11 C12 168.7(4) . . . . ? 
N4 C11 C12 N2 152.0(4) . . . . ? 
C11 C12 N2 C12 61.6(7) . . . 12_664 ? 
C11 C12 N2 C12 -170.6(4) . . . 6_566 ? 
  
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 
N3 H3A O42  0.92 2.07 2.953(6) 159.7 4_565 
N3 H3B O12  0.92 1.88 2.790(5) 170.7 . 
N3 H3B O12  0.92 2.58 3.028(5) 110.5 12_664 
N4 H4A O32  0.92 2.26 2.975(6) 133.8 . 
N4 H4A O41  0.92 2.37 2.992(6) 124.8 5_564 
N4 H4B O1W  0.92 1.83 2.712(6) 159.3 . 
O1W H1WA O12  1.08 1.75 2.782(5) 159.8 . 
O1W H1WB O43  0.92 2.26 3.049(6) 142.6 7_564 
  
_diffrn_measured_fraction_theta_max    0.999 
_diffrn_reflns_theta_full              24.99 
_diffrn_measured_fraction_theta_full   0.999 
_refine_diff_density_max    0.405 
_refine_diff_density_min   -0.278 
_refine_diff_density_rms    0.065 
 
data_complex3
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C36 H64 N14 O20' 
_chemical_formula_weight          1013.01 
 
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            ? 
_symmetry_space_group_name_H-M    ? 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
 
_cell_length_a                    10.1676(8) 
_cell_length_b                    10.3453(8) 
_cell_length_c                    25.510(2) 
_cell_angle_alpha                 80.453(2) 
_cell_angle_beta                  84.666(2) 
_cell_angle_gamma                 62.182(2) 
_cell_volume                      2339.9(3) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           ? 
_exptl_crystal_size_mid           ? 
_exptl_crystal_size_min           ? 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.438 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1076 
_exptl_absorpt_coefficient_mu     0.118 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       150(2) 
_diffrn_radiation_wavelength      0.69230 
_diffrn_radiation_type            ? 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   ? 
_diffrn_measurement_method        ? 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             21993 
_diffrn_reflns_av_R_equivalents   0.0364 
_diffrn_reflns_av_sigmaI/netI     0.0595 
_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        -33 
_diffrn_reflns_limit_l_max        34 
_diffrn_reflns_theta_min          2.19 
_diffrn_reflns_theta_max          27.50 
_reflns_number_total              11319 
_reflns_number_gt                 8787 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR 
and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and 
is 
 not relevant to the choice of reflections for refinement.  R-factors 
based 
 on F^2^ are statistically about twice as large as those based on F, and 
R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[\s^2^(Fo^2^)+(0.0741P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          11319 
_refine_ls_number_parameters      640 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0582 
_refine_ls_R_factor_gt            0.0441 
_refine_ls_wR_factor_ref          0.1272 
_refine_ls_wR_factor_gt           0.1238 
_refine_ls_goodness_of_fit_ref    1.024 
_refine_ls_restrained_S_all       1.024 
_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 0.95467(11) 0.27261(11) 0.43552(4) 0.0205(2) Uani 1 1 d . . . 
C1A C 0.83218(15) 0.25590(15) 0.46640(5) 0.0237(3) Uani 1 1 d . . . 
H1A1 H 0.7491 0.3552 0.4695 0.028 Uiso 1 1 calc R . . 
H1A2 H 0.8671 0.2067 0.5027 0.028 Uiso 1 1 calc R . . 
C2A C 0.77432(15) 0.16789(14) 0.44243(5) 0.0244(3) Uani 1 1 d . . . 
H2A1 H 0.8595 0.0812 0.4297 0.029 Uiso 1 1 calc R . . 
H2A2 H 0.7204 0.1313 0.4703 0.029 Uiso 1 1 calc R . . 
N3A N 0.67253(12) 0.25779(12) 0.39726(4) 0.0239(2) Uani 1 1 d . . . 
C3A C 0.62533(15) 0.16680(14) 0.37154(5) 0.0256(3) Uani 1 1 d . . . 
H3A1 H 0.5755 0.1230 0.3985 0.031 Uiso 1 1 calc R . . 
H3A2 H 0.7145 0.0850 0.3580 0.031 Uiso 1 1 calc R . . 
C4A C 0.52126(14) 0.25579(14) 0.32641(5) 0.0229(2) Uani 1 1 d . . . 
C5A C 0.38056(15) 0.36807(15) 0.33559(5) 0.0260(3) Uani 1 1 d . . . 
H5A H 0.3515 0.3936 0.3704 0.031 Uiso 1 1 calc R . . 
C6A C 0.28220(15) 0.44318(15) 0.29394(6) 0.0283(3) Uani 1 1 d . . . 
H6A H 0.1868 0.5213 0.3003 0.034 Uiso 1 1 calc R . . 
C7A C 0.32263(15) 0.40458(15) 0.24316(5) 0.0266(3) Uani 1 1 d . . . 
H7A H 0.2535 0.4533 0.2151 0.032 Uiso 1 1 calc R . . 
C8A C 0.46422(15) 0.29458(14) 0.23340(5) 0.0231(2) Uani 1 1 d . . . 
C9A C 0.56350(14) 0.22122(14) 0.27504(5) 0.0238(3) Uani 1 1 d . . . 
