 
data_02sot039b 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C34 H31 N7 O12 S2' 
_chemical_formula_weight          793.78 
 
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
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
 
_cell_length_a                    8.608(5) 
_cell_length_b                    15.212(5) 
_cell_length_c                    15.257(5) 
_cell_angle_alpha                 67.786(5) 
_cell_angle_beta                  84.475(5) 
_cell_angle_gamma                 73.886(5) 
_cell_volume                      1776.8(13) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     120(2) 
_cell_measurement_reflns_used     12215 
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        plate
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.15 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.02 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.484 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              824 
_exptl_absorpt_coefficient_mu     0.225 
_exptl_absorpt_correction_type    multiscans 
_exptl_absorpt_correction_T_min   0.9670 
_exptl_absorpt_correction_T_max   0.9955 
_exptl_absorpt_process_details    'SORTAV (Blessing, 1997)' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       120(2) 
_diffrn_radiation_wavelength      0.71069 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'Bruker-Nonius FR591 rotating anode' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Bruker-Nonius KappaCCD'
_diffrn_measurement_method        'Φ & ω scans'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             19499 
_diffrn_reflns_av_R_equivalents   0.1126 
_diffrn_reflns_av_sigmaI/netI     0.1403 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -18 
_diffrn_reflns_limit_k_max        18 
_diffrn_reflns_limit_l_min        -18 
_diffrn_reflns_limit_l_max        18 
_diffrn_reflns_theta_min          3.16 
_diffrn_reflns_theta_max          25.03 
_reflns_number_total              6028 
_reflns_number_gt                 3187 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'
_computing_cell_refinement        'DENZO & COLLECT'
_computing_data_reduction         'DENZO & COLLECT'
_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 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)+(0.0480P)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      SHELXL 
_refine_ls_extinction_coef        0.0025(6) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          6028 
_refine_ls_number_parameters      501 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.1424 
_refine_ls_R_factor_gt            0.0559 
_refine_ls_wR_factor_ref          0.1242 
_refine_ls_wR_factor_gt           0.0998 
_refine_ls_goodness_of_fit_ref    0.909 
_refine_ls_restrained_S_all       0.909 
_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 
C1 C 0.1869(4) 0.4926(3) 0.1351(3) 0.0227(9) Uani 1 1 d . . . 
H1 H 0.2179 0.4567 0.1996 0.027 Uiso 1 1 calc R . . 
C2 C 0.0499(4) 0.5698(3) 0.1105(3) 0.0218(9) Uani 1 1 d . . . 
C3 C -0.0024(5) 0.6250(3) 0.0184(3) 0.0239(9) Uani 1 1 d . . . 
H3 H -0.0972 0.6782 0.0029 0.029 Uiso 1 1 calc R . . 
C4 C 0.0934(4) 0.5971(3) -0.0500(3) 0.0221(9) Uani 1 1 d . . . 
C5 C 0.2313(4) 0.5204(3) -0.0308(3) 0.0218(9) Uani 1 1 d . . . 
H5 H 0.2917 0.5038 -0.0804 0.026 Uiso 1 1 calc R . . 
C6 C 0.2797(4) 0.4680(3) 0.0632(3) 0.0224(9) Uani 1 1 d . . . 
C7 C 0.5198(4) 0.3451(3) 0.0369(3) 0.0208(9) Uani 1 1 d . . . 
C8 C 0.6454(4) 0.2562(3) 0.0902(3) 0.0201(9) Uani 1 1 d . . . 
C9 C 0.6793(4) 0.2024(3) 0.1852(3) 0.0209(9) Uani 1 1 d . . . 
C10 C 0.8279(4) 0.1314(3) 0.1905(3) 0.0200(9) Uani 1 1 d . . . 
C11 C 0.8788(4) 0.1438(3) 0.0978(3) 0.0197(9) Uani 1 1 d . . . 
C12 C 1.0223(4) 0.0844(3) 0.0665(3) 0.0208(9) Uani 1 1 d . . . 
C13 C 1.1846(4) 0.0761(3) -0.0742(3) 0.0218(9) Uani 1 1 d . . . 
C14 C 1.2037(5) 0.1309(3) -0.1689(3) 0.0236(9) Uani 1 1 d . . . 
H14 H 1.1252 0.1903 -0.2009 0.028 Uiso 1 1 calc R . . 
C15 C 1.3384(4) 0.0976(3) -0.2157(3) 0.0228(9) Uani 1 1 d . . . 
C16 C 1.4575(4) 0.0121(3) -0.1734(3) 0.0225(9) Uani 1 1 d . . . 
H16 H 1.5509 -0.0088 -0.2064 0.027 Uiso 1 1 calc R . . 
C17 C 1.4315(4) -0.0401(3) -0.0809(3) 0.0215(9) Uani 1 1 d . . . 
