  
data_08032b 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety    'C15 H16 N6 O4 S, 2(H2 O)'
_chemical_formula_sum       'C15 H20 N6 O6 S' 
_chemical_formula_weight          412.43 
  
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' 
 'S'  'S'   0.1246   0.1234 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Orthorhombic 
_symmetry_space_group_name_H-M    'P 21 21 21' 
_symmetry_space_group_name_Hall   'P 2ac 2ab' 
  
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' 
  
_cell_length_a                    4.8367(6) 
_cell_length_b                    12.1128(18) 
_cell_length_c                    30.967(5) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      1814.2(5) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     66011
_cell_measurement_theta_min       2.04 
_cell_measurement_theta_max       25.03 
  
_exptl_crystal_description        needle
_exptl_crystal_colour             colourless 
_exptl_crystal_size_max           0.75 
_exptl_crystal_size_mid           0.13 
_exptl_crystal_size_min           0.03 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.510 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              864 
_exptl_absorpt_coefficient_mu     0.227 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.8482 
_exptl_absorpt_correction_T_max   0.9943 
_exptl_absorpt_process_details    'DENZO-SMN (Otwinowski & Minor, 1997)' 
  
_exptl_special_details 
; 
Only low quality crystals could be obtained and a theta(max)
of 25 deg could not be collected. 
; 
  
_diffrn_ambient_temperature       150(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   'Nonius Kappa-CCD' 
_diffrn_measurement_method        'φ scans, and ω scans with κ offsets' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          0 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             6165
_diffrn_reflns_av_R_equivalents   0.0910 
_diffrn_reflns_av_sigmaI/netI     0.0524 
_diffrn_reflns_limit_h_min        -4 
_diffrn_reflns_limit_h_max        4 
_diffrn_reflns_limit_k_min        -11 
_diffrn_reflns_limit_k_max        10 
_diffrn_reflns_limit_l_min        -27 
_diffrn_reflns_limit_l_max        27 
_diffrn_reflns_theta_min          2.59 
_diffrn_reflns_theta_max          18.84 
_reflns_number_total              1347 
_reflns_number_gt                 1113 
_reflns_threshold_expression      I>2σ(I) 
  
_computing_data_collection        'COLLECT (Nonius, 1997-2001)' 
_computing_cell_refinement        'DENZO-SMN (Otwinowski & Minor, 1997)' 
_computing_data_reduction         DENZO-SMN 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'SHELXTL/PC (Sheldrick, 2001)' 
_computing_publication_material   SHELXTL/PC 
  
