 
data_kkam103m 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C27 H30 N10 O9' 
_chemical_formula_weight          638.61 
 
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                    8.9805(14) 
_cell_length_b                    13.021(2) 
_cell_length_c                    13.710(2) 
_cell_angle_alpha                 90.878(4) 
_cell_angle_beta                  108.591(3) 
_cell_angle_gamma                 102.259(4) 
_cell_volume                      1478.9(4) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     298(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ROD  
_exptl_crystal_colour             COLORLESS 
_exptl_crystal_size_max           0.33 
_exptl_crystal_size_mid           0.12 
_exptl_crystal_size_min           0.06 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.434 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              668 
_exptl_absorpt_coefficient_mu     0.111 
_exptl_absorpt_correction_type    'MULTI-SCAN' 
_exptl_absorpt_correction_T_min   0.9644 
_exptl_absorpt_correction_T_max   0.9934 
_exptl_absorpt_process_details    'SADABS' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       298(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   'BRUKER SMART CCD AREA DETECTOR' 
_diffrn_measurement_method        'PHI-OMEGA SCAN'  
_diffrn_detector_area_resol_mean  0.3  
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             8992 
_diffrn_reflns_av_R_equivalents   0.0287 
_diffrn_reflns_av_sigmaI/netI     0.1063 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -13 
_diffrn_reflns_limit_k_max        17 
_diffrn_reflns_limit_l_min        -18 
_diffrn_reflns_limit_l_max        16 
_diffrn_reflns_theta_min          1.57 
_diffrn_reflns_theta_max          28.26 
_reflns_number_total              6524 
_reflns_number_gt                 3093 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'BRUKER AXS SMART 3'  
_computing_cell_refinement        'BRUKER AXS SMART 3'  
_computing_data_reduction         'BRUKER AXS SAINT'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'BRUKER SHELXLTL'
_computing_publication_material   'MERCURY 1.4'
 