C18 C 1.2992(4) -0.0119(3) -0.0298(3) 0.0213(9) Uani 1 1 d . . . 
H18 H 1.2866 -0.0517 0.0342 0.026 Uiso 1 1 calc R . . 
C19 C 0.5763(4) 0.2147(3) 0.2660(3) 0.0226(9) Uani 1 1 d . . . 
C20 C 0.6320(5) 0.2406(3) 0.3331(3) 0.0267(10) Uani 1 1 d . . . 
H20 H 0.7387 0.2482 0.3287 0.032 Uiso 1 1 calc R . . 
C21 C 0.5333(5) 0.2555(3) 0.4060(3) 0.0329(11) Uani 1 1 d . . . 
H21 H 0.5719 0.2735 0.4513 0.039 Uiso 1 1 calc R . . 
C22 C 0.3782(5) 0.2440(3) 0.4127(3) 0.0331(11) Uani 1 1 d . . . 
H22 H 0.3103 0.2542 0.4627 0.040 Uiso 1 1 calc R . . 
C23 C 0.3222(5) 0.2180(3) 0.3474(3) 0.0300(10) Uani 1 1 d . . . 
H23 H 0.2154 0.2105 0.3521 0.036 Uiso 1 1 calc R . . 
C24 C 0.4212(5) 0.2026(3) 0.2748(3) 0.0248(9) Uani 1 1 d . . . 
H24 H 0.3823 0.1834 0.2304 0.030 Uiso 1 1 calc R . . 
C25 C 0.9112(4) 0.0569(3) 0.2797(3) 0.0221(9) Uani 1 1 d . . . 
C26 C 1.0704(4) 0.0483(3) 0.2988(3) 0.0247(9) Uani 1 1 d . . . 
H26 H 1.1287 0.0898 0.2540 0.030 Uiso 1 1 calc R . . 
C27 C 1.1446(5) -0.0205(3) 0.3829(3) 0.0319(11) Uani 1 1 d . . . 
H27 H 1.2536 -0.0260 0.3956 0.038 Uiso 1 1 calc R . . 
C28 C 1.0599(6) -0.0810(3) 0.4483(3) 0.0376(11) Uani 1 1 d . . . 
H28 H 1.1117 -0.1288 0.5054 0.045 Uiso 1 1 calc R . . 
C29 C 0.9007(6) -0.0725(3) 0.4313(3) 0.0353(11) Uani 1 1 d . . . 
H29 H 0.8426 -0.1141 0.4763 0.042 Uiso 1 1 calc R . . 
C30 C 0.8266(5) -0.0023(3) 0.3475(3) 0.0279(10) Uani 1 1 d . . . 
H30 H 0.7161 0.0053 0.3364 0.033 Uiso 1 1 calc R . . 
C31 C 0.7663(5) 0.5259(3) 0.4853(3) 0.0411(12) Uani 1 1 d . . . 
H31A H 0.6649 0.5728 0.4904 0.062 Uiso 1 1 calc R . . 
H31B H 0.8345 0.5607 0.4371 0.062 Uiso 1 1 calc R . . 
H31C H 0.8232 0.4944 0.5465 0.062 Uiso 1 1 calc R . . 
C32 C 0.9243(5) 0.3597(3) 0.4584(3) 0.0445(12) Uani 1 1 d . . . 
H32A H 0.9671 0.3357 0.5229 0.067 Uiso 1 1 calc R . . 
H32B H 0.9925 0.3982 0.4141 0.067 Uiso 1 1 calc R . . 
H32C H 0.9239 0.3036 0.4416 0.067 Uiso 1 1 calc R . . 
C33 C 0.7290(7) 0.2044(4) 0.7351(4) 0.0593(16) Uani 1 1 d . . . 
H33A H 0.8310 0.1542 0.7394 0.089 Uiso 1 1 calc R . . 
H33B H 0.6760 0.2232 0.6742 0.089 Uiso 1 1 calc R . . 
H33C H 0.6581 0.1780 0.7868 0.089 Uiso 1 1 calc R . . 
C34 C 0.5679(6) 0.3761(5) 0.7450(4) 0.0673(18) Uani 1 1 d . . . 
H34A H 0.5084 0.3355 0.7944 0.101 Uiso 1 1 calc R . . 
H34B H 0.5169 0.3963 0.6833 0.101 Uiso 1 1 calc R . . 
H34C H 0.5664 0.4346 0.7582 0.101 Uiso 1 1 calc R . . 
N1 N -0.0469(4) 0.5927(3) 0.1879(3) 0.0295(8) Uani 1 1 d . . . 
N2 N 0.0413(4) 0.6506(2) -0.1489(2) 0.0264(8) Uani 1 1 d . . . 
N3 N 0.4153(4) 0.3873(2) 0.0920(2) 0.0251(8) Uani 1 1 d . . . 