_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)+(0.0294P)²+6.6721P] 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_abs_structure_details 
 'Flack H D (1983), 474 Fridel pairs, Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.0(3)
_chemical_absolute_configuration  'ad' 
_refine_ls_number_reflns          1347 
_refine_ls_number_parameters      279 
_refine_ls_number_restraints      366 
_refine_ls_R_factor_all           0.0752 
_refine_ls_R_factor_gt            0.0526 
_refine_ls_wR_factor_ref          0.1196 
_refine_ls_wR_factor_gt           0.1052 
_refine_ls_goodness_of_fit_ref    1.086 
_refine_ls_restrained_S_all       0.950 
_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 
S1A S -0.7458(9) 0.7019(4) 0.94736(14) 0.0462(11) Uani 0.75 1 d PDU A 1 
C2A C -0.496(5) 0.6160(17) 0.9261(8) 0.040(5) Uani 0.75 1 d PDU A 1 
H2A H -0.4325 0.6203 0.8971 0.048 Uiso 0.75 1 calc PR A 1 
C3A C -0.3999(17) 0.5425(7) 0.9550(3) 0.037(2) Uani 0.75 1 d PDU A 1 
C4A C -0.537(8) 0.547(3) 0.9956(7) 0.041(4) Uani 0.75 1 d PDU A 1 
H4A H -0.4991 0.4979 1.0187 0.049 Uiso 0.75 1 calc PR A 1 
C5A C -0.723(5) 0.6271(15) 0.9978(7) 0.044(3) Uani 0.75 1 d PDU A 1 
H5A H -0.8305 0.6431 1.0226 0.053 Uiso 0.75 1 calc PR A 1 
S1B S -0.762(5) 0.6509(16) 0.9958(6) 0.0462(11) Uani 0.25 1 d PDU A 2 
C2B C -0.51(2) 0.552(10) 0.9945(18) 0.041(4) Uani 0.25 1 d PDU A 2 
H2B H -0.4534 0.5087 1.0187 0.049 Uiso 0.25 1 calc PR A 2 
C3B C -0.3999(17) 0.5425(7) 0.9550(3) 0.037(2) Uani 0.25 1 d PDU A 2 
C4B C -0.462(16) 0.632(5) 0.927(2) 0.040(5) Uani 0.25 1 d PDU A 2 
H4B H -0.3622 0.6477 0.9011 0.048 Uiso 0.25 1 calc PR A 2 
C5B C -0.674(12) 0.691(5) 0.9409(13) 0.044(3) Uani 0.25 1 d PDU A 2 
H5B4 H -0.7665 0.7467 0.9247 0.053 Uiso 0.25 1 calc PR A 2 
N6 N -0.1902(13) 0.4624(5) 0.9454(2) 0.0295(16) Uani 1 1 d U . . 
N7 N -0.1453(15) 0.3792(6) 0.9732(2) 0.044(2) Uani 1 1 d U A . 
N8 N 0.0510(14) 0.3176(6) 0.9559(2) 0.0406(19) Uani 1 1 d U . . 
C9 C 0.1254(16) 0.3627(6) 0.9171(3) 0.030(2) Uani 1 1 d U A . 
C10 C -0.0360(16) 0.4553(7) 0.9097(3) 0.035(2) Uani 1 1 d U A . 
H10A H -0.0369 0.5024 0.8851 0.042 Uiso 1 1 calc R . . 
C11 C 0.3425(17) 0.3159(6) 0.8894(3) 0.030(2) Uani 1 1 d U . . 
C12 C 0.4717(16) 0.2114(6) 0.8974(3) 0.030(2) Uani 1 1 d U A . 
N13 N 0.6626(13) 0.1698(5) 0.8704(2) 0.0307(17) Uani 1 1 d U . . 
C14 C 0.7502(19) 0.2284(6) 0.8349(3) 0.028(2) Uani 1 1 d U A . 
N15 N 0.6300(13) 0.3310(5) 0.82723(19) 0.0239(16) Uani 1 1 d U . . 
C16 C 0.4361(15) 0.3718(7) 0.8544(3) 0.027(2) Uani 1 1 d U A . 
H16A H 0.3622 0.4430 0.8487 0.032 Uiso 1 1 calc R . . 
N17 N 0.4080(13) 0.1508(5) 0.9314(2) 0.042(2) Uani 1 1 d U . . 
H17A H 0.4895 0.0867 0.9355 0.050 Uiso 1 1 calc R A . 