_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)+(0.0580P)²+0.0847P] 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          6524 
_refine_ls_number_parameters      535 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1793 
_refine_ls_R_factor_gt            0.0861 
_refine_ls_wR_factor_ref          0.1918 
_refine_ls_wR_factor_gt           0.1526 
_refine_ls_goodness_of_fit_ref    1.128 
_refine_ls_restrained_S_all       1.128 
_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 0.4643(4) 0.6955(2) 0.2509(2) 0.0360(8) Uani 1 1 d . . . 
C2A C 0.6148(6) 0.7355(4) 0.3363(4) 0.0454(12) Uani 1 1 d . . . 
C3A C 0.6326(6) 0.6690(4) 0.4261(3) 0.0470(11) Uani 1 1 d . . . 
N4A N 0.6171(5) 0.5614(3) 0.3929(3) 0.0531(10) Uani 1 1 d . . . 
C5A C 0.6793(5) 0.4926(3) 0.4535(3) 0.0444(10) Uani 1 1 d . . . 
O6A O 0.7646(4) 0.5155(2) 0.54471(19) 0.0630(9) Uani 1 1 d . . . 
N7A N 0.6436(5) 0.3921(3) 0.4064(3) 0.0563(11) Uani 1 1 d . . . 
C8A C 0.7027(5) 0.3056(3) 0.4503(3) 0.0437(10) Uani 1 1 d . . . 
C9A C 0.8562(6) 0.3154(4) 0.5166(3) 0.0523(12) Uani 1 1 d . . . 
C10A C 0.9097(6) 0.2267(4) 0.5543(3) 0.0563(13) Uani 1 1 d . . . 
C11A C 0.8004(6) 0.1293(4) 0.5259(3) 0.0529(12) Uani 1 1 d . . . 
C12A C 0.6490(6) 0.1175(4) 0.4608(3) 0.0503(12) Uani 1 1 d . . . 
C13A C 0.5965(7) 0.2065(4) 0.4237(3) 0.0528(13) Uani 1 1 d . . . 
N14A N 0.8628(7) 0.0360(4) 0.5632(3) 0.0696(13) Uani 1 1 d . . . 
O15A O 1.0066(5) 0.0453(3) 0.6057(3) 0.0964(14) Uani 1 1 d . . . 
O16A O 0.7603(6) -0.0477(3) 0.5519(3) 0.1055(15) Uani 1 1 d . . . 
C2B C 0.3313(5) 0.7387(3) 0.2624(3) 0.0378(10) Uani 1 1 d . . . 
C3B C 0.1682(5) 0.6707(3) 0.2039(3) 0.0453(11) Uani 1 1 d . . . 
N4B N 0.1363(4) 0.5723(2) 0.2498(2) 0.0433(9) Uani 1 1 d . . . 
C5B C 0.0087(5) 0.4946(3) 0.2022(3) 0.0359(9) Uani 1 1 d . . . 
O6B O -0.0843(4) 0.4982(2) 0.1150(2) 0.0598(9) Uani 1 1 d . . . 
N7B N -0.0078(4) 0.4099(3) 0.2599(3) 0.0474(10) Uani 1 1 d . . . 
C8B C -0.1238(5) 0.3145(3) 0.2331(3) 0.0367(9) Uani 1 1 d . . . 
C9B C -0.2697(5) 0.3002(3) 0.1558(3) 0.0446(11) Uani 1 1 d . . . 
C10B C -0.3774(6) 0.2028(4) 0.1339(3) 0.0519(12) Uani 1 1 d . . . 
C11B C -0.3338(5) 0.1212(3) 0.1911(3) 0.0423(10) Uani 1 1 d . . . 
C12B C -0.1917(5) 0.1339(3) 0.2685(3) 0.0393(10) Uani 1 1 d . . . 
C13B C -0.0827(5) 0.2302(3) 0.2890(3) 0.0419(10) Uani 1 1 d . . . 
N14B N -0.4514(5) 0.0199(3) 0.1711(3) 0.0645(11) Uani 1 1 d . . . 
O15B O -0.5668(5) 0.0031(3) 0.0938(3) 0.1114(15) Uani 1 1 d . . . 
O16B O -0.4246(5) -0.0438(3) 0.2342(3) 0.1032(14) Uani 1 1 d . . . 
C2C C 0.4831(6) 0.7088(3) 0.1496(3) 0.0459(11) Uani 1 1 d . . . 
C3C C 0.5053(5) 0.6098(4) 0.1026(3) 0.0470(11) Uani 1 1 d . . . 
N4C N 0.3586(4) 0.5253(3) 0.0712(3) 0.0473(9) Uani 1 1 d . . . 
C5C C 0.3385(5) 0.4377(3) 0.1209(3) 0.0429(10) Uani 1 1 d . . . 
O6C O 0.4428(3) 0.4216(2) 0.1996(2) 0.0564(8) Uani 1 1 d . . . 
N7C N 0.1994(4) 0.3648(3) 0.0730(3) 0.0462(9) Uani 1 1 d . . . 
C8C C 0.1503(5) 0.2628(3) 0.0970(3) 0.0413(10) Uani 1 1 d . . . 
C9C C 0.2450(6) 0.2120(4) 0.1707(3) 0.0513(12) Uani 1 1 d . . . 
C10C C 0.1896(6) 0.1095(4) 0.1864(4) 0.0533(12) Uani 1 1 d . . . 
C11C C 0.0334(6) 0.0575(3) 0.1330(3) 0.0464(11) Uani 1 1 d . . . 
C12C C -0.0661(6) 0.1054(3) 0.0614(3) 0.0461(11) Uani 1 1 d . . . 
C13C C -0.0098(5) 0.2079(3) 0.0441(3) 0.0442(10) Uani 1 1 d . . . 
N14C N -0.0258(6) -0.0517(3) 0.1514(3) 0.0615(11) Uani 1 1 d . . . 
O15C O 0.0735(5) -0.0972(3) 0.2074(3) 0.0850(12) Uani 1 1 d . . . 
O16C O -0.1700(5) -0.0926(3) 0.1103(3) 0.0901(12) Uani 1 1 d . . . 
H2A H 0.646(5) 0.813(3) 0.355(3) 0.055(12) Uiso 1 1 d . . . 
H2A' H 0.673(5) 0.731(3) 0.312(3) 0.032(14) Uiso 1 1 d . . . 
H3A H 0.728(4) 0.697(3) 0.486(3) 0.034(10) Uiso 1 1 d . . . 
H3A' H 0.551(4) 0.673(2) 0.456(2) 0.027(10) Uiso 1 1 d . . . 
H4A H 0.548(5) 0.542(3) 0.333(3) 0.044(12) Uiso 1 1 d . . . 
H7A H 0.576(4) 0.377(3) 0.351(3) 0.029(10) Uiso 1 1 d . . . 
H9A H 0.899(7) 0.381(4) 0.539(4) 0.10(2) Uiso 1 1 d . . . 
H10A H 1.017(5) 0.233(3) 0.598(3) 0.051(12) Uiso 1 1 d . . . 
H12A H 0.581(6) 0.049(4) 0.442(4) 0.087(17) Uiso 1 1 d . . . 
H13A H 0.512(5) 0.204(3) 0.381(3) 0.058(15) Uiso 1 1 d . . . 
H2B H 0.329(3) 0.811(2) 0.2380(19) 0.012(7) Uiso 1 1 d . . . 
H2B' H 0.347(4) 0.744(2) 0.334(2) 0.018(8) Uiso 1 1 d . . . 
H3B H 0.080(4) 0.711(3) 0.206(2) 0.034(9) Uiso 1 1 d . . . 
H3B' H 0.164(4) 0.650(3) 0.130(3) 0.039(10) Uiso 1 1 d . . . 
H4B H 0.225(5) 0.566(3) 0.312(3) 0.053(11) Uiso 1 1 d . . . 
H7B H 0.056(5) 0.417(3) 0.319(3) 0.055(13) Uiso 1 1 d . . . 
H9B H -0.279(5) 0.357(3) 0.119(3) 0.073(15) Uiso 1 1 d . . . 
H10B H -0.476(5) 0.194(3) 0.086(3) 0.068(14) Uiso 1 1 d . . . 
H12B H -0.191(5) 0.076(3) 0.312(3) 0.066(13) Uiso 1 1 d . . . 
H13B H 0.023(5) 0.239(3) 0.341(3) 0.072(14) Uiso 1 1 d . . . 
H2C H 0.392(5) 0.723(3) 0.092(3) 0.043(11) Uiso 1 1 d . . . 
H2C' H 0.562(4) 0.769(3) 0.155(2) 0.036(11) Uiso 1 1 d . . . 
H3C H 0.549(4) 0.628(3) 0.034(3) 0.059(12) Uiso 1 1 d . . . 
H3C' H 0.599(5) 0.581(3) 0.153(3) 0.063(13) Uiso 1 1 d . . . 
H4C H 0.276(4) 0.529(2) 0.010(2) 0.024(9) Uiso 1 1 d . . . 
H7C H 0.168(6) 0.381(4) 0.016(4) 0.083(18) Uiso 1 1 d . . . 
H9C H 0.358(7) 0.239(4) 0.189(4) 0.12(2) Uiso 1 1 d . . . 
H10C H 0.232(5) 0.071(3) 0.238(3) 0.060(13) Uiso 1 1 d . . . 
H12C H -0.181(5) 0.070(3) 0.027(3) 0.048(11) Uiso 1 1 d . . . 
H13C H -0.091(4) 0.240(3) -0.011(3) 0.047(10) Uiso 1 1 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 
N1 C2C 1.461(5) . ? 
N1 C2A 1.463(5) . ? 
N1 C2B 1.473(5) . ? 
C2A C3A 1.503(6) . ? 
C2A H2A 0.99(4) . ? 
C2A H2A' 0.72(3) . ? 
C3A N4A 1.431(5) . ? 
C3A H3A 0.98(4) . ? 
C3A H3A' 0.96(3) . ? 
N4A C5A 1.320(5) . ? 
N4A H4A 0.85(4) . ? 
C5A O6A 1.233(4) . ? 
C5A N7A 1.377(5) . ? 
N7A C8A 1.409(5) . ? 
N7A H7A 0.80(3) . ? 
C8A C9A 1.366(6) . ? 
C8A C13A 1.395(6) . ? 
C9A C10A 1.389(6) . ? 
C9A H9A 0.86(5) . ? 
C10A C11A 1.390(7) . ? 
C10A H10A 0.95(4) . ? 
C11A C12A 1.343(6) . ? 
C11A N14A 1.476(5) . ? 
C12A C13A 1.385(6) . ? 
C12A H12A 0.95(5) . ? 
C13A H13A 0.79(4) . ? 
N14A O15A 1.214(5) . ? 
N14A O16A 1.239(6) . ? 
C2B C3B 1.500(6) . ? 
C2B H2B 1.01(3) . ? 
C2B H2B' 0.95(3) . ? 
C3B N4B 1.451(5) . ? 
C3B H3B 1.05(3) . ? 
C3B H3B' 1.03(3) . ? 
N4B C5B 1.331(5) . ? 
N4B H4B 0.98(4) . ? 
C5B O6B 1.229(4) . ? 
C5B N7B 1.377(5) . ? 
N7B C8B 1.399(5) . ? 
N7B H7B 0.82(4) . ? 
C8B C9B 1.371(5) . ? 
C8B C13B 1.395(5) . ? 
C9B C10B 1.384(6) . ? 
C9B H9B 0.91(4) . ? 
C10B C11B 1.380(5) . ? 
C10B H10B 0.90(4) . ? 
C11B C12B 1.351(5) . ? 
C11B N14B 1.464(5) . ? 
C12B C13B 1.380(5) . ? 
C12B H12B 0.97(4) . ? 
C13B H13B 0.97(4) . ? 
N14B O15B 1.201(5) . ? 
N14B O16B 1.212(4) . ? 
C2C C3C 1.510(6) . ? 
C2C H2C 0.99(4) . ? 
C2C H2C' 0.92(4) . ? 
C3C N4C 1.463(5) . ? 
C3C H3C 1.14(4) . ? 
C3C H3C' 1.04(4) . ? 
N4C C5C 1.346(5) . ? 
N4C H4C 0.93(3) . ? 
C5C O6C 1.237(4) . ? 
C5C N7C 1.359(5) . ? 
N7C C8C 1.386(5) . ? 
N7C H7C 0.79(4) . ? 
C8C C9C 1.376(5) . ? 
C8C C13C 1.410(6) . ? 
C9C C10C 1.367(6) . ? 
C9C H9C 0.95(6) . ? 
C10C C11C 1.374(6) . ? 
C10C H10C 0.90(4) . ? 
C11C C12C 1.359(5) . ? 
C11C N14C 1.464(5) . ? 
C12C C13C 1.375(6) . ? 
C12C H12C 0.99(4) . ? 
C13C H13C 1.03(3) . ? 
N14C O16C 1.229(5) . ? 
N14C O15C 1.240(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 
C2C N1 C2A 112.9(4) . . ? 
C2C N1 C2B 112.5(3) . . ? 
C2A N1 C2B 111.8(3) . . ? 
N1 C2A C3A 112.8(4) . . ? 
N1 C2A H2A 117(2) . . ? 
C3A C2A H2A 115(2) . . ? 
N1 C2A H2A' 101(3) . . ? 
C3A C2A H2A' 110(3) . . ? 
H2A C2A H2A' 100(4) . . ? 
N4A C3A C2A 110.4(4) . . ? 
N4A C3A H3A 114(2) . . ? 
C2A C3A H3A 114.1(19) . . ? 
N4A C3A H3A' 109(2) . . ? 
C2A C3A H3A' 109.6(19) . . ? 
H3A C3A H3A' 99(3) . . ? 
C5A N4A C3A 124.4(4) . . ? 
C5A N4A H4A 122(3) . . ? 
C3A N4A H4A 113(2) . . ? 
O6A C5A N4A 123.5(4) . . ? 
O6A C5A N7A 121.8(4) . . ? 
N4A C5A N7A 114.6(3) . . ? 
C5A N7A C8A 126.7(3) . . ? 
C5A N7A H7A 119(2) . . ? 
C8A N7A H7A 114(2) . . ? 
C9A C8A C13A 120.0(4) . . ? 
C9A C8A N7A 122.9(4) . . ? 
C13A C8A N7A 117.1(4) . . ? 
C8A C9A C10A 120.3(5) . . ? 
C8A C9A H9A 110(4) . . ? 
C10A C9A H9A 128(4) . . ? 
C9A C10A C11A 117.9(5) . . ? 
C9A C10A H10A 120(2) . . ? 
C11A C10A H10A 122(2) . . ? 
C12A C11A C10A 122.9(4) . . ? 
C12A C11A N14A 120.3(5) . . ? 
C10A C11A N14A 116.6(4) . . ? 
C11A C12A C13A 118.8(5) . . ? 
C11A C12A H12A 119(3) . . ? 
C13A C12A H12A 122(3) . . ? 
C12A C13A C8A 120.0(5) . . ? 
C12A C13A H13A 123(3) . . ? 
C8A C13A H13A 116(3) . . ? 
O15A N14A O16A 124.1(4) . . ? 
O15A N14A C11A 119.7(5) . . ? 
O16A N14A C11A 116.1(5) . . ? 
N1 C2B C3B 112.7(3) . . ? 
N1 C2B H2B 114.7(16) . . ? 
C3B C2B H2B 105.3(16) . . ? 
N1 C2B H2B' 106.3(18) . . ? 
C3B C2B H2B' 110.4(19) . . ? 
H2B C2B H2B' 107(2) . . ? 
N4B C3B C2B 111.8(3) . . ? 
N4B C3B H3B 107.4(18) . . ? 
C2B C3B H3B 108.7(19) . . ? 
N4B C3B H3B' 105.6(19) . . ? 
C2B C3B H3B' 110(2) . . ? 
H3B C3B H3B' 114(3) . . ? 
C5B N4B C3B 121.5(3) . . ? 
C5B N4B H4B 125(2) . . ? 
C3B N4B H4B 113(2) . . ? 
O6B C5B N4B 123.1(3) . . ? 
O6B C5B N7B 123.5(4) . . ? 
N4B C5B N7B 113.4(3) . . ? 
C5B N7B C8B 128.8(3) . . ? 
C5B N7B H7B 116(3) . . ? 
C8B N7B H7B 115(3) . . ? 
C9B C8B C13B 119.9(4) . . ? 
C9B C8B N7B 124.0(4) . . ? 
C13B C8B N7B 116.1(4) . . ? 
C8B C9B C10B 120.3(4) . . ? 
C8B C9B H9B 113(3) . . ? 
C10B C9B H9B 127(3) . . ? 
C11B C10B C9B 118.5(4) . . ? 
C11B C10B H10B 121(3) . . ? 
C9B C10B H10B 121(3) . . ? 
C12B C11B C10B 122.2(4) . . ? 
C12B C11B N14B 119.4(4) . . ? 
C10B C11B N14B 118.2(4) . . ? 
C11B C12B C13B 119.4(4) . . ? 
C11B C12B H12B 112(3) . . ? 
C13B C12B H12B 128(2) . . ? 
C12B C13B C8B 119.7(4) . . ? 
C12B C13B H13B 120(2) . . ? 
C8B C13B H13B 120(3) . . ? 
O15B N14B O16B 123.4(4) . . ? 
O15B N14B C11B 119.5(4) . . ? 
O16B N14B C11B 117.1(4) . . ? 
N1 C2C C3C 112.4(3) . . ? 
N1 C2C H2C 119(2) . . ? 
C3C C2C H2C 100(2) . . ? 
N1 C2C H2C' 108(2) . . ? 
C3C C2C H2C' 116(2) . . ? 
H2C C2C H2C' 101(3) . . ? 
N4C C3C C2C 112.8(4) . . ? 
N4C C3C H3C 110.1(19) . . ? 
C2C C3C H3C 110.3(18) . . ? 
N4C C3C H3C' 109(2) . . ? 
C2C C3C H3C' 112(2) . . ? 
H3C C3C H3C' 103(3) . . ? 
C5C N4C C3C 124.1(4) . . ? 
C5C N4C H4C 117.0(19) . . ? 
C3C N4C H4C 118.8(19) . . ? 
O6C C5C N4C 122.8(4) . . ? 
O6C C5C N7C 122.7(4) . . ? 
N4C C5C N7C 114.3(3) . . ? 
C5C N7C C8C 128.9(4) . . ? 
C5C N7C H7C 105(4) . . ? 
C8C N7C H7C 121(4) . . ? 
C9C C8C N7C 124.9(4) . . ? 
C9C C8C C13C 117.4(4) . . ? 
N7C C8C C13C 117.7(3) . . ? 
C10C C9C C8C 121.2(4) . . ? 
C10C C9C H9C 119(3) . . ? 
C8C C9C H9C 115(3) . . ? 
C9C C10C C11C 120.1(4) . . ? 
C9C C10C H10C 130(3) . . ? 
C11C C10C H10C 109(3) . . ? 
C12C C11C C10C 120.8(4) . . ? 
C12C C11C N14C 119.4(4) . . ? 
C10C C11C N14C 119.8(4) . . ? 
C11C C12C C13C 119.2(4) . . ? 
C11C C12C H12C 121(2) . . ? 
C13C C12C H12C 120(2) . . ? 
C12C C13C C8C 121.2(4) . . ? 
C12C C13C H13C 116(2) . . ? 
C8C C13C H13C 123(2) . . ? 
O16C N14C O15C 124.2(4) . . ? 
O16C N14C C11C 118.2(4) . . ? 
O15C N14C C11C 117.6(4) . . ? 
 
