  
data_07257 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety  'C25 H19 N3 O4 S2, 3(C2 H6 O S)'
_chemical_formula_sum     'C31 H37 N3 O7 S5' 
_chemical_formula_weight          723.94 
  
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            Triclinic 
_symmetry_space_group_name_H-M    'P -1' 
_symmetry_space_group_name_Hall   '-P 1' 
   
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
  
_cell_length_a                    10.6274(5) 
_cell_length_b                    10.8445(7) 
_cell_length_c                    14.7918(11) 
_cell_angle_alpha                 86.690(3) 
_cell_angle_beta                  87.617(3) 
_cell_angle_gamma                 81.397(3) 
_cell_volume                      1681.81(18) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     14842
_cell_measurement_theta_min       2.04
_cell_measurement_theta_max       27.48 
  
_exptl_crystal_description        plate
_exptl_crystal_colour             colourless 
_exptl_crystal_size_max           0.53 
_exptl_crystal_size_mid           0.11 
_exptl_crystal_size_min           0.03 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.430 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              760 
_exptl_absorpt_coefficient_mu     0.396 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.8193 
_exptl_absorpt_correction_T_max   0.9902 
_exptl_absorpt_process_details    'DENZO-SMN (Otwinowski & Minor, 1997)' 
  
_exptl_special_details 
; 
 ? 
; 
  
_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             15131
_diffrn_reflns_av_R_equivalents   0.041 
_diffrn_reflns_av_sigmaI/netI     0.0644 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -14 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        -16 
_diffrn_reflns_limit_l_max        19 
_diffrn_reflns_theta_min          2.29 
_diffrn_reflns_theta_max          27.70 
_reflns_number_total              7731 
_reflns_number_gt                 5567 
_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)+(0.0430P)²+1.1824P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          7731 
_refine_ls_number_parameters      421 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0787 
_refine_ls_R_factor_gt            0.0480 
_refine_ls_wR_factor_ref          0.1203 
_refine_ls_wR_factor_gt           0.1068 
_refine_ls_goodness_of_fit_ref    1.037 
_refine_ls_restrained_S_all       1.037 
_refine_ls_shift/su_max           0.001 
_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 
C1 C 0.3634(2) 0.1447(2) 0.56062(17) 0.0231(5) Uani 1 1 d . . . 
H1A H 0.3835 0.1315 0.4984 0.028 Uiso 1 1 calc R . . 
C2 C 0.2378(2) 0.1570(3) 0.59216(19) 0.0286(6) Uani 1 1 d . . . 
H2A H 0.1721 0.1544 0.5510 0.034 Uiso 1 1 calc R . . 
C3 C 0.2073(2) 0.1728(3) 0.68260(19) 0.0304(6) Uani 1 1 d . . . 
H3A H 0.1208 0.1817 0.7034 0.036 Uiso 1 1 calc R . . 
C4 C 0.3033(2) 0.1759(2) 0.74372(18) 0.0285(6) Uani 1 1 d . . . 
H4A H 0.2828 0.1845 0.8064 0.034 Uiso 1 1 calc R . . 
C5 C 0.4285(2) 0.1661(2) 0.71194(17) 0.0236(5) Uani 1 1 d . . . 
H5A H 0.4939 0.1691 0.7533 0.028 Uiso 1 1 calc R . . 
C6 C 0.4605(2) 0.1519(2) 0.62004(16) 0.0200(5) Uani 1 1 d . . . 
C7 C 0.5947(2) 0.1452(2) 0.58716(16) 0.0183(5) Uani 1 1 d . . . 
N8 N 0.61381(17) 0.17821(19) 0.49717(13) 0.0195(4) Uani 1 1 d . . . 
H8A H 0.5478 0.2155 0.4670 0.023 Uiso 1 1 calc R . . 
C9 C 0.7292(2) 0.1568(2) 0.45130(17) 0.0196(5) Uani 1 1 d . . . 