H9A H 0.6609 0.1469 0.2683 0.029 Uiso 1 1 calc R . . 
C10A C 0.51297(15) 0.25229(14) 0.17846(5) 0.0249(3) Uani 1 1 d . . . 
H10A H 0.6085 0.1605 0.1806 0.030 Uiso 1 1 calc R . . 
H10B H 0.4380 0.2329 0.1639 0.030 Uiso 1 1 calc R . . 
N4A N 0.53140(12) 0.37194(12) 0.14216(4) 0.0221(2) Uani 1 1 d . . . 
C11A C 0.59203(15) 0.32809(15) 0.08893(5) 0.0238(3) Uani 1 1 d . . . 
H11A H 0.5200 0.3109 0.0713 0.029 Uiso 1 1 calc R . . 
H11B H 0.6855 0.2343 0.0935 0.029 Uiso 1 1 calc R . . 
C12A C 0.62251(14) 0.44469(15) 0.05391(5) 0.0237(3) Uani 1 1 d . . . 
H12A H 0.6254 0.4306 0.0163 0.028 Uiso 1 1 calc R . . 
H12B H 0.5396 0.5432 0.0583 0.028 Uiso 1 1 calc R . . 
N2 N 0.76358(12) 0.44126(12) 0.06592(4) 0.0210(2) Uani 1 1 d . . . 
C1B C 1.09451(14) 0.13646(14) 0.44830(5) 0.0244(3) Uani 1 1 d . . . 
H1B1 H 1.0745 0.0506 0.4513 0.029 Uiso 1 1 calc R . . 
H1B2 H 1.1284 0.1372 0.4834 0.029 Uiso 1 1 calc R . . 
C2B C 1.21848(14) 0.11701(15) 0.40768(5) 0.0254(3) Uani 1 1 d . . . 
H2B1 H 1.2142 0.2143 0.3942 0.031 Uiso 1 1 calc R . . 
H2B2 H 1.3156 0.0533 0.4249 0.031 Uiso 1 1 calc R . . 
N3B N 1.20646(12) 0.04924(13) 0.36216(5) 0.0261(2) Uani 1 1 d . . . 
C3B C 1.33038(16) 0.02526(18) 0.32270(6) 0.0333(3) Uani 1 1 d . . . 
H3B1 H 1.4254 -0.0481 0.3396 0.040 Uiso 1 1 calc R . . 
H3B2 H 1.3360 0.1190 0.3120 0.040 Uiso 1 1 calc R . . 
C4B C 1.31127(14) -0.02843(16) 0.27376(6) 0.0274(3) Uani 1 1 d . . . 
C5B C 1.34182(16) -0.17435(16) 0.27403(6) 0.0309(3) Uani 1 1 d . . . 
H5B H 1.3720 -0.2422 0.3059 0.037 Uiso 1 1 calc R . . 
C6B C 1.32817(17) -0.22083(16) 0.22765(6) 0.0323(3) Uani 1 1 d . . . 
H6B H 1.3470 -0.3200 0.2281 0.039 Uiso 1 1 calc R . . 
C7B C 1.28731(15) -0.12356(16) 0.18067(6) 0.0296(3) Uani 1 1 d . . . 
H7B H 1.2798 -0.1566 0.1490 0.036 Uiso 1 1 calc R . . 
C8B C 1.25732(14) 0.02225(15) 0.17993(6) 0.0264(3) Uani 1 1 d . . . 
C9B C 1.26670(14) 0.06914(15) 0.22687(6) 0.0281(3) Uani 1 1 d . . . 
H9B H 1.2422 0.1697 0.2269 0.034 Uiso 1 1 calc R . . 
C10B C 1.22186(16) 0.12808(17) 0.12899(6) 0.0329(3) Uani 1 1 d . . . 
H10E H 1.2253 0.2185 0.1351 0.039 Uiso 1 1 calc R . . 
H10F H 1.2987 0.0824 0.1018 0.039 Uiso 1 1 calc R . . 
N4B N 1.07295(12) 0.16935(13) 0.10857(4) 0.0252(2) Uani 1 1 d . . . 
C11B C 1.03893(15) 0.27926(16) 0.05928(5) 0.0272(3) Uani 1 1 d . . . 
H11C H 1.1145 0.2356 0.0314 0.033 Uiso 1 1 calc R . . 
H11D H 1.0448 0.3672 0.0669 0.033 Uiso 1 1 calc R . . 
C12B C 0.88532(15) 0.32642(16) 0.03866(5) 0.0266(3) Uani 1 1 d . . . 
H12E H 0.8831 0.3636 0.0002 0.032 Uiso 1 1 calc R . . 
H12F H 0.8678 0.2388 0.0426 0.032 Uiso 1 1 calc R . . 
C1C C 0.96823(14) 0.39613(14) 0.45197(5) 0.0232(2) Uani 1 1 d . . . 
H1A H 1.0675 0.3876 0.4408 0.028 Uiso 1 1 calc R . . 
H1B H 0.9615 0.3879 0.4912 0.028 Uiso 1 1 calc R . . 
C2C C 0.85010(15) 0.54690(14) 0.42875(5) 0.0242(3) Uani 1 1 d . . . 
H2A H 0.7547 0.5435 0.4277 0.029 Uiso 1 1 calc R . . 