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 
N4B H4B O6A  0.98(4) 2.23(4) 2.995(4) 133(3) 2_666 
N4C H4C O6B  0.93(3) 1.97(3) 2.886(4) 167(3) 2_565 
N7B H7B O6A  0.82(4) 2.07(4) 2.860(4) 162(4) 2_666 
N7C H7C O6B  0.79(4) 2.45(5) 3.182(4) 154(5) 2_565 
C2A H2A O16B  0.99(4) 2.57(4) 3.252(6) 126(3) 1_665 
C3B H3B O15C  1.05(3) 2.51(3) 3.312(5) 133(2) 1_565 
C12B H12B O15A  0.97(4) 2.55(4) 3.335(5) 138(3) 2_656 
C12C H12C O15B  0.99(4) 2.32(4) 3.294(6) 165(3) 2_455 
 
_diffrn_measured_fraction_theta_max    0.891 
_diffrn_reflns_theta_full              28.26 
_diffrn_measured_fraction_theta_full   0.891 
_refine_diff_density_max    0.271 
_refine_diff_density_min   -0.259 
_refine_diff_density_rms    0.055 
#===END

 
data_kkam68m 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C30 H37 N11 O10' 
_chemical_formula_weight          711.71 
 
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                    8.000(2) 
_cell_length_b                    14.482(4) 
_cell_length_c                    14.837(4) 
_cell_angle_alpha                 99.560(4) 
_cell_angle_beta                  91.818(4) 
_cell_angle_gamma                 93.915(5) 
_cell_volume                      1689.3(7) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     298(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ROD 
_exptl_crystal_colour             COLORLESS
_exptl_crystal_size_max           0.35 
_exptl_crystal_size_mid           0.11 
_exptl_crystal_size_min           0.04 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.399 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              748 
_exptl_absorpt_coefficient_mu     0.108 
_exptl_absorpt_correction_type    'MULTI-SCAN' 
_exptl_absorpt_correction_T_min   0.9633 
_exptl_absorpt_correction_T_max   0.9957 
_exptl_absorpt_process_details    'SADABS' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       298(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   'BRUKER SMART CCD AREA DETECTOR' 
_diffrn_measurement_method        'PHI-OMEGA SCAN'  
_diffrn_detector_area_resol_mean  0.3 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             10163 
_diffrn_reflns_av_R_equivalents   0.0175 
_diffrn_reflns_av_sigmaI/netI     0.0468 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -17 
_diffrn_reflns_limit_k_max        19 
_diffrn_reflns_limit_l_min        -16 
_diffrn_reflns_limit_l_max        19 
_diffrn_reflns_theta_min          1.39 
_diffrn_reflns_theta_max          28.22 
_reflns_number_total              7442 
_reflns_number_gt                 4503 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'BRUKER AXS SMART 3'  
_computing_cell_refinement        'BRUKER AXS SMART 3'  
_computing_data_reduction         'BRUKER AXS SAINT'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'BRUKER SHELXLTL'
_computing_publication_material   'MERCURY 1.4' 
 
_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)+(0.1111P)²+0.2146P] 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          7442 
_refine_ls_number_parameters      582 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0959 
_refine_ls_R_factor_gt            0.0569 
_refine_ls_wR_factor_ref          0.1995 
_refine_ls_wR_factor_gt           0.1530 
_refine_ls_goodness_of_fit_ref    0.983 
_refine_ls_restrained_S_all       0.983 
_refine_ls_shift/su_max           0.006 
_refine_ls_shift/su_mean          0.001 
 