H17B H 0.2841 0.1746 0.9500 0.050 Uiso 1 1 calc R . . 
O18 O 0.9257(12) 0.1921(4) 0.80998(19) 0.0453(17) Uani 1 1 d U . . 
C19 C 0.7335(17) 0.3977(6) 0.7911(3) 0.0289(19) Uani 1 1 d U A . 
H19A H 0.8677 0.3533 0.7737 0.035 Uiso 1 1 calc R . . 
O20 O 0.8734(10) 0.4918(4) 0.80977(17) 0.0300(14) Uani 1 1 d U . . 
C21 C 0.8477(17) 0.5854(6) 0.7799(3) 0.029(2) Uani 1 1 d U A . 
H21A H 1.0353 0.6038 0.7684 0.035 Uiso 1 1 calc R . . 
C22 C 0.6712(16) 0.5438(6) 0.7433(3) 0.033(2) Uani 1 1 d U . . 
H22A H 0.5392 0.6021 0.7334 0.039 Uiso 1 1 calc R A . 
C23 C 0.5179(17) 0.4459(6) 0.7618(3) 0.0312(19) Uani 1 1 d U A . 
H23A H 0.3517 0.4693 0.7781 0.037 Uiso 1 1 calc R . . 
H23B H 0.4631 0.3931 0.7389 0.037 Uiso 1 1 calc R . . 
C24 C 0.7436(16) 0.6820(6) 0.8053(3) 0.035(2) Uani 1 1 d U . . 
H24A H 0.8601 0.6925 0.8312 0.042 Uiso 1 1 calc R A . 
H24B H 0.7559 0.7497 0.7875 0.042 Uiso 1 1 calc R . . 
O25 O 0.4647(11) 0.6642(4) 0.8179(2) 0.0456(17) Uani 1 1 d U A . 
H25A H 0.4052 0.7205 0.8308 0.068 Uiso 1 1 calc R . . 
O26 O 0.8329(12) 0.5036(4) 0.70816(19) 0.0425(16) Uani 1 1 d U A . 
H26A H 0.9261 0.5556 0.6977 0.064 Uiso 1 1 calc R . . 
O31 O 0.6868(14) 0.3647(5) 0.6428(2) 0.0477(17) Uani 1 1 d D . . 
H31A H 0.70(2) 0.398(7) 0.6679(17) 0.072 Uiso 1 1 d D . . 
H31B H 0.639(19) 0.328(7) 0.620(2) 0.072 Uiso 1 1 d D . . 
O41 O 0.2102(13) 0.4500(4) 0.6055(2) 0.0472(17) Uani 1 1 d D . . 
H41A H 0.204(19) 0.510(5) 0.621(2) 0.071 Uiso 1 1 d D . . 
H41B H 0.056(13) 0.416(7) 0.611(3) 0.071 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 
S1A C2A 1.725(16) . ? 
S1A C5A 1.808(16) . ? 
C2A C3A 1.35(2) . ? 
C2A H2A 0.9500 . ? 
C3A C4A 1.422(19) . ? 
C3A N6 1.435(10) . ? 
C4A C5A 1.32(2) . ? 
C4A H4A 0.9500 . ? 
C5A H5A 0.9500 . ? 
S1B C2B 1.72(3) . ? 
S1B C5B 1.82(2) . ? 
C2B H2B 0.9500 . ? 
C4B C5B 1.33(3) . ? 
C4B H4B 0.9500 . ? 
C5B H5B4 0.9500 . ? 
N6 C10 1.337(9) . ? 
N6 N7 1.342(8) . ? 
N7 N8 1.320(8) . ? 
N8 C9 1.368(10) . ? 
C9 C10 1.386(10) . ? 
C9 C11 1.469(11) . ? 
C10 H10A 0.9500 . ? 
C11 C16 1.356(10) . ? 
C11 C12 1.434(10) . ? 
C12 N17 1.319(9) . ? 
C12 N13 1.343(9) . ? 
N13 C14 1.377(9) . ? 
C14 O18 1.228(9) . ? 
C14 N15 1.392(9) . ? 
N15 C16 1.354(9) . ? 
N15 C19 1.468(9) . ? 
C16 H16A 0.9500 . ? 
N17 H17A 0.8800 . ? 
N17 H17B 0.8800 . ? 
C19 O20 1.446(8) . ? 
C19 C23 1.501(10) . ? 
C19 H19A 1.0000 . ? 
O20 C21 1.469(8) . ? 
C21 C24 1.496(10) . ? 
C21 C22 1.507(11) . ? 
C21 H21A 1.0000 . ? 
C22 O26 1.425(8) . ? 
C22 C23 1.511(10) . ? 
C22 H22A 1.0000 . ? 
C23 H23A 0.9900 . ? 
C23 H23B 0.9900 . ? 
C24 O25 1.421(9) . ? 
C24 H24A 0.9900 . ? 
C24 H24B 0.9900 . ? 
O25 H25A 0.8400 . ? 
O26 H26A 0.8400 . ? 
O31 H31A 0.87(4) . ? 
O31 H31B 0.87(4) . ? 
O41 H41A 0.88(4) . ? 
O41 H41B 0.87(4) . ? 
  