C10 C 0.8405(2) 0.1217(2) 0.49358(17) 0.0223(5) Uani 1 1 d . . . 
H10A H 0.9162 0.1001 0.4580 0.027 Uiso 1 1 calc R . . 
S11 S 0.84901(6) 0.11525(6) 0.60888(4) 0.02628(16) Uani 1 1 d . . . 
O12 O 0.92960(18) 0.0031(2) 0.63947(14) 0.0434(5) Uani 1 1 d . . . 
O13 O 0.88610(17) 0.2292(2) 0.63766(14) 0.0403(5) Uani 1 1 d . . . 
C14 C 0.6945(2) 0.1063(2) 0.64177(17) 0.0242(5) Uani 1 1 d . . . 
H14A H 0.6775 0.0726 0.7009 0.029 Uiso 1 1 calc R . . 
C15 C 0.7228(2) 0.1667(2) 0.35103(17) 0.0189(5) Uani 1 1 d . . . 
N16 N 0.60742(17) 0.15865(18) 0.31934(14) 0.0183(4) Uani 1 1 d . . . 
C17 C 0.5966(2) 0.1627(2) 0.22970(16) 0.0186(5) Uani 1 1 d . . . 
C18 C 0.6963(2) 0.1768(2) 0.16827(17) 0.0219(5) Uani 1 1 d . . . 
H18A H 0.6845 0.1789 0.1049 0.026 Uiso 1 1 calc R . . 
C19 C 0.8139(2) 0.1878(2) 0.20202(17) 0.0228(5) Uani 1 1 d . . . 
H19A H 0.8839 0.1984 0.1618 0.027 Uiso 1 1 calc R . . 
C20 C 0.8278(2) 0.1830(2) 0.29450(17) 0.0206(5) Uani 1 1 d . . . 
H20A H 0.9073 0.1907 0.3191 0.025 Uiso 1 1 calc R . . 
C21 C 0.4680(2) 0.1504(2) 0.19809(16) 0.0195(5) Uani 1 1 d . . . 
N22 N 0.36591(17) 0.20915(18) 0.24653(14) 0.0196(4) Uani 1 1 d . . . 
H22A H 0.3795 0.2405 0.2982 0.024 Uiso 1 1 calc R . . 
C23 C 0.2427(2) 0.2211(2) 0.21753(17) 0.0199(5) Uani 1 1 d . . . 
C24 C 0.2113(2) 0.1613(2) 0.14583(17) 0.0220(5) Uani 1 1 d . . . 
H24A H 0.1263 0.1796 0.1260 0.026 Uiso 1 1 calc R . . 
S25 S 0.31513(5) 0.05504(6) 0.08909(4) 0.02314(15) Uani 1 1 d . . . 
O26 O 0.30533(16) 0.0793(2) -0.00785(12) 0.0350(5) Uani 1 1 d . . . 
O27 O 0.29750(17) -0.07030(17) 0.11947(15) 0.0372(5) Uani 1 1 d . . . 
C28 C 0.4577(2) 0.0848(2) 0.12447(17) 0.0220(5) Uani 1 1 d . . . 
H28A H 0.5331 0.0540 0.0911 0.026 Uiso 1 1 calc R . . 
C29 C 0.1439(2) 0.3055(2) 0.26719(17) 0.0210(5) Uani 1 1 d . . . 
C30 C 0.1384(2) 0.3019(3) 0.36149(17) 0.0260(6) Uani 1 1 d . . . 
H30A H 0.1994 0.2462 0.3948 0.031 Uiso 1 1 calc R . . 
C31 C 0.0437(2) 0.3800(3) 0.4070(2) 0.0335(7) Uani 1 1 d . . . 
H31A H 0.0394 0.3767 0.4713 0.040 Uiso 1 1 calc R . . 
C32 C -0.0441(2) 0.4624(3) 0.3586(2) 0.0337(7) Uani 1 1 d . . . 
H32A H -0.1073 0.5172 0.3897 0.040 Uiso 1 1 calc R . . 