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 0.3887(3) 0.41892(12) 0.18533(13) 0.0454(5) Uani 1 1 d . . . 
C2A C 0.2647(4) 0.37029(18) 0.23488(18) 0.0503(6) Uani 1 1 d . . . 
C3A C 0.2741(4) 0.40645(17) 0.33669(18) 0.0491(6) Uani 1 1 d . . . 
N4A N 0.2109(3) 0.49876(15) 0.35781(15) 0.0524(5) Uani 1 1 d . . . 
C5A C 0.1982(3) 0.53978(17) 0.44498(16) 0.0453(5) Uani 1 1 d . . . 
O6A O 0.2483(2) 0.50461(13) 0.51002(12) 0.0611(5) Uani 1 1 d . . . 
N7A N 0.1236(3) 0.62364(15) 0.45377(15) 0.0502(5) Uani 1 1 d . . . 
C8A C 0.0935(3) 0.68564(16) 0.53268(16) 0.0430(5) Uani 1 1 d . . . 
C9A C 0.1594(4) 0.6799(2) 0.61908(18) 0.0582(7) Uani 1 1 d . . . 
C10A C 0.1267(4) 0.7469(2) 0.6931(2) 0.0655(8) Uani 1 1 d . . . 
C11A C 0.0321(3) 0.81912(18) 0.68077(18) 0.0540(6) Uani 1 1 d . . . 
C12A C -0.0365(3) 0.82623(19) 0.59603(19) 0.0547(6) Uani 1 1 d . . . 
C13A C -0.0046(3) 0.75979(18) 0.52256(18) 0.0522(6) Uani 1 1 d . . . 
N14A N -0.0007(4) 0.8898(2) 0.7596(2) 0.0794(8) Uani 1 1 d . . . 
O15A O 0.0644(5) 0.8857(2) 0.83204(19) 0.1479(15) Uani 1 1 d . . . 
O16A O -0.0936(4) 0.94979(19) 0.74785(18) 0.1060(9) Uani 1 1 d . . . 
C2B C 0.3435(4) 0.40536(19) 0.08708(18) 0.0583(7) Uani 1 1 d . . . 
C3B C 0.2265(4) 0.47805(19) 0.0649(2) 0.0604(7) Uani 1 1 d . . . 
N4B N 0.3118(3) 0.57005(15) 0.09678(15) 0.0565(6) Uani 1 1 d . . . 
C5B C 0.2834(3) 0.64685(17) 0.06017(16) 0.0478(6) Uani 1 1 d . . . 
O6B O 0.1882(2) 0.64655(13) -0.00605(13) 0.0623(5) Uani 1 1 d . . . 
N7B N 0.3759(3) 0.72544(14) 0.10597(16) 0.0531(6) Uani 1 1 d . . . 
C8B C 0.3677(3) 0.81955(16) 0.09740(16) 0.0455(6) Uani 1 1 d . . . 
C9B C 0.2731(4) 0.8507(2) 0.02933(18) 0.0574(7) Uani 1 1 d . . . 
C10B C 0.2700(4) 0.94645(19) 0.0294(2) 0.0611(7) Uani 1 1 d . . . 
C11B C 0.3635(4) 1.00882(18) 0.09434(18) 0.0565(7) Uani 1 1 d . . . 
C12B C 0.4608(4) 0.9788(2) 0.1596(2) 0.0609(7) Uani 1 1 d . . . 
C13B C 0.4611(4) 0.88504(18) 0.16145(18) 0.0547(7) Uani 1 1 d . . . 
N14B N 0.3593(4) 1.10969(18) 0.0947(2) 0.0772(8) Uani 1 1 d . . . 
O15B O 0.4398(4) 1.16313(16) 0.1559(2) 0.1066(9) Uani 1 1 d . . . 
O16B O 0.2791(4) 1.13635(17) 0.0348(2) 0.1124(10) Uani 1 1 d . . . 
C2C C 0.5591(4) 0.39241(18) 0.20152(19) 0.0522(6) Uani 1 1 d . . . 
C3C C 0.6854(4) 0.4770(2) 0.22067(18) 0.0538(6) Uani 1 1 d . . . 
N4C N 0.6653(3) 0.53579(15) 0.30912(15) 0.0529(5) Uani 1 1 d . . . 
C5C C 0.5966(3) 0.61840(17) 0.31927(16) 0.0462(6) Uani 1 1 d . . . 
O6C O 0.5467(3) 0.65529(13) 0.25630(12) 0.0613(5) Uani 1 1 d . . . 
N7C N 0.5891(3) 0.65929(15) 0.41035(14) 0.0510(5) Uani 1 1 d . . . 
C8C C 0.5161(3) 0.74217(16) 0.44612(16) 0.0459(6) Uani 1 1 d . . . 
C9C C 0.4241(3) 0.79401(19) 0.39404(19) 0.0553(6) Uani 1 1 d . . . 
C10C C 0.3548(4) 0.87399(19) 0.43581(19) 0.0576(7) Uani 1 1 d . . . 
C11C C 0.3753(3) 0.90180(16) 0.52878(17) 0.0485(6) Uani 1 1 d . . . 
C12C C 0.4663(3) 0.85185(18) 0.58141(19) 0.0530(6) Uani 1 1 d . . . 
C13C C 0.5381(3) 0.77264(18) 0.53991(17) 0.0513(6) Uani 1 1 d . . . 
N14C N 0.2928(3) 0.98383(15) 0.57260(17) 0.0576(6) Uani 1 1 d . . . 
O15C O 0.2128(3) 1.02706(16) 0.52529(16) 0.0836(7) Uani 1 1 d . . . 
O16C O 0.3071(3) 1.00477(15) 0.65587(15) 0.0824(7) Uani 1 1 d . . . 
C17 C 0.0343(8) 0.1751(3) 0.7257(3) 0.152(2) Uani 1 1 d . . . 
H17A H -0.0726 0.1770 0.6950 0.229 Uiso 1 1 calc R . . 
H17B H 0.0407 0.1153 0.7450 0.229 Uiso 1 1 calc R . . 
H17C H 0.1221 0.1839 0.6846 0.229 Uiso 1 1 calc R . . 
N18 N 0.0530(3) 0.24740(17) 0.80300(15) 0.0591(6) Uani 1 1 d . . . 
C19 C 0.1271(5) 0.2275(3) 0.8863(2) 0.0997(12) Uani 1 1 d . . . 
H19A H 0.2328 0.2015 0.8742 0.150 Uiso 1 1 calc R . . 
H19B H 0.0537 0.1833 0.9105 0.150 Uiso 1 1 calc R . . 
H19C H 0.1442 0.2845 0.9300 0.150 Uiso 1 1 calc R . . 
C20 C 0.0134(4) 0.3328(2) 0.7957(2) 0.0654(7) Uani 1 1 d . . . 
H20 H 0.0334 0.3785 0.8476 0.078 Uiso 1 1 calc R . . 
O21 O -0.0461(3) 0.35839(17) 0.72880(15) 0.0881(7) Uani 1 1 d . . . 
H2A H 0.289(3) 0.3050(19) 0.2301(16) 0.046(6) Uiso 1 1 d . . . 
H2A' H 0.164(3) 0.3811(17) 0.2123(17) 0.047(7) Uiso 1 1 d . . . 
H3A H 0.389(3) 0.4069(17) 0.3630(17) 0.052(7) Uiso 1 1 d . . . 
H3A' H 0.217(3) 0.366(2) 0.3681(19) 0.063(8) Uiso 1 1 d . . . 
H4A H 0.190(4) 0.527(2) 0.315(2) 0.070(9) Uiso 1 1 d . . . 
H7A H 0.090(3) 0.6383(19) 0.402(2) 0.060(8) Uiso 1 1 d . . . 
H9A H 0.236(4) 0.629(2) 0.628(2) 0.076(9) Uiso 1 1 d . . . 
H10A H 0.178(4) 0.747(2) 0.755(2) 0.080(9) Uiso 1 1 d . . . 
H12A H -0.102(3) 0.8769(19) 0.5871(18) 0.056(7) Uiso 1 1 d . . . 
H13A H -0.065(3) 0.7584(19) 0.460(2) 0.066(8) Uiso 1 1 d . . . 
H2B H 0.276(4) 0.341(2) 0.066(2) 0.089(10) Uiso 1 1 d . . . 
H2B' H 0.451(4) 0.417(2) 0.055(2) 0.074(9) Uiso 1 1 d . . . 
H3B H 0.192(3) 0.469(2) -0.002(2) 0.069(8) Uiso 1 1 d . . . 
H3B' H 0.120(4) 0.475(2) 0.098(2) 0.079(10) Uiso 1 1 d . . . 
H4B H 0.382(3) 0.5784(17) 0.1470(18) 0.050(7) Uiso 1 1 d . . . 
H7B H 0.429(3) 0.7183(18) 0.1510(19) 0.048(7) Uiso 1 1 d . . . 
H9B H 0.201(4) 0.804(2) -0.016(2) 0.071(9) Uiso 1 1 d . . . 
H10B H 0.202(4) 0.966(2) -0.019(2) 0.085(10) Uiso 1 1 d . . . 
H12B H 0.515(4) 1.020(2) 0.199(2) 0.066(9) Uiso 1 1 d . . . 
H13B H 0.519(3) 0.8632(19) 0.2029(19) 0.058(8) Uiso 1 1 d . . . 
H2C H 0.597(4) 0.352(2) 0.148(2) 0.070(8) Uiso 1 1 d . . . 
H2C' H 0.550(3) 0.3558(19) 0.2514(19) 0.061(8) Uiso 1 1 d . . . 
H3C H 0.811(4) 0.461(2) 0.218(2) 0.074(9) Uiso 1 1 d . . . 
H3C' H 0.667(3) 0.5149(18) 0.1776(18) 0.050(7) Uiso 1 1 d . . . 
H4C H 0.699(3) 0.5161(19) 0.362(2) 0.057(8) Uiso 1 1 d . . . 
H7C H 0.641(3) 0.630(2) 0.4516(19) 0.061(8) Uiso 1 1 d . . . 
H9C H 0.400(4) 0.772(2) 0.326(2) 0.075(9) Uiso 1 1 d . . . 
H10C H 0.291(4) 0.913(2) 0.405(2) 0.074(9) Uiso 1 1 d . . . 
H12C H 0.484(3) 0.870(2) 0.646(2) 0.068(8) Uiso 1 1 d . . . 
H13C H 0.617(4) 0.734(2) 0.5757(19) 0.070(8) Uiso 1 1 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 
N1 C2A 1.464(3) . ? 
N1 C2C 1.464(3) . ? 
N1 C2B 1.468(3) . ? 
C2A C3A 1.512(4) . ? 
C2A H2A 0.97(3) . ? 
C2A H2A' 0.90(3) . ? 
C3A N4A 1.451(3) . ? 
C3A H3A 0.98(3) . ? 
C3A H3A' 0.91(3) . ? 
N4A C5A 1.341(3) . ? 
N4A H4A 0.84(3) . ? 
C5A O6A 1.232(3) . ? 