H2B H 0.8356 0.6200 0.4522 0.029 Uiso 1 1 calc R . . 
N3C N 0.89039(12) 0.59594(12) 0.37408(4) 0.0234(2) Uani 1 1 d . . . 
C3C C 0.76518(15) 0.73643(15) 0.34942(5) 0.0295(3) Uani 1 1 d . . . 
H3A H 0.7430 0.8155 0.3711 0.035 Uiso 1 1 calc R . . 
H3B H 0.6751 0.7225 0.3497 0.035 Uiso 1 1 calc R . . 
C4C C 0.80048(14) 0.78399(14) 0.29309(5) 0.0254(3) Uani 1 1 d . . . 
C5C C 0.89788(15) 0.84526(15) 0.28204(6) 0.0292(3) Uani 1 1 d . . . 
H5 H 0.9471 0.8535 0.3102 0.035 Uiso 1 1 calc R . . 
C6C C 0.92336(16) 0.89430(16) 0.23001(6) 0.0318(3) Uani 1 1 d . . . 
H6 H 0.9911 0.9346 0.2226 0.038 Uiso 1 1 calc R . . 
C7C C 0.85021(15) 0.88460(15) 0.18876(5) 0.0283(3) Uani 1 1 d . . . 
H7 H 0.8674 0.9190 0.1532 0.034 Uiso 1 1 calc R . . 
C8C C 0.75165(14) 0.82463(14) 0.19927(5) 0.0252(3) Uani 1 1 d . . . 
C9C C 0.73000(14) 0.77182(14) 0.25143(5) 0.0257(3) Uani 1 1 d . . . 
H9 H 0.6662 0.7268 0.2587 0.031 Uiso 1 1 calc R . . 
C10C C 0.66304(16) 0.82132(16) 0.15585(6) 0.0305(3) Uani 1 1 d . . . 
H10C H 0.5812 0.8009 0.1721 0.037 Uiso 1 1 calc R . . 
H10D H 0.6181 0.9195 0.1339 0.037 Uiso 1 1 calc R . . 
N4C N 0.75559(13) 0.70753(13) 0.12098(5) 0.0263(2) Uani 1 1 d . . . 
C11C C 0.66379(16) 0.70449(15) 0.07914(6) 0.0286(3) Uani 1 1 d . . . 
H11E H 0.6193 0.8019 0.0567 0.034 Uiso 1 1 calc R . . 
H11F H 0.5817 0.6859 0.0963 0.034 Uiso 1 1 calc R . . 
C12C C 0.75594(16) 0.58623(15) 0.04450(5) 0.0262(3) Uani 1 1 d . . . 
H12C H 0.7128 0.6177 0.0086 0.031 Uiso 1 1 calc R . . 
H12D H 0.8581 0.5759 0.0409 0.031 Uiso 1 1 calc R . . 
N11 N 0.90201(14) 0.33439(14) 0.31514(4) 0.0294(3) Uani 1 1 d . . . 
O11 O 0.77447(11) 0.43512(12) 0.32274(4) 0.0344(2) Uani 1 1 d . . . 
O12 O 0.92135(12) 0.20541(12) 0.31561(4) 0.0344(2) Uani 1 1 d . . . 
O13 O 1.01092(12) 0.36108(12) 0.30959(4) 0.0342(2) Uani 1 1 d . . . 
N21 N 0.81519(13) 0.38479(14) 0.18570(4) 0.0276(2) Uani 1 1 d . . . 
O21 O 0.68635(11) 0.48618(11) 0.19164(4) 0.0304(2) Uani 1 1 d . . . 
O22 O 0.83509(11) 0.25589(11) 0.18545(4) 0.0309(2) Uani 1 1 d . . . 
O23 O 0.92237(11) 0.41379(13) 0.17769(4) 0.0364(2) Uani 1 1 d . . . 
N31 N 1.41330(14) 0.18304(13) 0.51656(5) 0.0328(3) Uani 1 1 d . . . 
O31 O 1.51001(14) 0.19207(15) 0.53991(6) 0.0527(3) Uani 1 1 d . . . 
O32 O 1.35656(15) 0.10326(14) 0.53746(5) 0.0485(3) Uani 1 1 d . . . 
O33 O 1.36863(17) 0.25886(15) 0.47240(5) 0.0527(3) Uani 1 1 d . . . 
N41 N 0.63327(14) 0.06945(14) 0.02383(5) 0.0315(3) Uani 1 1 d . . . 
O41 O 0.63458(14) 0.16588(14) -0.01259(5) 0.0455(3) Uani 1 1 d . . . 
O42 O 0.75224(13) -0.04364(14) 0.03663(6) 0.0497(3) Uani 1 1 d . . . 
O43 O 0.51495(12) 0.08743(12) 0.04771(5) 0.0388(3) Uani 1 1 d . . . 
N51 N 0.16924(13) 0.59432(13) 0.10558(4) 0.0268(2) Uani 1 1 d . . . 
O51 O 0.20530(16) 0.46363(13) 0.10416(6) 0.0537(3) Uani 1 1 d . . . 
O52 O 0.26158(12) 0.62820(12) 0.12025(5) 0.0400(3) Uani 1 1 d . . . 
O53 O 0.04309(11) 0.69498(13) 0.09115(4) 0.0354(2) Uani 1 1 d . . . 