C33 C -0.0400(2) 0.4651(3) 0.2650(2) 0.0311(6) Uani 1 1 d . . . 
H33A H -0.1013 0.5209 0.2320 0.037 Uiso 1 1 calc R . . 
C34 C 0.0535(2) 0.3867(2) 0.21885(18) 0.0250(5) Uani 1 1 d . . . 
H34A H 0.0558 0.3886 0.1545 0.030 Uiso 1 1 calc R . . 
S40 S 0.43138(6) 0.48723(6) 0.39624(5) 0.02637(15) Uani 1 1 d . . . 
C41 C 0.5906(3) 0.4895(3) 0.3542(2) 0.0343(6) Uani 1 1 d . . . 
H41A H 0.6502 0.4479 0.3991 0.051 Uiso 1 1 calc R . . 
H41B H 0.6053 0.5762 0.3426 0.051 Uiso 1 1 calc R . . 
H41C H 0.6040 0.4457 0.2977 0.051 Uiso 1 1 calc R . . 
C42 C 0.3490(3) 0.5538(3) 0.2989(2) 0.0349(7) Uani 1 1 d . . . 
H42A H 0.3814 0.5069 0.2460 0.052 Uiso 1 1 calc R . . 
H42B H 0.3624 0.6410 0.2886 0.052 Uiso 1 1 calc R . . 
H42C H 0.2578 0.5500 0.3083 0.052 Uiso 1 1 calc R . . 
O43 O 0.41275(16) 0.35206(16) 0.40236(12) 0.0261(4) Uani 1 1 d . . . 
S50 S 0.62053(7) 0.56064(7) 0.11309(5) 0.03481(18) Uani 1 1 d . . . 
C51 C 0.7270(3) 0.5341(3) 0.0175(2) 0.0506(9) Uani 1 1 d . . . 
H51A H 0.7887 0.4590 0.0300 0.076 Uiso 1 1 calc R . . 
H51B H 0.7722 0.6061 0.0056 0.076 Uiso 1 1 calc R . . 
H51C H 0.6786 0.5227 -0.0356 0.076 Uiso 1 1 calc R . . 
C52 C 0.5177(3) 0.6889(3) 0.0638(2) 0.0425(7) Uani 1 1 d . . . 
H52A H 0.4856 0.6647 0.0073 0.064 Uiso 1 1 calc R . . 
H52B H 0.5647 0.7594 0.0510 0.064 Uiso 1 1 calc R . . 
H52C H 0.4459 0.7134 0.1060 0.064 Uiso 1 1 calc R . . 
O53 O 0.5457(2) 0.45375(18) 0.12316(15) 0.0427(5) Uani 1 1 d . . . 
S60 S 0.01363(6) 0.25194(7) -0.08633(5) 0.02782(16) Uani 1 1 d . . . 
C61 C 0.0219(3) 0.0906(3) -0.1061(2) 0.0327(6) Uani 1 1 d . . . 
H61A H 0.0995 0.0441 -0.0803 0.049 Uiso 1 1 calc R . . 
H61B H 0.0233 0.0797 -0.1714 0.049 Uiso 1 1 calc R . . 
H61C H -0.0527 0.0591 -0.0774 0.049 Uiso 1 1 calc R . . 
C62 C -0.1305(3) 0.3045(3) -0.14320(19) 0.0317(6) Uani 1 1 d . . . 
H62A H -0.1987 0.2619 -0.1155 0.048 Uiso 1 1 calc R . . 
H62B H -0.1188 0.2856 -0.2073 0.048 Uiso 1 1 calc R . . 
H62C H -0.1534 0.3948 -0.1382 0.048 Uiso 1 1 calc R . . 
O63 O -0.01688(19) 0.2657(2) 0.01283(13) 0.0423(5) Uani 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 
C1 C2 1.385(3) . ? 
C1 C6 1.397(3) . ? 
C1 H1A 0.9500 . ? 