C5A N7A 1.378(3) . ? 
N7A C8A 1.390(3) . ? 
N7A H7A 0.87(3) . ? 
C8A C9A 1.388(3) . ? 
C8A C13A 1.397(3) . ? 
C9A C10A 1.383(4) . ? 
C9A H9A 1.01(3) . ? 
C10A C11A 1.365(4) . ? 
C10A H10A 0.99(3) . ? 
C11A C12A 1.378(4) . ? 
C11A N14A 1.464(4) . ? 
C12A C13A 1.372(4) . ? 
C12A H12A 0.96(3) . ? 
C13A H13A 1.03(3) . ? 
N14A O15A 1.192(4) . ? 
N14A O16A 1.212(4) . ? 
C2B C3B 1.524(4) . ? 
C2B H2B 1.04(3) . ? 
C2B H2B' 1.01(3) . ? 
C3B N4B 1.453(3) . ? 
C3B H3B 1.01(3) . ? 
C3B H3B' 1.00(3) . ? 
N4B C5B 1.346(3) . ? 
N4B H4B 0.91(3) . ? 
C5B O6B 1.223(3) . ? 
C5B N7B 1.379(3) . ? 
N7B C8B 1.395(3) . ? 
N7B H7B 0.80(3) . ? 
C8B C13B 1.385(4) . ? 
C8B C9B 1.394(3) . ? 
C9B C10B 1.389(4) . ? 
C9B H9B 1.01(3) . ? 
C10B C11B 1.370(4) . ? 
C10B H10B 0.98(3) . ? 
C11B C12B 1.368(4) . ? 
C11B N14B 1.463(4) . ? 
C12B C13B 1.363(4) . ? 
C12B H12B 0.84(3) . ? 
C13B H13B 0.87(3) . ? 
N14B O16B 1.209(4) . ? 
N14B O15B 1.224(4) . ? 
C2C C3C 1.517(4) . ? 
C2C H2C 0.97(3) . ? 
C2C H2C' 0.98(3) . ? 
C3C N4C 1.461(3) . ? 
C3C H3C 1.05(3) . ? 
C3C H3C' 0.92(3) . ? 
N4C C5C 1.338(3) . ? 
N4C H4C 0.92(3) . ? 
C5C O6C 1.220(3) . ? 
C5C N7C 1.387(3) . ? 
N7C C8C 1.403(3) . ? 
N7C H7C 0.90(3) . ? 
C8C C13C 1.390(3) . ? 
C8C C9C 1.391(3) . ? 
C9C C10C 1.380(4) . ? 
C9C H9C 1.01(3) . ? 
C10C C11C 1.373(4) . ? 
C10C H10C 0.95(3) . ? 
C11C C12C 1.373(3) . ? 
C11C N14C 1.465(3) . ? 
C12C C13C 1.379(4) . ? 
C12C H12C 0.95(3) . ? 
C13C H13C 1.05(3) . ? 
N14C O15C 1.211(3) . ? 
N14C O16C 1.222(3) . ? 
C17 N18 1.416(5) . ? 
C17 H17A 0.9600 . ? 
C17 H17B 0.9600 . ? 
C17 H17C 0.9600 . ? 
N18 C20 1.319(4) . ? 
N18 C19 1.434(4) . ? 
C19 H19A 0.9600 . ? 
C19 H19B 0.9600 . ? 
C19 H19C 0.9600 . ? 
C20 O21 1.210(3) . ? 
C20 H20 0.9300 . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
C2A N1 C2C 112.3(2) . . ? 
C2A N1 C2B 111.5(2) . . ? 
C2C N1 C2B 111.2(2) . . ? 
N1 C2A C3A 113.0(2) . . ? 
N1 C2A H2A 109.3(14) . . ? 
C3A C2A H2A 104.0(14) . . ? 
N1 C2A H2A' 106.1(16) . . ? 
C3A C2A H2A' 108.4(16) . . ? 
H2A C2A H2A' 116(2) . . ? 
N4A C3A C2A 111.6(2) . . ? 
N4A C3A H3A 110.8(15) . . ? 
C2A C3A H3A 111.6(15) . . ? 
N4A C3A H3A' 109.4(18) . . ? 
C2A C3A H3A' 111.8(18) . . ? 
H3A C3A H3A' 101(2) . . ? 
C5A N4A C3A 120.4(2) . . ? 
C5A N4A H4A 121(2) . . ? 
C3A N4A H4A 118(2) . . ? 
O6A C5A N4A 122.4(2) . . ? 
O6A C5A N7A 124.1(2) . . ? 
N4A C5A N7A 113.4(2) . . ? 
C5A N7A C8A 129.2(2) . . ? 
C5A N7A H7A 114.0(19) . . ? 
C8A N7A H7A 116.8(19) . . ? 
C9A C8A N7A 124.1(2) . . ? 
C9A C8A C13A 118.8(2) . . ? 
N7A C8A C13A 117.1(2) . . ? 
C10A C9A C8A 119.8(3) . . ? 
C10A C9A H9A 119.8(17) . . ? 
C8A C9A H9A 120.3(17) . . ? 
C11A C10A C9A 120.0(3) . . ? 
C11A C10A H10A 118.2(19) . . ? 
C9A C10A H10A 121.6(19) . . ? 
C10A C11A C12A 121.6(3) . . ? 
C10A C11A N14A 119.4(3) . . ? 
C12A C11A N14A 119.0(3) . . ? 
C13A C12A C11A 118.5(3) . . ? 
C13A C12A H12A 119.6(17) . . ? 
C11A C12A H12A 121.8(16) . . ? 
C12A C13A C8A 121.3(3) . . ? 
C12A C13A H13A 120.3(16) . . ? 
C8A C13A H13A 117.9(16) . . ? 
O15A N14A O16A 123.1(3) . . ? 
O15A N14A C11A 118.8(3) . . ? 
O16A N14A C11A 118.1(3) . . ? 
N1 C2B C3B 111.5(2) . . ? 
N1 C2B H2B 111.1(18) . . ? 
C3B C2B H2B 104.4(18) . . ? 
N1 C2B H2B' 106.6(18) . . ? 
C3B C2B H2B' 106.4(17) . . ? 
H2B C2B H2B' 117(3) . . ? 
N4B C3B C2B 107.2(2) . . ? 
N4B C3B H3B 112.0(16) . . ? 
C2B C3B H3B 112.5(17) . . ? 
N4B C3B H3B' 107.3(18) . . ? 
C2B C3B H3B' 112.2(18) . . ? 
H3B C3B H3B' 105(2) . . ? 
C5B N4B C3B 123.8(2) . . ? 
C5B N4B H4B 116.8(16) . . ? 
C3B N4B H4B 119.2(16) . . ? 
O6B C5B N4B 124.0(2) . . ? 
O6B C5B N7B 124.3(2) . . ? 
N4B C5B N7B 111.7(2) . . ? 
C5B N7B C8B 129.6(2) . . ? 
C5B N7B H7B 115.8(19) . . ? 
C8B N7B H7B 113.3(19) . . ? 
C13B C8B C9B 119.0(2) . . ? 
C13B C8B N7B 116.7(2) . . ? 
C9B C8B N7B 124.3(2) . . ? 
C10B C9B C8B 119.3(3) . . ? 
C10B C9B H9B 120.7(17) . . ? 
C8B C9B H9B 119.9(17) . . ? 
C11B C10B C9B 119.8(3) . . ? 
C11B C10B H10B 122.7(19) . . ? 
C9B C10B H10B 117.5(19) . . ? 
C12B C11B C10B 121.4(2) . . ? 
C12B C11B N14B 118.9(3) . . ? 
C10B C11B N14B 119.7(3) . . ? 
C13B C12B C11B 119.2(3) . . ? 
C13B C12B H12B 123(2) . . ? 
C11B C12B H12B 118(2) . . ? 
C12B C13B C8B 121.3(3) . . ? 
C12B C13B H13B 122.1(18) . . ? 
C8B C13B H13B 116.6(18) . . ? 
O16B N14B O15B 123.2(3) . . ? 
O16B N14B C11B 119.1(3) . . ? 
O15B N14B C11B 117.7(3) . . ? 
N1 C2C C3C 112.1(2) . . ? 
N1 C2C H2C 111.3(17) . . ? 
C3C C2C H2C 106.0(17) . . ? 
N1 C2C H2C' 104.7(16) . . ? 
C3C C2C H2C' 114.6(16) . . ? 
H2C C2C H2C' 108(2) . . ? 
N4C C3C C2C 112.9(2) . . ? 
N4C C3C H3C 107.2(16) . . ? 
C2C C3C H3C 114.4(16) . . ? 
N4C C3C H3C' 105.4(16) . . ? 
C2C C3C H3C' 108.5(16) . . ? 
H3C C3C H3C' 108(2) . . ? 
C5C N4C C3C 123.9(2) . . ? 
C5C N4C H4C 116.0(17) . . ? 
C3C N4C H4C 120.1(17) . . ? 
O6C C5C N4C 124.6(2) . . ? 
O6C C5C N7C 122.8(2) . . ? 
N4C C5C N7C 112.6(2) . . ? 
C5C N7C C8C 127.9(2) . . ? 
C5C N7C H7C 116.3(18) . . ? 
C8C N7C H7C 115.8(18) . . ? 
C13C C8C C9C 119.1(2) . . ? 
C13C C8C N7C 116.7(2) . . ? 
C9C C8C N7C 124.2(2) . . ? 
C10C C9C C8C 119.9(2) . . ? 
C10C C9C H9C 118.7(18) . . ? 
C8C C9C H9C 121.3(18) . . ? 
C11C C10C C9C 120.0(2) . . ? 
C11C C10C H10C 114.9(18) . . ? 
C9C C10C H10C 125.0(18) . . ? 
C10C C11C C12C 121.0(2) . . ? 
C10C C11C N14C 119.2(2) . . ? 
C12C C11C N14C 119.7(2) . . ? 
C11C C12C C13C 119.3(2) . . ? 
C11C C12C H12C 123.0(18) . . ? 
C13C C12C H12C 117.7(18) . . ? 
C12C C13C C8C 120.6(2) . . ? 
C12C C13C H13C 122.9(16) . . ? 
C8C C13C H13C 116.3(16) . . ? 
O15C N14C O16C 123.1(2) . . ? 
O15C N14C C11C 119.0(2) . . ? 
O16C N14C C11C 118.0(2) . . ? 
N18 C17 H17A 109.5 . . ? 
N18 C17 H17B 109.5 . . ? 
H17A C17 H17B 109.5 . . ? 
N18 C17 H17C 109.5 . . ? 
H17A C17 H17C 109.5 . . ? 
H17B C17 H17C 109.5 . . ? 
C20 N18 C17 119.9(3) . . ? 
C20 N18 C19 121.2(3) . . ? 
C17 N18 C19 118.8(3) . . ? 
N18 C19 H19A 109.5 . . ? 
N18 C19 H19B 109.5 . . ? 
H19A C19 H19B 109.5 . . ? 
N18 C19 H19C 109.5 . . ? 
H19A C19 H19C 109.5 . . ? 
H19B C19 H19C 109.5 . . ? 
O21 C20 N18 127.1(3) . . ? 
O21 C20 H20 116.4 . . ? 
N18 C20 H20 116.4 . . ? 
 