N61 N 1.13029(13) 0.74524(13) 0.39949(4) 0.0270(2) Uani 1 1 d . . . 
O61 O 1.00924(14) 0.85575(14) 0.39682(5) 0.0515(3) Uani 1 1 d . . . 
O62 O 1.24766(13) 0.75750(13) 0.40091(4) 0.0377(2) Uani 1 1 d . . . 
O63 O 1.13942(12) 0.62019(12) 0.40177(5) 0.0377(2) Uani 1 1 d . . . 
O1W O 1.07280(13) -0.04207(13) 0.06160(5) 0.0411(3) Uani 1 1 d . . . 
O2W O 1.4601(3) 0.4689(2) 0.45489(10) 0.0325(5) Uani 0.50 1 d P . . 
O2W' O 1.4972(3) 0.5170(3) 0.43628(11) 0.0444(6) Uani 0.50 1 d P . . 
H3A1 H 0.5843 0.3367 0.4100 0.040 Uiso 1 1 d . . . 
H3A2 H 0.7154 0.2948 0.3716 0.040 Uiso 1 1 d . . . 
H4A1 H 0.5871 0.4046 0.1587 0.040 Uiso 1 1 d . . . 
H4A2 H 0.4407 0.4541 0.1367 0.040 Uiso 1 1 d . . . 
H3B1 H 1.1211 0.1055 0.3460 0.040 Uiso 1 1 d . . . 
H3B2 H 1.2105 -0.0444 0.3744 0.040 Uiso 1 1 d . . . 
H4B1 H 1.0786 0.0828 0.1000 0.040 Uiso 1 1 d . . . 
H4B2 H 1.0049 0.2085 0.1336 0.040 Uiso 1 1 d . . . 
H3C1 H 0.9722 0.6127 0.3758 0.040 Uiso 1 1 d . . . 
H3C2 H 0.9167 0.5233 0.3534 0.040 Uiso 1 1 d . . . 
H4C1 H 0.8006 0.6178 0.1418 0.040 Uiso 1 1 d . . . 
H4C2 H 0.8207 0.7335 0.1038 0.040 Uiso 1 1 d . . . 
H1WA H 1.0528 -0.1229 0.0718 0.040 Uiso 1 1 d . . . 
H1WB H 1.1560 -0.0767 0.0390 0.040 Uiso 1 1 d . . . 
 
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 
N1 0.0219(5) 0.0198(5) 0.0186(5) -0.0018(4) -0.0020(4) -0.0087(4) 
C1A 0.0263(6) 0.0270(6) 0.0183(6) -0.0045(5) 0.0012(5) -0.0127(5) 
C2A 0.0256(6) 0.0235(6) 0.0236(6) -0.0007(5) -0.0032(5) -0.0113(5) 
N3A 0.0266(5) 0.0223(5) 0.0245(5) -0.0026(4) -0.0023(4) -0.0124(5) 
C3A 0.0294(6) 0.0223(6) 0.0278(6) -0.0034(5) -0.0031(5) -0.0138(5) 
C4A 0.0255(6) 0.0229(6) 0.0251(6) -0.0023(5) -0.0011(5) -0.0154(5) 
C5A 0.0285(6) 0.0259(6) 0.0264(6) -0.0057(5) 0.0043(5) -0.0149(6) 
C6A 0.0229(6) 0.0258(7) 0.0328(7) -0.0044(5) 0.0041(5) -0.0092(5) 
C7A 0.0248(6) 0.0271(7) 0.0274(6) 0.0003(5) -0.0016(5) -0.0127(6) 
C8A 0.0275(6) 0.0229(6) 0.0233(6) -0.0033(5) 0.0012(5) -0.0157(5) 
C9A 0.0234(6) 0.0216(6) 0.0282(6) -0.0039(5) 0.0014(5) -0.0121(5) 
C10A 0.0309(7) 0.0214(6) 0.0242(6) -0.0026(5) 0.0007(5) -0.0138(5) 
N4A 0.0241(5) 0.0223(5) 0.0224(5) -0.0034(4) -0.0004(4) -0.0126(4) 
C11A 0.0272(6) 0.0255(6) 0.0229(6) -0.0065(5) 0.0008(5) -0.0147(5) 
C12A 0.0268(6) 0.0271(6) 0.0201(6) -0.0015(5) -0.0046(5) -0.0145(5) 
N2 0.0242(5) 0.0227(5) 0.0185(5) -0.0019(4) -0.0011(4) -0.0130(4) 
C1B 0.0259(6) 0.0215(6) 0.0230(6) -0.0005(5) -0.0044(5) -0.0085(5) 
C2B 0.0222(6) 0.0238(6) 0.0296(7) -0.0059(5) -0.0031(5) -0.0089(5) 
N3B 0.0247(5) 0.0259(6) 0.0305(6) -0.0086(4) 0.0033(4) -0.0131(5) 
C3B 0.0271(7) 0.0414(8) 0.0381(8) -0.0167(6) 0.0084(6) -0.0193(6) 
C4B 0.0222(6) 0.0305(7) 0.0333(7) -0.0115(5) 0.0072(5) -0.0143(6) 
C5B 0.0295(7) 0.0288(7) 0.0338(7) -0.0036(5) 0.0051(6) -0.0142(6) 
C6B 0.0354(7) 0.0235(7) 0.0409(8) -0.0081(6) 0.0063(6) -0.0161(6) 
C7B 0.0293(7) 0.0298(7) 0.0341(7) -0.0100(6) 0.0045(5) -0.0162(6) 
C8B 0.0197(6) 0.0265(7) 0.0345(7) -0.0036(5) 0.0012(5) -0.0123(5) 
C9B 0.0222(6) 0.0222(6) 0.0417(8) -0.0090(5) 0.0043(5) -0.0112(5) 
C10B 0.0251(7) 0.0347(8) 0.0420(8) 0.0029(6) -0.0033(6) -0.0186(6) 