H3A H 0.4359 0.3603 0.1532 0.030 Uiso 1 1 calc R . . 
N4 N 0.7654(3) 0.2207(2) 0.0379(2) 0.0194(7) Uani 1 1 d . . . 
H4 H 0.7697 0.2433 -0.0244 0.023 Uiso 1 1 calc R . . 
N5 N 1.0493(4) 0.1152(2) -0.0291(2) 0.0237(8) Uani 1 1 d . . . 
H5A H 0.9742 0.1644 -0.0656 0.028 Uiso 1 1 calc R . . 
N6 N 1.3551(4) 0.1585(3) -0.3156(2) 0.0293(8) Uani 1 1 d . . . 
N7 N 1.5525(4) -0.1327(2) -0.0309(3) 0.0244(8) Uani 1 1 d . . . 
O1 O 0.0052(3) 0.5475(2) 0.2690(2) 0.0341(7) Uani 1 1 d . . . 
O2 O -0.1755(3) 0.6564(2) 0.1662(2) 0.0391(8) Uani 1 1 d . . . 
O3 O -0.0786(4) 0.7208(2) -0.1671(2) 0.0385(8) Uani 1 1 d . . . 
O4 O 0.1190(3) 0.6215(2) -0.20953(19) 0.0357(7) Uani 1 1 d . . . 
O5 O 0.5147(3) 0.3793(2) -0.04923(19) 0.0284(7) Uani 1 1 d . . . 
O6 O 1.1102(3) 0.0112(2) 0.12324(18) 0.0301(7) Uani 1 1 d . . . 
O7 O 1.2495(4) 0.2339(2) -0.35233(19) 0.0420(8) Uani 1 1 d . . . 
O8 O 1.4744(4) 0.1290(2) -0.3580(2) 0.0427(8) Uani 1 1 d . . . 
O9 O 1.6663(3) -0.1620(2) -0.07674(19) 0.0336(7) Uani 1 1 d . . . 
O10 O 1.5345(3) -0.1748(2) 0.0539(2) 0.0315(7) Uani 1 1 d . . . 
O11 O 0.6356(3) 0.3780(2) 0.53394(19) 0.0348(7) Uani 1 1 d . . . 
O12 O 0.8331(3) 0.2750(2) 0.84337(17) 0.0272(7) Uani 1 1 d . . . 
S1 S 0.72342(13) 0.43523(8) 0.45242(8) 0.0338(3) Uani 1 1 d . . . 
S2 S 0.76805(12) 0.30797(8) 0.74368(7) 0.0271(3) 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 1.376(5) . ? 
C1 C6 1.398(5) . ? 
C2 C3 1.379(5) . ? 
C2 N1 1.473(5) . ? 
C3 C4 1.387(5) . ? 
C4 C5 1.377(5) . ? 
C4 N2 1.463(5) . ? 
C5 C6 1.390(5) . ? 
C6 N3 1.400(5) . ? 
C7 O5 1.216(4) . ? 
C7 N3 1.368(5) . ? 
C7 C8 1.478(5) . ? 
C8 N4 1.362(5) . ? 
C8 C9 1.381(5) . ? 
C9 C10 1.413(5) . ? 
C9 C19 1.489(5) . ? 
C10 C11 1.396(5) . ? 
C10 C25 1.491(5) . ? 
C11 N4 1.374(5) . ? 
C11 C12 1.471(5) . ? 
C12 O6 1.221(4) . ? 
C12 N5 1.371(5) . ? 
C13 C14 1.389(5) . ? 
C13 C18 1.391(5) . ? 
C13 N5 1.398(5) . ? 
C14 C15 1.377(5) . ? 
C15 C16 1.382(5) . ? 
C15 N6 1.473(5) . ? 
C16 C17 1.365(5) . ? 
C17 C18 1.377(5) . ? 
C17 N7 1.476(5) . ? 
C19 C24 1.385(5) . ? 
C19 C20 1.391(5) . ? 
C20 C21 1.383(5) . ? 
C21 C22 1.383(6) . ? 
C22 C23 1.370(6) . ? 
C23 C24 1.384(5) . ? 
C25 C30 1.388(5) . ? 
C25 C26 1.388(5) . ? 
C26 C27 1.385(6) . ? 
C27 C28 1.383(6) . ? 
C28 C29 1.381(6) . ? 
C29 C30 1.388(6) . ? 
C31 S1 1.769(4) . ? 
C32 S1 1.780(4) . ? 
C33 S2 1.753(5) . ? 
C34 S2 1.749(5) . ? 
N1 O1 1.223(4) . ? 
N1 O2 1.228(4) . ? 
N2 O3 1.226(4) . ? 
N2 O4 1.235(4) . ? 
N6 O7 1.220(4) . ? 
N6 O8 1.229(4) . ? 