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 
N4A H4A O21  0.84(3) 2.25(3) 2.969(3) 145(3) 2_566 
N4C H4C O6A  0.92(3) 2.01(3) 2.912(3) 169(2) 2_666 
N7A H7A O21  0.87(3) 1.97(3) 2.818(3) 164(3) 2_566 
C2A H2A O15B  0.97(3) 2.56(3) 3.442(4) 150.9(18) 1_545 
C10B H10B O15A  0.98(3) 2.50(3) 3.270(4) 135(2) 1_554 
C12A H12A O15C  0.96(3) 2.52(3) 3.356(4) 146(2) 2_576 
C17 H17B O16A  0.96 2.57 3.423(6) 148.7 1_545 
 
_diffrn_measured_fraction_theta_max    0.892 
_diffrn_reflns_theta_full              28.22 
_diffrn_measured_fraction_theta_full   0.892 
_refine_diff_density_max    0.373 
_refine_diff_density_min   -0.341 
_refine_diff_density_rms    0.096 
#===END
 
data_adduct 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C25.50 H40.53 N5.75 O7.25 S0.50' 
_chemical_formula_weight          559.70 
 
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            'TRIGONAL' 
_symmetry_space_group_name_H-M    'R32' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-y, x-y, z' 
 '-x+y, -x, z' 
 'y, x, -z' 
 'x-y, -y, -z' 
 '-x, -x+y, -z' 
 'x+2/3, y+1/3, z+1/3' 
 '-y+2/3, x-y+1/3, z+1/3' 
 '-x+y+2/3, -x+1/3, z+1/3' 
 'y+2/3, x+1/3, -z+1/3' 
 'x-y+2/3, -y+1/3, -z+1/3' 
 '-x+2/3, -x+y+1/3, -z+1/3' 
 'x+1/3, y+2/3, z+2/3' 
 '-y+1/3, x-y+2/3, z+2/3' 
 '-x+y+1/3, -x+2/3, z+2/3' 
 'y+1/3, x+2/3, -z+2/3' 
 'x-y+1/3, -y+2/3, -z+2/3' 
 '-x+1/3, -x+y+2/3, -z+2/3' 
 
_cell_length_a                    17.230(10) 
_cell_length_b                    17.230(10) 
_cell_length_c                    39.99(5) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      10282(15) 
_cell_formula_units_Z             12 
_cell_measurement_temperature     100(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        PLATE 
_exptl_crystal_colour             COLORLESS 
_exptl_crystal_size_max           0.28 
_exptl_crystal_size_mid           0.08 
_exptl_crystal_size_min           0.03 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.085 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              3597 
_exptl_absorpt_coefficient_mu     0.109 
_exptl_absorpt_correction_type    'MULTI-SCAN' 
_exptl_absorpt_correction_T_min   0.9702 
_exptl_absorpt_correction_T_max   0.9967 
_exptl_absorpt_process_details    'SADABS' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       100(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   'BRUKER SMART CCD AREA DETECTOR' 
_diffrn_measurement_method        'PHI-OMEGA SCAN'  
_diffrn_detector_area_resol_mean  0.3  
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             29554 
_diffrn_reflns_av_R_equivalents   0.0473 
_diffrn_reflns_av_sigmaI/netI     0.0463 
_diffrn_reflns_limit_h_min        -22 
_diffrn_reflns_limit_h_max        22 
_diffrn_reflns_limit_k_min        -22 
_diffrn_reflns_limit_k_max        22 
_diffrn_reflns_limit_l_min        -51 
_diffrn_reflns_limit_l_max        52 
_diffrn_reflns_theta_min          1.46 
_diffrn_reflns_theta_max          28.59 
_reflns_number_total              5532 
_reflns_number_gt                 3885 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'BRUKER AXS SMART 3'  
_computing_cell_refinement        'BRUKER AXS SMART 3'  
_computing_data_reduction         'BRUKER AXS SAINT'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'BRUKER SHELXLTL'
_computing_publication_material   'MERCURY 1.4' 
 