C2 C3 1.378(4) . ? 
C2 H2A 0.9500 . ? 
C3 C4 1.396(4) . ? 
C3 H3A 0.9500 . ? 
C4 C5 1.384(3) . ? 
C4 H4A 0.9500 . ? 
C5 C6 1.399(3) . ? 
C5 H5A 0.9500 . ? 
C6 C7 1.480(3) . ? 
C7 C14 1.362(3) . ? 
C7 N8 1.373(3) . ? 
N8 C9 1.371(3) . ? 
N8 H8A 0.8800 . ? 
C9 C10 1.355(3) . ? 
C9 C15 1.485(3) . ? 
C10 S11 1.709(3) . ? 
C10 H10A 0.9500 . ? 
S11 O12 1.440(2) . ? 
S11 O13 1.443(2) . ? 
S11 C14 1.708(3) . ? 
C14 H14A 0.9500 . ? 
C15 N16 1.348(3) . ? 
C15 C20 1.393(3) . ? 
N16 C17 1.333(3) . ? 
C17 C18 1.388(3) . ? 
C17 C21 1.490(3) . ? 
C18 C19 1.388(3) . ? 
C18 H18A 0.9500 . ? 
C19 C20 1.379(3) . ? 
C19 H19A 0.9500 . ? 
C20 H20A 0.9500 . ? 
C21 C28 1.351(3) . ? 
C21 N22 1.370(3) . ? 
N22 C23 1.380(3) . ? 
N22 H22A 0.8800 . ? 
C23 C24 1.353(3) . ? 
C23 C29 1.485(3) . ? 
C24 S25 1.704(2) . ? 
C24 H24A 0.9500 . ? 
S25 O27 1.443(2) . ? 
S25 O26 1.4481(19) . ? 
S25 C28 1.705(2) . ? 
C28 H28A 0.9500 . ? 
C29 C30 1.392(3) . ? 
C29 C34 1.393(3) . ? 
C30 C31 1.392(4) . ? 
C30 H30A 0.9500 . ? 
C31 C32 1.384(4) . ? 
C31 H31A 0.9500 . ? 
C32 C33 1.382(4) . ? 
C32 H32A 0.9500 . ? 
C33 C34 1.391(3) . ? 
C33 H33A 0.9500 . ? 
C34 H34A 0.9500 . ? 
S40 O43 1.5054(18) . ? 
S40 C42 1.777(3) . ? 
S40 C41 1.782(3) . ? 
C41 H41A 0.9800 . ? 
C41 H41B 0.9800 . ? 
C41 H41C 0.9800 . ? 
C42 H42A 0.9800 . ? 
C42 H42B 0.9800 . ? 
C42 H42C 0.9800 . ? 
S50 O53 1.498(2) . ? 
S50 C52 1.776(3) . ? 
S50 C51 1.782(3) . ? 
C51 H51A 0.9800 . ? 
C51 H51B 0.9800 . ? 
C51 H51C 0.9800 . ? 
C52 H52A 0.9800 . ? 
C52 H52B 0.9800 . ? 
C52 H52C 0.9800 . ? 
S60 O63 1.500(2) . ? 
S60 C61 1.779(3) . ? 
S60 C62 1.781(3) . ? 
C61 H61A 0.9800 . ? 
C61 H61B 0.9800 . ? 
C61 H61C 0.9800 . ? 
C62 H62A 0.9800 . ? 
C62 H62B 0.9800 . ? 
C62 H62C 0.9800 . ? 
  
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
C2 C1 C6 120.2(2) . . ? 
C2 C1 H1A 119.9 . . ? 
C6 C1 H1A 119.9 . . ? 
C3 C2 C1 120.7(2) . . ? 
C3 C2 H2A 119.7 . . ? 
C1 C2 H2A 119.7 . . ? 
C2 C3 C4 120.1(2) . . ? 
C2 C3 H3A 119.9 . . ? 
C4 C3 H3A 119.9 . . ? 