N7 O10 1.223(4) . ? 
N7 O9 1.229(4) . ? 
O11 S1 1.497(3) . ? 
O12 S2 1.520(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 
C2 C1 C6 118.7(4) . . ? 
C1 C2 C3 123.8(3) . . ? 
C1 C2 N1 117.4(3) . . ? 
C3 C2 N1 118.8(3) . . ? 
C2 C3 C4 115.1(4) . . ? 
C5 C4 C3 124.4(4) . . ? 
C5 C4 N2 117.8(3) . . ? 
C3 C4 N2 117.7(3) . . ? 
C4 C5 C6 118.1(4) . . ? 
C5 C6 C1 119.9(4) . . ? 
C5 C6 N3 123.5(3) . . ? 
C1 C6 N3 116.5(3) . . ? 
O5 C7 N3 123.2(4) . . ? 
O5 C7 C8 122.1(3) . . ? 
N3 C7 C8 114.6(3) . . ? 
N4 C8 C9 109.2(3) . . ? 
N4 C8 C7 116.2(3) . . ? 
C9 C8 C7 134.4(3) . . ? 
C8 C9 C10 106.7(3) . . ? 
C8 C9 C19 126.5(3) . . ? 
C10 C9 C19 126.7(3) . . ? 
C11 C10 C9 107.4(3) . . ? 
C11 C10 C25 127.3(3) . . ? 
C9 C10 C25 125.3(3) . . ? 
N4 C11 C10 107.7(3) . . ? 
N4 C11 C12 124.4(3) . . ? 
C10 C11 C12 127.9(3) . . ? 
O6 C12 N5 122.5(3) . . ? 
O6 C12 C11 121.2(3) . . ? 
N5 C12 C11 116.3(3) . . ? 
C14 C13 C18 119.3(3) . . ? 
C14 C13 N5 116.5(3) . . ? 
C18 C13 N5 124.1(3) . . ? 
C15 C14 C13 118.9(4) . . ? 
C14 C15 C16 123.6(4) . . ? 
C14 C15 N6 117.1(3) . . ? 
C16 C15 N6 119.3(3) . . ? 
C17 C16 C15 115.3(3) . . ? 
C16 C17 C18 124.3(4) . . ? 
C16 C17 N7 118.6(3) . . ? 
C18 C17 N7 117.0(3) . . ? 
C17 C18 C13 118.5(4) . . ? 
C24 C19 C20 118.7(3) . . ? 
C24 C19 C9 120.4(3) . . ? 
C20 C19 C9 120.9(3) . . ? 
C21 C20 C19 120.5(4) . . ? 
C20 C21 C22 119.8(4) . . ? 
C23 C22 C21 120.2(4) . . ? 
C22 C23 C24 120.0(4) . . ? 
C23 C24 C19 120.8(4) . . ? 
C30 C25 C26 118.8(4) . . ? 
C30 C25 C10 119.7(3) . . ? 
C26 C25 C10 121.4(3) . . ? 
C27 C26 C25 120.4(4) . . ? 
C28 C27 C26 119.9(4) . . ? 
C29 C28 C27 120.5(4) . . ? 
C28 C29 C30 119.1(4) . . ? 
C25 C30 C29 121.1(4) . . ? 
O1 N1 O2 124.3(3) . . ? 
O1 N1 C2 118.5(3) . . ? 
O2 N1 C2 117.2(3) . . ? 
O3 N2 O4 123.4(3) . . ? 
O3 N2 C4 118.4(3) . . ? 
O4 N2 C4 118.2(3) . . ? 
C7 N3 C6 128.1(3) . . ? 
C8 N4 C11 109.0(3) . . ? 
C12 N5 C13 126.4(3) . . ? 
O7 N6 O8 123.6(3) . . ? 
O7 N6 C15 118.8(3) . . ? 
O8 N6 C15 117.5(3) . . ? 
O10 N7 O9 124.1(3) . . ? 
O10 N7 C17 118.0(3) . . ? 
O9 N7 C17 117.9(3) . . ? 
O11 S1 C31 106.3(2) . . ? 
O11 S1 C32 106.1(2) . . ? 
C31 S1 C32 98.0(2) . . ? 
O12 S2 C34 105.52(19) . . ? 
O12 S2 C33 106.0(2) . . ? 
C34 S2 C33 98.3(3) . . ? 
 
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 
N4 H4 O12  0.88 1.95 2.812(4) 166.2 1_554 
N5 H5A O12  0.88 1.91 2.787(4) 172.5 1_554 
 
_diffrn_measured_fraction_theta_max    0.963 
_diffrn_reflns_theta_full              25.03 
_diffrn_measured_fraction_theta_full   0.963 
_refine_diff_density_max    0.297 
_refine_diff_density_min   -0.310 
_refine_diff_density_rms    0.069 