N4B 0.0235(5) 0.0265(6) 0.0273(5) -0.0044(4) 0.0031(4) -0.0133(5) 
C11B 0.0265(6) 0.0293(7) 0.0273(6) -0.0032(5) 0.0046(5) -0.0151(6) 
C12B 0.0299(7) 0.0309(7) 0.0211(6) -0.0078(5) 0.0019(5) -0.0148(6) 
C1C 0.0263(6) 0.0222(6) 0.0218(6) -0.0025(5) -0.0044(5) -0.0111(5) 
C2C 0.0257(6) 0.0229(6) 0.0222(6) -0.0038(5) -0.0003(5) -0.0095(5) 
N3C 0.0243(5) 0.0207(5) 0.0230(5) -0.0018(4) -0.0019(4) -0.0086(4) 
C3C 0.0262(6) 0.0241(7) 0.0275(7) 0.0003(5) -0.0017(5) -0.0036(5) 
C4C 0.0238(6) 0.0193(6) 0.0264(6) -0.0013(5) -0.0011(5) -0.0049(5) 
C5C 0.0272(7) 0.0263(7) 0.0326(7) -0.0037(5) -0.0059(5) -0.0103(6) 
C6C 0.0265(7) 0.0320(7) 0.0379(8) -0.0024(6) 0.0007(6) -0.0153(6) 
C7C 0.0270(6) 0.0254(7) 0.0274(7) -0.0014(5) 0.0030(5) -0.0091(6) 
C8C 0.0244(6) 0.0193(6) 0.0271(6) -0.0047(5) -0.0019(5) -0.0055(5) 
C9C 0.0237(6) 0.0221(6) 0.0299(7) -0.0020(5) -0.0004(5) -0.0099(5) 
C10C 0.0278(7) 0.0287(7) 0..0307(7) -0.0068(5) -0.0039(5) -0.0081(6) 
N4C 0.0272(6) 0.0291(6) 0.0264(5) -0.0051(4) 0.0004(4) -0.0159(5) 
C11C 0.0326(7) 0.0237(6) 0.0304(7) -0.0013(5) -0.0092(5) -0.0131(6) 
C12C 0.0342(7) 0.0276(7) 0.0210(6) 0.0011(5) -0.0019(5) -0.0189(6) 
N11 0.0364(6) 0.0367(7) 0.0179(5) -0.0016(4) -0.0035(4) -0.0194(6) 
O11 0.0306(5) 0.0334(6) 0.0345(5) 0.0004(4) -0.0064(4) -0.0115(5) 
O12 0.0418(6) 0.0346(6) 0.0334(5) -0.0099(4) -0.0007(4) -0.0212(5) 
O13 0.0367(6) 0.0420(6) 0.0302(5) -0.0042(4) 0.0017(4) -0.0241(5) 
N21 0.0305(6) 0.0355(6) 0.0188(5) -0.0032(4) -0.0028(4) -0.0165(5) 
O21 0.0295(5) 0.0326(5) 0.0282(5) -0.0083(4) 0.0020(4) -0.0126(4) 
O22 0.0341(5) 0.0292(5) 0.0280(5) -0.0013(4) 0.0000(4) -0.0144(4) 
O23 0.0307(5) 0.0468(6) 0.0395(6) -0.0097(5) -0.0022(4) -0.0229(5) 
N31 0.0352(6) 0.0251(6) 0.0311(6) -0.0061(5) 0.0034(5) -0.0080(5) 
O31 0.0430(7) 0.0481(7) 0.0596(8) -0.0036(6) -0.0124(6) -0.0141(6) 
O32 0.0599(8) 0.0389(6) 0.0466(7) -0.0044(5) 0.0158(6) -0.0261(6) 
O33 0.0829(10) 0.0494(7) 0.0324(6) 0.0052(5) -0.0113(6) -0.0375(7) 
N41 0.0353(6) 0.0320(6) 0.0341(6) -0.0101(5) 0.0025(5) -0.0201(6) 
O41 0.0519(7) 0.0495(7) 0.0382(6) 0.0016(5) 0.0034(5) -0.0290(6) 
O42 0.0313(6) 0.0438(7) 0.0656(8) -0.0021(6) 0.0004(5) -0.0122(5) 
O43 0.0354(6) 0.0374(6) 0.0477(6) -0.0122(5) 0.0106(5) -0.0203(5) 
N51 0.0298(6) 0.0301(6) 0.0220(5) -0.0025(4) -0.0003(4) -0.0155(5) 
O51 0.0692(9) 0.0318(6) 0.0706(9) 0.0006(6) -0.0272(7) -0.0298(6) 
O52 0.0352(6) 0.0282(5) 0.0600(7) -0.0052(5) -0.0143(5) -0.0154(5) 
O53 0.0248(5) 0.0445(6) 0.0329(5) -0.0041(4) 0.0002(4) -0.0130(5) 
N61 0.0323(6) 0.0280(6) 0.0204(5) -0.0071(4) -0.0017(4) -0.0123(5) 
O61 0.0426(7) 0.0373(6) 0.0613(8) -0.0231(6) -0.0187(6) 0.0009(5) 
O62 0.0430(6) 0.0457(6) 0.0366(6) -0.0051(5) 0.0003(5) -0.0309(5) 
O63 0.0335(5) 0.0285(5) 0.0551(7) -0.0105(5) -0.0016(5) -0.0159(5) 
O1W 0.0500(7) 0.0372(6) 0.0448(6) -0.0140(5) 0.0086(5) -0.0264(5) 
O2W 0.0304(11) 0.0253(11) 0.0380(13) -0.0041(9) -0.0026(9) -0.0095(9) 
O2W' 0.0389(14) 0.0400(15) 0.0474(15) -0.0157(12) -0.0064(11) -0.0083(11) 
 
_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 C1A 1.4749(16) . ? 