C5 C4 C3 119.2(2) . . ? 
C5 C4 H4A 120.4 . . ? 
C3 C4 H4A 120.4 . . ? 
C4 C5 C6 121.2(2) . . ? 
C4 C5 H5A 119.4 . . ? 
C6 C5 H5A 119.4 . . ? 
C1 C6 C5 118.6(2) . . ? 
C1 C6 C7 121.2(2) . . ? 
C5 C6 C7 120.2(2) . . ? 
C14 C7 N8 121.2(2) . . ? 
C14 C7 C6 122.5(2) . . ? 
N8 C7 C6 116.21(19) . . ? 
C9 N8 C7 124.16(19) . . ? 
C9 N8 H8A 117.9 . . ? 
C7 N8 H8A 117.9 . . ? 
C10 C9 N8 122.9(2) . . ? 
C10 C9 C15 121.9(2) . . ? 
N8 C9 C15 115.07(19) . . ? 
C9 C10 S11 122.07(19) . . ? 
C9 C10 H10A 119.0 . . ? 
S11 C10 H10A 119.0 . . ? 
O12 S11 O13 114.47(13) . . ? 
O12 S11 C14 109.77(13) . . ? 
O13 S11 C14 110.37(12) . . ? 
O12 S11 C10 110.20(12) . . ? 
O13 S11 C10 109.84(13) . . ? 
C14 S11 C10 101.42(12) . . ? 
C7 C14 S11 123.1(2) . . ? 
C7 C14 H14A 118.5 . . ? 
S11 C14 H14A 118.5 . . ? 
N16 C15 C20 122.9(2) . . ? 
N16 C15 C9 114.5(2) . . ? 
C20 C15 C9 122.6(2) . . ? 
C17 N16 C15 117.4(2) . . ? 
N16 C17 C18 123.7(2) . . ? 
N16 C17 C21 115.4(2) . . ? 
C18 C17 C21 120.9(2) . . ? 
C17 C18 C19 118.2(2) . . ? 
C17 C18 H18A 120.9 . . ? 
C19 C18 H18A 120.9 . . ? 
C20 C19 C18 119.3(2) . . ? 
C20 C19 H19A 120.3 . . ? 
C18 C19 H19A 120.3 . . ? 
C19 C20 C15 118.5(2) . . ? 
C19 C20 H20A 120.7 . . ? 
C15 C20 H20A 120.7 . . ? 
C28 C21 N22 124.0(2) . . ? 
C28 C21 C17 119.5(2) . . ? 
N22 C21 C17 116.5(2) . . ? 
C21 N22 C23 122.6(2) . . ? 
C21 N22 H22A 118.7 . . ? 
C23 N22 H22A 118.7 . . ? 
C24 C23 N22 122.4(2) . . ? 
C24 C23 C29 120.3(2) . . ? 
N22 C23 C29 117.3(2) . . ? 
C23 C24 S25 123.85(18) . . ? 
C23 C24 H24A 118.1 . . ? 
S25 C24 H24A 118.1 . . ? 
O27 S25 O26 113.71(12) . . ? 
O27 S25 C24 110.31(12) . . ? 
O26 S25 C24 110.56(12) . . ? 
O27 S25 C28 109.29(12) . . ? 
O26 S25 C28 110.88(12) . . ? 
C24 S25 C28 101.40(12) . . ? 
C21 C28 S25 122.67(19) . . ? 
C21 C28 H28A 118.7 . . ? 
S25 C28 H28A 118.7 . . ? 
C30 C29 C34 119.6(2) . . ? 
C30 C29 C23 120.8(2) . . ? 
C34 C29 C23 119.6(2) . . ? 
C31 C30 C29 120.0(2) . . ? 
C31 C30 H30A 120.0 . . ? 
C29 C30 H30A 120.0 . . ? 
C32 C31 C30 120.1(3) . . ? 
C32 C31 H31A 119.9 . . ? 
C30 C31 H31A 119.9 . . ? 