_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)+(0.1257P)²+0.0000P] 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), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.11(12) 
_refine_ls_number_reflns          5532 
_refine_ls_number_parameters      263 
_refine_ls_number_restraints      3 
_refine_ls_R_factor_all           0.0878 
_refine_ls_R_factor_gt            0.0624 
_refine_ls_wR_factor_ref          0.1770 
_refine_ls_wR_factor_gt           0.1633 
_refine_ls_goodness_of_fit_ref    0.923 
_refine_ls_restrained_S_all       0.926 
_refine_ls_shift/su_max           0.008 
_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 
S1 S 1.0000 1.0000 0.07400(2) 0.0314(2) Uani 1 3 d S . . 
O1S O 0.90802(11) 0.93947(11) 0.06218(4) 0.0367(4) Uani 1 1 d . . . 
O2S O 1.0000 1.0000 0.11109(6) 0.0438(7) Uani 1 3 d S . . 
O3W O 0.85799(16) 0.85799(16) 0.0000 0.0439(6) Uani 1 2 d S . . 
H3W H 0.870(3) 0.885(2) 0.0151(8) 0.071(12) Uiso 1 1 d . . . 
N1 N 1.0000 1.0000 0.19726(9) 0.0527(9) Uani 1 3 d S . . 
C2 C 0.9066(2) 0.9545(2) 0.20805(6) 0.0581(7) Uani 1 1 d . . . 
H2A H 0.9027 0.9753 0.2307 0.055(8) Uiso 1 1 calc R . . 
H2B H 0.8835 0.8892 0.2091 0.044(7) Uiso 1 1 calc R . . 
C3 C 0.8489(2) 0.9734(2) 0.18385(7) 0.0554(7) Uani 1 1 d . . . 
H3A H 0.7883 0.9496 0.1935 0.082(11) Uiso 1 1 calc R . . 
H3B H 0.8757 1.0389 0.1811 0.054(8) Uiso 1 1 calc R . . 
N4 N 0.84179(17) 0.93300(17) 0.15158(5) 0.0514(6) Uani 1 1 d . . . 
H4 H 0.8867 0.9593 0.1374 0.056(9) Uiso 1 1 calc R . . 
C5 C 0.7684(2) 0.8563(2) 0.14250(6) 0.0513(7) Uani 1 1 d . . . 
O6 O 0.70231(16) 0.81550(15) 0.16050(5) 0.0675(6) Uani 1 1 d . . . 
N7 N 0.77248(16) 0.82803(16) 0.11066(5) 0.0533(6) Uani 1 1 d . . . 
H7 H 0.8165 0.8667 0.0979 0.048(8) Uiso 1 1 calc R . . 
C8 C 0.7144(2) 0.7447(2) 0.09641(7) 0.0544(7) Uani 1 1 d . . . 
C9 C 0.6478(2) 0.6716(2) 0.11388(8) 0.0705(10) Uani 1 1 d . . . 
H9 H 0.6374 0.6783 0.1367 0.065(9) Uiso 1 1 calc R . . 
C10 C 0.5972(2) 0.5903(2) 0.09862(9) 0.0740(10) Uani 1 1 d . . . 
H10 H 0.5532 0.5404 0.1109 0.049(8) Uiso 1 1 calc R . . 
C11 C 0.6107(2) 0.5818(2) 0.06527(9) 0.0683(10) Uani 1 1 d . . . 
C12 C 0.6768(2) 0.6529(2) 0.04725(8) 0.0610(8) Uani 1 1 d . . . 
H12 H 0.6864 0.6457 0.0243 0.056(8) Uiso 1 1 calc R . . 
C13 C 0.7279(2) 0.73311(19) 0.06270(7) 0.0532(7) Uani 1 1 d . . . 
H13 H 0.7733 0.7819 0.0504 0.043(7) Uiso 1 1 calc R . . 
N14 N 0.5564(2) 0.4953(2) 0.04876(9) 0.0899(11) Uani 1 1 d . . . 
O15 O 0.4968(2) 0.4339(2) 0.06481(8) 0.1093(12) Uani 1 1 d . . . 
O16 O 0.5711(3) 0.4875(2) 0.02053(9) 0.1308(16) Uani 1 1 d . . . 
N17 N 1.0000 0.71456(17) 0.0000 0.0590(9) Uani 1 2 d S . . 
C18 C 0.9754(3) 0.7550(2) 0.02892(9) 0.0623(8) Uani 1 1 d . . . 
H18A H 1.0300 0.8099 0.0364 0.075 Uiso 1 1 calc R . . 
H18B H 0.9323 0.7729 0.0208 0.075 Uiso 1 1 calc R . . 
C19 C 0.9347(3) 0.6934(2) 0.05869(10) 0.0758(10) Uani 1 1 d . . . 
H19A H 0.9711 0.6654 0.0644 0.067(10) Uiso 1 1 calc R . . 
H19B H 0.8734 0.6451 0.0531 0.047(8) Uiso 1 1 calc R . . 
C20 C 0.9314(3) 0.7468(2) 0.08865(9) 0.0759(11) Uani 1 1 d . . . 
H20A H 0.9932 0.7893 0.0961 0.15(2) Uiso 1 1 calc R . . 
H20B H 0.9030 0.7820 0.0818 0.068(9) Uiso 1 1 calc R . . 
C21 C 0.8793(4) 0.6862(3) 0.11743(11) 0.1162(19) Uani 1 1 d . . . 
H21A H 0.8218 0.6376 0.1092 0.174 Uiso 1 1 calc R . . 
H21B H 0.8685 0.7209 0.1343 0.174 Uiso 1 1 calc R . . 
H21C H 0.9138 0.6609 0.1274 0.174 Uiso 1 1 calc R . . 
C22 C 0.9237(2) 0.6232(2) -0.00974(10) 0.0701(10) Uani 1 1 d . . . 
H13A H 0.9446 0.5995 -0.0281 0.054(8) Uiso 1 1 calc R . . 
H13B H 0.9096 0.5825 0.0096 0.068(10) Uiso 1 1 calc R . . 
C23 C 0.8382(3) 0.6196(3) -0.02089(19) 0.1085(18) Uani 1 1 d . B . 
H23A H 0.8459 0.6449 -0.0437 0.30(6) Uiso 1 1 calc R . . 
H23B H 0.8235 0.6555 -0.0056 0.16(2) Uiso 1 1 calc R . . 
C24 C 0.7602(4) 0.5192(5) -0.0208(3) 0.199(4) Uani 1 1 d D . . 
H24A H 0.7778 0.4828 -0.0346 0.239 Uiso 1 1 calc R A 1 
H24B H 0.7059 0.5154 -0.0308 0.239 Uiso 1 1 calc R A 1 
C25A C 0.7381(19) 0.4798(16) 0.0162(4) 0.166(8) Uiso 0.34 1 d PD B 1 
H25A H 0.6738 0.4368 0.0181 0.249 Uiso 0.34 1 calc PR B 1 
H25B H 0.7548 0.5287 0.0322 0.249 Uiso 0.34 1 calc PR B 1 
H25C H 0.7721 0.4494 0.0211 0.249 Uiso 0.34 1 calc PR B 1 
C25B C 0.7836(14) 0.4794(13) -0.0519(4) 0.159(6) Uiso 0.43 1 d PD B 2 
C25C C 0.770(2) 0.499(2) -0.0846(8) 0.151(10) Uiso 0.23 1 d P B 2 
 