N1 C1B 1.4753(16) . ? 
N1 C1C 1.4769(16) . ? 
C1A C2A 1.5167(18) . ? 
C2A N3A 1.4940(16) . ? 
N3A C3A 1.4939(16) . ? 
C3A C4A 1.5028(18) . ? 
C4A C5A 1.3884(19) . ? 
C4A C9A 1.3917(18) . ? 
C5A C6A 1.390(2) . ? 
C6A C7A 1.3878(19) . ? 
C7A C8A 1.3884(19) . ? 
C8A C9A 1.3929(18) . ? 
C8A C10A 1.5076(18) . ? 
C10A N4A 1.4929(16) . ? 
N4A C11A 1.4892(16) . ? 
C11A C12A 1.5130(18) . ? 
C12A N2 1.4775(15) . ? 
N2 C12B 1.4726(17) . ? 
N2 C12C 1.4769(16) . ? 
C1B C2B 1.5142(18) . ? 
C2B N3B 1.4936(17) . ? 
N3B C3B 1.4892(17) . ? 
C3B C4B 1.510(2) . ? 
C4B C9B 1.389(2) . ? 
C4B C5B 1.391(2) . ? 
C5B C6B 1.390(2) . ? 
C6B C7B 1.387(2) . ? 
C7B C8B 1.3896(19) . ? 
C8B C9B 1.391(2) . ? 
C8B C10B 1.5046(19) . ? 
C10B N4B 1.4885(17) . ? 
N4B C11B 1.4943(17) . ? 
C11B C12B 1.5200(19) . ? 
C1C C2C 1.5178(17) . ? 
C2C N3C 1.4910(16) . ? 
N3C C3C 1.4992(16) . ? 
C3C C4C 1.5066(18) . ? 
C4C C9C 1.3889(19) . ? 
C4C C5C 1.392(2) . ? 
C5C C6C 1.386(2) . ? 
C6C C7C 1.386(2) . ? 
C7C C8C 1.3915(19) . ? 
C8C C9C 1.3905(18) . ? 
C8C C10C 1.5057(19) . ? 
C10C N4C 1.4900(18) . ? 
N4C C11C 1.4950(17) . ? 
C11C C12C 1.513(2) . ? 
N11 O11 1.2506(16) . ? 
N11 O13 1.2513(15) . ? 
N11 O12 1.2528(16) . ? 
N21 O23 1.2501(15) . ? 
N21 O22 1.2529(16) . ? 
N21 O21 1.2541(15) . ? 
N31 O32 1.2408(17) . ? 
N31 O31 1.2424(18) . ? 
N31 O33 1.2490(17) . ? 
N41 O43 1.2431(16) . ? 
N41 O41 1.2495(16) . ? 
N41 O42 1.2508(17) . ? 
N51 O51 1.2307(16) . ? 
N51 O52 1.2492(15) . ? 
N51 O53 1.2566(15) . ? 
N61 O61 1.2259(16) . ? 
N61 O63 1.2448(16) . ? 
N61 O62 1.2619(15) . ? 
O2W O2W' 0.823(3) . ? 
 
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 
C1A N1 C1B 108.59(10) . . ? 
C1A N1 C1C 108.72(10) . . ? 
C1B N1 C1C 108.16(10) . . ? 
N1 C1A C2A 114.04(10) . . ? 
N3A C2A C1A 112.11(11) . . ? 
C3A N3A C2A 111.47(10) . . ? 
N3A C3A C4A 112.27(10) . . ? 
C5A C4A C9A 119.38(12) . . ? 
C5A C4A C3A 120.83(12) . . ? 
C9A C4A C3A 119.73(12) . . ? 
C4A C5A C6A 120.13(12) . . ? 
C7A C6A C5A 120.32(12) . . ? 
C6A C7A C8A 119.89(12) . . ? 
C7A C8A C9A 119.63(12) . . ? 
C7A C8A C10A 121.28(12) . . ? 
C9A C8A C10A 119.09(12) . . ? 
C4A C9A C8A 120.58(12) . . ? 