C33 C32 C31 120.0(2) . . ? 
C33 C32 H32A 120.0 . . ? 
C31 C32 H32A 120.0 . . ? 
C32 C33 C34 120.4(3) . . ? 
C32 C33 H33A 119.8 . . ? 
C34 C33 H33A 119.8 . . ? 
C33 C34 C29 119.8(3) . . ? 
C33 C34 H34A 120.1 . . ? 
C29 C34 H34A 120.1 . . ? 
O43 S40 C42 105.39(12) . . ? 
O43 S40 C41 105.91(12) . . ? 
C42 S40 C41 98.99(14) . . ? 
S40 C41 H41A 109.5 . . ? 
S40 C41 H41B 109.5 . . ? 
H41A C41 H41B 109.5 . . ? 
S40 C41 H41C 109.5 . . ? 
H41A C41 H41C 109.5 . . ? 
H41B C41 H41C 109.5 . . ? 
S40 C42 H42A 109.5 . . ? 
S40 C42 H42B 109.5 . . ? 
H42A C42 H42B 109.5 . . ? 
S40 C42 H42C 109.5 . . ? 
H42A C42 H42C 109.5 . . ? 
H42B C42 H42C 109.5 . . ? 
O53 S50 C52 106.37(14) . . ? 
O53 S50 C51 107.28(15) . . ? 
C52 S50 C51 97.18(17) . . ? 
S50 C51 H51A 109.5 . . ? 
S50 C51 H51B 109.5 . . ? 
H51A C51 H51B 109.5 . . ? 
S50 C51 H51C 109.5 . . ? 
H51A C51 H51C 109.5 . . ? 
H51B C51 H51C 109.5 . . ? 
S50 C52 H52A 109.5 . . ? 
S50 C52 H52B 109.5 . . ? 
H52A C52 H52B 109.5 . . ? 
S50 C52 H52C 109.5 . . ? 
H52A C52 H52C 109.5 . . ? 
H52B C52 H52C 109.5 . . ? 
O63 S60 C61 106.81(13) . . ? 
O63 S60 C62 106.43(12) . . ? 
C61 S60 C62 96.99(13) . . ? 
S60 C61 H61A 109.5 . . ? 
S60 C61 H61B 109.5 . . ? 
H61A C61 H61B 109.5 . . ? 
S60 C61 H61C 109.5 . . ? 
H61A C61 H61C 109.5 . . ? 
H61B C61 H61C 109.5 . . ? 
S60 C62 H62A 109.5 . . ? 
S60 C62 H62B 109.5 . . ? 
H62A C62 H62B 109.5 . . ? 
S60 C62 H62C 109.5 . . ? 
H62A C62 H62C 109.5 . . ? 
H62B C62 H62C 109.5 . . ? 
  
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
C6 C1 C2 C3 -1.8(4) . . . . ? 
C1 C2 C3 C4 -0.4(4) . . . . ? 
C2 C3 C4 C5 1.7(4) . . . . ? 
C3 C4 C5 C6 -0.7(4) . . . . ? 
C2 C1 C6 C5 2.7(4) . . . . ? 
C2 C1 C6 C7 -177.0(2) . . . . ? 
C4 C5 C6 C1 -1.5(4) . . . . ? 
C4 C5 C6 C7 178.3(2) . . . . ? 
C1 C6 C7 C14 -155.2(2) . . . . ? 
C5 C6 C7 C14 25.0(3) . . . . ? 
C1 C6 C7 N8 23.5(3) . . . . ? 
C5 C6 C7 N8 -156.2(2) . . . . ? 
C14 C7 N8 C9 10.9(3) . . . . ? 
C6 C7 N8 C9 -167.8(2) . . . . ? 
C7 N8 C9 C10 -12.6(4) . . . . ? 
C7 N8 C9 C15 163.7(2) . . . . ? 
N8 C9 C10 S11 -6.3(3) . . . . ? 