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
C2A S1A C5A 89.1(9) . . ? 
C3A C2A S1A 112.8(14) . . ? 
C3A C2A H2A 123.6 . . ? 
S1A C2A H2A 123.6 . . ? 
C2A C3A C4A 113.7(9) . . ? 
C2A C3A N6 123.6(11) . . ? 
C4A C3A N6 122.6(10) . . ? 
C5A C4A C3A 113.0(16) . . ? 
C5A C4A H4A 123.5 . . ? 
C3A C4A H4A 123.5 . . ? 
C4A C5A S1A 111.4(15) . . ? 
C4A C5A H5A 124.3 . . ? 
S1A C5A H5A 124.3 . . ? 
C2B S1B C5B 90.0(17) . . ? 
S1B C2B H2B 124.5 . . ? 
C5B C4B H4B 124.0 . . ? 
C4B C5B S1B 110(2) . . ? 
C4B C5B H5B4 125.0 . . ? 
S1B C5B H5B4 125.0 . . ? 
C10 N6 N7 113.1(7) . . ? 
C10 N6 C3A 127.5(7) . . ? 
N7 N6 C3A 119.3(7) . . ? 
N8 N7 N6 106.3(7) . . ? 
N7 N8 C9 108.6(7) . . ? 
N8 C9 C10 108.7(7) . . ? 
N8 C9 C11 123.1(7) . . ? 
C10 C9 C11 128.1(8) . . ? 
N6 C10 C9 103.2(7) . . ? 
N6 C10 H10A 128.4 . . ? 
C9 C10 H10A 128.4 . . ? 
C16 C11 C12 115.7(7) . . ? 
C16 C11 C9 120.9(7) . . ? 
C12 C11 C9 123.4(7) . . ? 
N17 C12 N13 116.6(7) . . ? 
N17 C12 C11 121.8(8) . . ? 
N13 C12 C11 121.5(7) . . ? 
C12 N13 C14 121.1(7) . . ? 
O18 C14 N13 122.0(8) . . ? 
O18 C14 N15 120.2(8) . . ? 
N13 C14 N15 117.9(7) . . ? 
C16 N15 C14 120.6(7) . . ? 
C16 N15 C19 120.6(6) . . ? 
C14 N15 C19 118.6(6) . . ? 
N15 C16 C11 123.1(7) . . ? 
N15 C16 H16A 118.4 . . ? 
C11 C16 H16A 118.4 . . ? 
C12 N17 H17A 120.0 . . ? 
C12 N17 H17B 120.0 . . ? 
H17A N17 H17B 120.0 . . ? 
O20 C19 N15 106.8(6) . . ? 
O20 C19 C23 105.1(5) . . ? 
N15 C19 C23 116.0(7) . . ? 
O20 C19 H19A 109.6 . . ? 
N15 C19 H19A 109.6 . . ? 
C23 C19 H19A 109.6 . . ? 
C19 O20 C21 108.5(5) . . ? 
O20 C21 C24 107.5(6) . . ? 
O20 C21 C22 105.3(6) . . ? 
C24 C21 C22 117.8(7) . . ? 
O20 C21 H21A 108.6 . . ? 
C24 C21 H21A 108.6 . . ? 
C22 C21 H21A 108.6 . . ? 
O26 C22 C21 112.2(6) . . ? 
O26 C22 C23 106.9(6) . . ? 
C21 C22 C23 104.8(7) . . ? 
O26 C22 H22A 110.9 . . ? 
C21 C22 H22A 110.9 . . ? 
C23 C22 H22A 110.9 . . ? 
C19 C23 C22 101.2(6) . . ? 
C19 C23 H23A 111.5 . . ? 
C22 C23 H23A 111.5 . . ? 
C19 C23 H23B 111.5 . . ? 
C22 C23 H23B 111.5 . . ? 
H23A C23 H23B 109.3 . . ? 
O25 C24 C21 110.3(6) . . ? 
O25 C24 H24A 109.6 . . ? 
C21 C24 H24A 109.6 . . ? 
O25 C24 H24B 109.6 . . ? 
C21 C24 H24B 109.6 . . ? 
H24A C24 H24B 108.1 . . ? 
C24 O25 H25A 109.5 . . ? 
C22 O26 H26A 109.5 . . ? 
H31A O31 H31B 168(9) . . ? 
H41A O41 H41B 104(9) . . ? 
  