N4A C10A C8A 111.08(10) . . ? 
C11A N4A C10A 112.26(10) . . ? 
N4A C11A C12A 111.98(10) . . ? 
N2 C12A C11A 113.36(10) . . ? 
C12B N2 C12C 109.10(10) . . ? 
C12B N2 C12A 108.08(10) . . ? 
C12C N2 C12A 108.09(10) . . ? 
N1 C1B C2B 113.99(10) . . ? 
N3B C2B C1B 111.37(11) . . ? 
C3B N3B C2B 111.94(10) . . ? 
N3B C3B C4B 112.53(11) . . ? 
C9B C4B C5B 119.17(13) . . ? 
C9B C4B C3B 119.16(13) . . ? 
C5B C4B C3B 121.63(14) . . ? 
C6B C5B C4B 119.92(14) . . ? 
C7B C6B C5B 120.52(13) . . ? 
C6B C7B C8B 119.99(13) . . ? 
C7B C8B C9B 119.16(13) . . ? 
C7B C8B C10B 121.27(13) . . ? 
C9B C8B C10B 119.50(13) . . ? 
C4B C9B C8B 121.18(13) . . ? 
N4B C10B C8B 112.54(11) . . ? 
C10B N4B C11B 111.04(10) . . ? 
N4B C11B C12B 111.90(10) . . ? 
N2 C12B C11B 114.04(11) . . ? 
N1 C1C C2C 113.44(10) . . ? 
N3C C2C C1C 112.38(10) . . ? 
C2C N3C C3C 111.57(10) . . ? 
N3C C3C C4C 112.51(11) . . ? 
C9C C4C C5C 119.26(12) . . ? 
C9C C4C C3C 119.36(12) . . ? 
C5C C4C C3C 121.33(13) . . ? 
C6C C5C C4C 120.23(13) . . ? 
C7C C6C C5C 120.14(13) . . ? 
C6C C7C C8C 120.23(13) . . ? 
C9C C8C C7C 119.23(12) . . ? 
C9C C8C C10C 119.14(12) . . ? 
C7C C8C C10C 121.58(12) . . ? 
C4C C9C C8C 120.85(12) . . ? 
N4C C10C C8C 112.45(11) . . ? 
C10C N4C C11C 111.15(11) . . ? 
N4C C11C C12C 111.55(11) . . ? 
N2 C12C C11C 113.04(11) . . ? 
O11 N11 O13 120.01(12) . . ? 
O11 N11 O12 119.80(12) . . ? 
O13 N11 O12 120.10(12) . . ? 
O23 N21 O22 120.19(12) . . ? 
O23 N21 O21 119.91(12) . . ? 
O22 N21 O21 119.82(11) . . ? 
O32 N31 O31 120.70(14) . . ? 
O32 N31 O33 119.40(14) . . ? 
O31 N31 O33 119.85(14) . . ? 
O43 N41 O41 120.08(13) . . ? 
O43 N41 O42 120.46(13) . . ? 
O41 N41 O42 119.45(13) . . ? 
O51 N51 O52 119.29(12) . . ? 
O51 N51 O53 121.56(12) . . ? 
O52 N51 O53 119.12(12) . . ? 
O61 N61 O63 121.01(13) . . ? 
O61 N61 O62 119.80(13) . . ? 
O63 N61 O62 119.18(12) . . ? 
 
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 
C1B N1 C1A C2A -80.66(13) . . . . ? 
C1C N1 C1A C2A 161.89(10) . . . . ? 
N1 C1A C2A N3A -78.79(14) . . . . ? 
C1A C2A N3A C3A 175.83(10) . . . . ? 
C2A N3A C3A C4A 179.27(11) . . . . ? 
N3A C3A C4A C5A -65.58(16) . . . . ? 
N3A C3A C4A C9A 117.32(13) . . . . ? 
C9A C4A C5A C6A 1.15(19) . . . . ? 
C3A C4A C5A C6A -175.96(12) . . . . ? 
C4A C5A C6A C7A 1.3(2) . . . . ? 
C5A C6A C7A C8A -2.7(2) . . . . ? 
C6A C7A C8A C9A 1.57(19) . . . . ? 
C6A C7A C8A C10A -178.59(12) . . . . ? 
C5A C4A C9A C8A -2.28(18) . . . . ? 
C3A C4A C9A C8A 174.86(11) . . . . ? 
C7A C8A C9A C4A 0.93(19) . . . . ? 
C10A C8A C9A C4A -178.91(11) . . . . ? 
C7A C8A C10A N4A 69.90(15) . . . . ? 
C9A C8A C10A N4A -110.26(13) . . . . ? 
C8A C10A N4A C11A 175.07(11) . . . . ? 
C10A N4A C11A C12A -175..23(10) . . . . ? 
N4A C11A C12A N2 79.70(13) . . . . ? 
C11A C12A N2 C12B 82.21(13) . . . . ? 
C11A C12A N2 C12C -159.84(11) . . . . ? 
C1A N1 C1B C2B 161.25(10) . . . . ? 
C1C N1 C1B C2B -80.93(13) . . . . ? 
N1 C1B C2B N3B -83.87(13) . . . . ? 
C1B C2B N3B C3B -178.26(11) . . . . ? 
C2B N3B C3B C4B -174.07(12) . . . . ? 