C15 C9 C10 S11 177.73(18) . . . . ? 
C9 C10 S11 O12 136.6(2) . . . . ? 
C9 C10 S11 O13 -96.4(2) . . . . ? 
C9 C10 S11 C14 20.4(2) . . . . ? 
N8 C7 C14 S11 9.3(3) . . . . ? 
C6 C7 C14 S11 -172.07(18) . . . . ? 
O12 S11 C14 C7 -138.5(2) . . . . ? 
O13 S11 C14 C7 94.4(2) . . . . ? 
C10 S11 C14 C7 -22.0(2) . . . . ? 
C10 C9 C15 N16 157.7(2) . . . . ? 
N8 C9 C15 N16 -18.6(3) . . . . ? 
C10 C9 C15 C20 -22.3(4) . . . . ? 
N8 C9 C15 C20 161.4(2) . . . . ? 
C20 C15 N16 C17 2.1(3) . . . . ? 
C9 C15 N16 C17 -177.8(2) . . . . ? 
C15 N16 C17 C18 -1.1(3) . . . . ? 
C15 N16 C17 C21 178.6(2) . . . . ? 
N16 C17 C18 C19 -0.2(4) . . . . ? 
C21 C17 C18 C19 -180.0(2) . . . . ? 
C17 C18 C19 C20 0.7(4) . . . . ? 
C18 C19 C20 C15 0.3(4) . . . . ? 
N16 C15 C20 C19 -1.7(4) . . . . ? 
C9 C15 C20 C19 178.2(2) . . . . ? 
N16 C17 C21 C28 -142.2(2) . . . . ? 
C18 C17 C21 C28 37.6(4) . . . . ? 
N16 C17 C21 N22 38.5(3) . . . . ? 
C18 C17 C21 N22 -141.7(2) . . . . ? 
C28 C21 N22 C23 -9.0(4) . . . . ? 
C17 C21 N22 C23 170.2(2) . . . . ? 
C21 N22 C23 C24 9.3(4) . . . . ? 
C21 N22 C23 C29 -169.5(2) . . . . ? 
N22 C23 C24 S25 5.7(4) . . . . ? 
C29 C23 C24 S25 -175.53(19) . . . . ? 
C23 C24 S25 O27 99.3(2) . . . . ? 
C23 C24 S25 O26 -134.1(2) . . . . ? 
C23 C24 S25 C28 -16.5(3) . . . . ? 
N22 C21 C28 S25 -6.3(4) . . . . ? 
C17 C21 C28 S25 174.47(19) . . . . ? 
O27 S25 C28 C21 -99.9(2) . . . . ? 
O26 S25 C28 C21 134.0(2) . . . . ? 
C24 S25 C28 C21 16.6(3) . . . . ? 
C24 C23 C29 C30 136.2(3) . . . . ? 
N22 C23 C29 C30 -45.0(3) . . . . ? 
C24 C23 C29 C34 -42.1(3) . . . . ? 
N22 C23 C29 C34 136.7(2) . . . . ? 
C34 C29 C30 C31 -0.5(4) . . . . ? 
C23 C29 C30 C31 -178.8(2) . . . . ? 
C29 C30 C31 C32 -0.9(4) . . . . ? 
C30 C31 C32 C33 1.7(4) . . . . ? 
C31 C32 C33 C34 -1.1(4) . . . . ? 
C32 C33 C34 C29 -0.3(4) . . . . ? 
C30 C29 C34 C33 1.1(4) . . . . ? 
C23 C29 C34 C33 179.4(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 
N8 H8A O43  0.88 2.12 2.971(3) 163.2 . 
N22 H22A O43  0.88 2.09 2.950(3) 166.9 . 
  
_diffrn_measured_fraction_theta_max    0.979 
_diffrn_reflns_theta_full              27.70 
_diffrn_measured_fraction_theta_full   0.979 
_refine_diff_density_max    0.282 
_refine_diff_density_min   -0.463 
_refine_diff_density_rms    0.073 