 
_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 
S1 O1S 1.4730(18) 3_675 ? 
S1 O1S 1.4730(18) 2_765 ? 
S1 O1S 1.4730(18) . ? 
S1 O1S 1.4730(18) 1 ? 
S1 O2S 1.483(3) 1 ? 
S1 O2S 1.483(3) . ? 
O3W H3W 0.72(3) . ? 
N1 C2 1.458(3) 3_675 ? 
N1 C2 1.458(3) 2_765 ? 
N1 C2 1.458(3) . ? 
C2 C3 1.534(4) . ? 
C2 H2A 0.9900 . ? 
C2 H2B 0.9900 . ? 
C3 N4 1.442(4) . ? 
C3 H3A 0.9900 . ? 
C3 H3B 0.9900 . ? 
N4 C5 1.344(4) . ? 
N4 H4 0.8800 . ? 
C5 O6 1.229(4) . ? 
C5 N7 1.378(4) . ? 
N7 C8 1.397(4) . ? 
N7 H7 0.8800 . ? 
C8 C9 1.395(4) . ? 
C8 C13 1.399(4) . ? 
C9 C10 1.368(5) . ? 
C9 H9 0.9500 . ? 
C10 C11 1.375(5) . ? 
C10 H10 0.9500 . ? 
C11 C12 1.387(4) . ? 
C11 N14 1.463(5) . ? 
C12 C13 1.360(4) . ? 
C12 H12 0.9500 . ? 
C13 H13 0.9500 . ? 
N14 O16 1.179(4) . ? 
N14 O15 1.224(4) . ? 
N17 C22 1.513(4) . ? 
N17 C22 1.513(4) 6_765 ? 
N17 C18 1.516(4) . ? 
N17 C18 1.516(4) 6_765 ? 
C18 C19 1.513(5) . ? 
C18 H18A 0.9900 . ? 
C18 H18B 0.9900 . ? 
C19 C20 1.529(6) . ? 
C19 H19A 0.9900 . ? 
C19 H19B 0.9900 . ? 
C20 C21 1.511(6) . ? 
C20 H20A 0.9900 . ? 
C20 H20B 0.9900 . ? 
C21 H21A 0.9800 . ? 
C21 H21B 0.9800 . ? 
C21 H21C 0.9800 . ? 
C22 C23 1.510(5) . ? 
C22 H13A 0.9900 . ? 
C22 H13B 0.9900 . ? 
C23 C24 1.572(8) . ? 
C23 H23A 0.9900 . ? 
C23 H23B 0.9900 . ? 
C24 C25B 1.569(8) . ? 
C24 C25A 1.592(8) . ? 
C24 H24A 0.9900 . ? 
C24 H24B 0.9900 . ? 
C25A H25A 0.9800 . ? 
C25A H25B 0.9800 . ? 
C25A H25C 0.9800 . ? 
C25B C25C 1.40(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 
O1S S1 O1S 110.23(7) 3_675 2_765 ? 
O1S S1 O1S 110.23(7) 3_675 . ? 
O1S S1 O1S 110.22(7) 2_765 . ? 
O1S S1 O1S 110.23(7) 3_675 1 ? 
O1S S1 O1S 110.22(7) 2_765 1 ? 
O1S S1 O1S 0.0(2) . 1 ? 
O1S S1 O2S 108.71(7) 3_675 1 ? 
O1S S1 O2S 108.71(7) 2_765 1 ? 
O1S S1 O2S 108.71(7) . 1 ? 
O1S S1 O2S 108.71(7) 1 1 ? 
O1S S1 O2S 108.71(7) 3_675 . ? 
O1S S1 O2S 108.71(7) 2_765 . ? 
O1S S1 O2S 108.71(7) . . ? 
O1S S1 O2S 108.71(7) 1 . ? 
C2 N1 C2 111.63(15) 3_675 2_765 ? 
C2 N1 C2 111.63(15) 3_675 . ? 
C2 N1 C2 111.63(15) 2_765 . ? 
N1 C2 C3 110.9(2) . . ? 
N1 C2 H2A 109.5 . . ? 
C3 C2 H2A 109.5 . . ? 
N1 C2 H2B 109.5 . . ? 
C3 C2 H2B 109.5 . . ? 
H2A C2 H2B 108.0 . . ? 
N4 C3 C2 111.8(3) . . ? 
N4 C3 H3A 109.3 . . ? 
C2 C3 H3A 109.3 . . ? 
N4 C3 H3B 109.3 . . ? 
C2 C3 H3B 109.3 . . ? 
H3A C3 H3B 107.9 . . ? 
C5 N4 C3 121.9(2) . . ? 
C5 N4 H4 119.1 . . ? 
C3 N4 H4 119.1 . . ? 
O6 C5 N4 123.5(3) . . ? 
O6 C5 N7 122.4(3) . . ? 
N4 C5 N7 114.1(2) . . ? 
C5 N7 C8 127.1(2) . . ? 
C5 N7 H7 116.4 . . ? 
C8 N7 H7 116.4 . . ? 
C9 C8 N7 124.6(3) . . ? 
C9 C8 C13 118.3(3) . . ? 
N7 C8 C13 117.0(2) . . ? 
C10 C9 C8 121.1(3) . . ? 
C10 C9 H9 119.4 . . ? 
C8 C9 H9 119.4 . . ? 
C9 C10 C11 119.1(3) . . ? 
C9 C10 H10 120.5 . . ? 
C11 C10 H10 120.5 . . ? 
C10 C11 C12 121.2(3) . . ? 
C10 C11 N14 119.4(3) . . ? 
C12 C11 N14 119.4(3) . . ? 
C13 C12 C11 119.3(3) . . ? 
C13 C12 H12 120.3 . . ? 
C11 C12 H12 120.3 . . ? 
C12 C13 C8 120.9(3) . . ? 
C12 C13 H13 119.6 . . ? 
C8 C13 H13 119.6 . . ? 
O16 N14 O15 122.6(4) . . ? 
O16 N14 C11 118.9(3) . . ? 
O15 N14 C11 118.4(4) . . ? 
C22 N17 C22 105.4(3) . 6_765 ? 
C22 N17 C18 112.2(2) . . ? 
C22 N17 C18 110.4(2) 6_765 . ? 
C22 N17 C18 110.4(2) . 6_765 ? 
C22 N17 C18 112.2(2) 6_765 6_765 ? 
C18 N17 C18 106.4(3) . 6_765 ? 
C19 C18 N17 114.6(2) . . ? 
C19 C18 H18A 108.6 . . ? 
N17 C18 H18A 108.6 . . ? 
C19 C18 H18B 108.6 . . ? 
N17 C18 H18B 108.6 . . ? 
H18A C18 H18B 107.6 . . ? 
C18 C19 C20 109.8(3) . . ? 
C18 C19 H19A 109.7 . . ? 
C20 C19 H19A 109.7 . . ? 
C18 C19 H19B 109.7 . . ? 
C20 C19 H19B 109.7 . . ? 
H19A C19 H19B 108.2 . . ? 
C21 C20 C19 111.7(3) . . ? 
C21 C20 H20A 109.3 . . ? 
C19 C20 H20A 109.3 . . ? 
C21 C20 H20B 109.3 . . ? 
C19 C20 H20B 109.3 . . ? 
H20A C20 H20B 107.9 . . ? 
C20 C21 H21A 109.5 . . ? 
C20 C21 H21B 109.5 . . ? 
H21A C21 H21B 109.5 . . ? 
C20 C21 H21C 109.5 . . ? 
H21A C21 H21C 109.5 . . ? 
H21B C21 H21C 109.5 . . ? 
C23 C22 N17 116.2(3) . . ? 
C23 C22 H13A 108.2 . . ? 
N17 C22 H13A 108.2 . . ? 
C23 C22 H13B 108.2 . . ? 
N17 C22 H13B 108.2 . . ? 
H13A C22 H13B 107.4 . . ? 
C22 C23 C24 108.9(4) . . ? 
C22 C23 H23A 109.9 . . ? 
C24 C23 H23A 109.9 . . ? 
C22 C23 H23B 109.9 . . ? 
C24 C23 H23B 109.9 . . ? 
H23A C23 H23B 108.3 . . ? 
C25B C24 C23 102.3(10) . . ? 
C25B C24 C25A 127.6(14) . . ? 
C23 C24 C25A 111.3(10) . . ? 
C25B C24 H24A 18.8 . . ? 
C23 C24 H24A 109.4 . . ? 
C25A C24 H24A 109.4 . . ? 
C25B C24 H24B 95.1 . . ? 
C23 C24 H24B 109.4 . . ? 
C25A C24 H24B 109.4 . . ? 
H24A C24 H24B 108.0 . . ? 
C24 C25A H25A 109.5 . . ? 
C24 C25A H25B 109.5 . . ? 
C24 C25A H25C 109.5 . . ? 
C25C C25B C24 121(2) . . ? 
 
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 
O3W H3W O1S  0.72(3) 2.06(3) 2.773(3) 168(4) 1 
N4 H4 O2S  0.88 2.01 2.870(3) 165.3 1 
N7 H7 O1S  0.88 2.03 2.901(3) 170.0 1 
C10 H10 O6  0.95 2.51 3.161(5) 126.1 11_565 
C13 H13 O1S  0.95 2.58 3.353(4) 138.3 1 
C13 H13 O3W  0.95 2.45 3.335(4) 154.9 1 
C19 H19A O15  0.99 2.55 3.307(4) 132.9 3_665 
 
_diffrn_measured_fraction_theta_max    0.960 
_diffrn_reflns_theta_full              28.59 
_diffrn_measured_fraction_theta_full   0.960 
_refine_diff_density_max    0.512 
_refine_diff_density_min   -0.189 
_refine_diff_density_rms    0.052 
#===END