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 
C5A S1A C2A C3A -2(2) . . . . ? 
S1A C2A C3A C4A 4(3) . . . . ? 
S1A C2A C3A N6 -179.6(10) . . . . ? 
C2A C3A C4A C5A -3(5) . . . . ? 
N6 C3A C4A C5A 180(3) . . . . ? 
C3A C4A C5A S1A 1(5) . . . . ? 
C2A S1A C5A C4A 0(3) . . . . ? 
C2B S1B C5B C4B -2(9) . . . . ? 
C2A C3A N6 C10 8.5(19) . . . . ? 
C4A C3A N6 C10 -175(3) . . . . ? 
C2A C3A N6 N7 -167.2(17) . . . . ? 
C4A C3A N6 N7 9(3) . . . . ? 
C10 N6 N7 N8 2.2(9) . . . . ? 
C3A N6 N7 N8 178.5(6) . . . . ? 
N6 N7 N8 C9 -0.5(9) . . . . ? 
N7 N8 C9 C10 -1.1(9) . . . . ? 
N7 N8 C9 C11 179.0(7) . . . . ? 
N7 N6 C10 C9 -2.8(9) . . . . ? 
C3A N6 C10 C9 -178.7(7) . . . . ? 
N8 C9 C10 N6 2.3(9) . . . . ? 
C11 C9 C10 N6 -177.8(7) . . . . ? 
N8 C9 C11 C16 -170.5(8) . . . . ? 
C10 C9 C11 C16 9.7(12) . . . . ? 
N8 C9 C11 C12 8.5(12) . . . . ? 
C10 C9 C11 C12 -171.3(8) . . . . ? 
C16 C11 C12 N17 177.1(7) . . . . ? 
C9 C11 C12 N17 -1.9(12) . . . . ? 
C16 C11 C12 N13 -3.4(11) . . . . ? 
C9 C11 C12 N13 177.6(7) . . . . ? 
N17 C12 N13 C14 -177.7(7) . . . . ? 
C11 C12 N13 C14 2.8(11) . . . . ? 
C12 N13 C14 O18 179.6(7) . . . . ? 
C12 N13 C14 N15 -1.5(10) . . . . ? 
O18 C14 N15 C16 179.9(7) . . . . ? 
N13 C14 N15 C16 0.9(10) . . . . ? 
O18 C14 N15 C19 -4.9(10) . . . . ? 
N13 C14 N15 C19 176.1(7) . . . . ? 
C14 N15 C16 C11 -1.8(10) . . . . ? 
C19 N15 C16 C11 -176.9(7) . . . . ? 
C12 C11 C16 N15 2.9(11) . . . . ? 
C9 C11 C16 N15 -178.1(7) . . . . ? 
C16 N15 C19 O20 64.2(8) . . . . ? 
C14 N15 C19 O20 -111.0(6) . . . . ? 
C16 N15 C19 C23 -52.6(9) . . . . ? 
C14 N15 C19 C23 132.2(7) . . . . ? 
N15 C19 O20 C21 -149.8(6) . . . . ? 
C23 C19 O20 C21 -26.0(8) . . . . ? 
C19 O20 C21 C24 129.3(6) . . . . ? 
C19 O20 C21 C22 2.9(8) . . . . ? 
O20 C21 C22 O26 -94.6(7) . . . . ? 
C24 C21 C22 O26 145.7(7) . . . . ? 
O20 C21 C22 C23 21.0(8) . . . . ? 
C24 C21 C22 C23 -98.7(8) . . . . ? 
O20 C19 C23 C22 38.0(8) . . . . ? 
N15 C19 C23 C22 155.6(6) . . . . ? 
O26 C22 C23 C19 83.3(7) . . . . ? 
C21 C22 C23 C19 -35.9(8) . . . . ? 
O20 C21 C24 O25 -69.4(8) . . . . ? 
C22 C21 C24 O25 49.2(9) . . . . ? 
  
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 
N17 H17A O41  0.88 2.54 3.261(8) 139.5 3_646 
N17 H17B N8  0.88 2.08 2.764(10) 134.4 . 
O25 H25A O31  0.84 1.98 2.813(8) 171.4 3_656 
O26 H26A O18  0.84 1.82 2.625(7) 160.8 3_756 
O31 H31A O26  0.87(4) 1.90(5) 2.724(8) 157(9) . 
O31 H31B O41  0.87(4) 2.59(9) 2.778(10) 93(6) . 
O41 H41A N13  0.88(4) 2.05(6) 2.833(8) 147(8) 3_656 
O41 H41B O31  0.87(4) 2.12(5) 2.968(9) 162(9) 1_455 
  
_diffrn_measured_fraction_theta_max    0.978 
_diffrn_reflns_theta_full              18.84 
_diffrn_measured_fraction_theta_full   0.978 
_refine_diff_density_max    0.244 
_refine_diff_density_min   -0.211 
_refine_diff_density_rms    0.054 