N3B C3B C4B C9B 104.78(15) . . . . ? 
N3B C3B C4B C5B -77.33(17) . . . . ? 
C9B C4B C5B C6B 0.3(2) . . . . ? 
C3B C4B C5B C6B -177.60(13) . . . . ? 
C4B C5B C6B C7B 1.4(2) . . . . ? 
C5B C6B C7B C8B -1.0(2) . . . . ? 
C6B C7B C8B C9B -1.0(2) . . . . ? 
C6B C7B C8B C10B 176.22(12) . . . . ? 
C5B C4B C9B C8B -2.3(2) . . . . ? 
C3B C4B C9B C8B 175.62(12) . . . . ? 
C7B C8B C9B C4B 2.66(19) . . . . ? 
C10B C8B C9B C4B -174.57(12) . . . . ? 
C7B C8B C10B N4B 70.80(17) . . . . ? 
C9B C8B C10B N4B -112.03(14) . . . . ? 
C8B C10B N4B C11B 177.61(12) . . . . ? 
C10B N4B C11B C12B -178.29(12) . . . . ? 
C12C N2 C12B C11B 79.25(13) . . . . ? 
C12A N2 C12B C11B -163.45(10) . .. . . ? 
N4B C11B C12B N2 81.59(14) . . . . ? 
C1A N1 C1C C2C -77.01(13) . . . . ? 
C1B N1 C1C C2C 165.25(10) . . . . ? 
N1 C1C C2C N3C -83.88(13) . . . . ? 
C1C C2C N3C C3C 173.39(11) . . . . ? 
C2C N3C C3C C4C -177.05(11) . . . . ? 
N3C C3C C4C C9C 108.09(14) . . . . ? 
N3C C3C C4C C5C -74.47(16) . . . . ? 
C9C C4C C5C C6C 0.4(2) . . . . ? 
C3C C4C C5C C6C -177.07(13) . . . . ? 
C4C C5C C6C C7C 1.0(2) . . . . ? 
C5C C6C C7C C8C -0.5(2) . . . . ? 
C6C C7C C8C C9C -1.4(2) . . . . ? 
C6C C7C C8C C10C 176.03(13) . . . . ? 
C5C C4C C9C C8C -2.3(2) . . . . ? 
C3C C4C C9C C8C 175.24(12) . . . . ? 
C7C C8C C9C C4C 2.7(2) . . . . ? 
C10C C8C C9C C4C -174.72(12) . . . . ? 
C9C C8C C10C N4C -108.32(14) . . . . ? 
C7C C8C C10C N4C 74.28(16) . . . . ? 
C8C C10C N4C C11C 178.61(11) . . . . ? 
C10C N4C C11C C12C -178.35(11) . . . . ? 
C12B N2 C12C C11C -164.68(11) . . . . ? 
C12A N2 C12C C11C 78.02(13) . . . . ? 
N4C C11C C12C N2 87.99(13) . . . . ? 
 
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 
N3A H3A1 O2W  0.96 1.85 2.769(3) 159.2 1_455 
N3A H3A1 O2W'  0.96 1.86 2.730(3) 148.2 1_455 
N3A H3A2 O11  0.89 2.02 2.8819(15) 162.8 . 
N3A H3A2 O12  0.89 2.31 3.0244(15) 137.2 . 
N4A H4A1 O21  0.94 1.90 2.8415(14) 175.4 . 
N4A H4A1 O22  0.94 2.35 2.9882(15) 124.5 . 
N4A H4A2 O52  0.92 1.89 2.8058(15) 175.1 . 
N3B H3B1 O12  0.88 1.97 2.8384(16) 170.4 . 
N3B H3B1 O13  0.88 2.39 3.0386(16) 130.4 . 
N3B H3B2 O62  0.95 1.91 2.8582(16) 171.9 1_545 
N4B H4B1 O1W  0.93 1.77 2.6632(16) 159.6 . 
N4B H4B2 O22  0.89 1.99 2.8595(15) 164.1 . 
N4B H4B2 O23  0.89 2.33 3.0350(16) 136.0 . 
N3C H3C1 O63  0.93 1.92 2.8209(15) 162.1 . 
N3C H3C2 O13  0.91 1.98 2.8781(16) 169.5 . 
N3C H3C2 O11  0.91 2.28 2.9518(15) 129.8 . 
N4C H4C1 O23  0.92 1.99 2.8968(16) 170.9 . 
N4C H4C1 O21  0.92 2.33 2.9814(15) 127.5 . 
N4C H4C2 O53  0.88 2.11 2.8992(15) 149.2 1_655 
N4C H4C2 O42  0.88 2.48 3.0580(18) 123.8 1_565 
O1W H1WA O53  0.94 1.91 2.8467(16) 171.5 1_645 
O1W H1WA O52  0.94 2.64 3.2076(16) 119.0 1_645 
O1W H1WB O41  0.93 1.99 2.8877(17) 161.8 2_755 
O1W H1WB O42  0.93 2.47 3.1837(17) 133.4 2_755 
 
_diffrn_measured_fraction_theta_max    0.973 
_diffrn_reflns_theta_full              27.50 
_diffrn_measured_fraction_theta_full   0.973 
_refine_diff_density_max    0.436 
_refine_diff_density_min   -0.232 
_refine_diff_density_rms    0.045