 
data_compound 1a 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C15 H12 N2 S5' 
_chemical_formula_weight          380.57 
 
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' 
 'S'  'S'   0.1246   0.1234 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Monoclinic
_symmetry_space_group_name_H-M    P2(1)/c 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
 
_cell_length_a                    19.646(4) 
_cell_length_b                    5.849(1) 
_cell_length_c                    29.643(6) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  101.67(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      3335.8(11) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     7484 
_cell_measurement_theta_min       2.29 
_cell_measurement_theta_max       27.48  
 
_exptl_crystal_description        'Needle'? 
_exptl_crystal_colour             'Yellow' 
_exptl_crystal_size_max           0.50 
_exptl_crystal_size_mid           0.15 
_exptl_crystal_size_min           0.04 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.516 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1568 
_exptl_absorpt_coefficient_mu     0.690 
_exptl_absorpt_correction_type    'empirical' 
_exptl_absorpt_correction_T_min   0.8841 
_exptl_absorpt_correction_T_max   1.0631 
 
_exptl_special_details 
; 
 ABSCOR by T.Higashi    8 March, 1995
; 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(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   'Rigaku RAXIS RIPAD IP' 
_diffrn_measurement_method        'Oscillation' 
_diffrn_detector_area_resol_mean  '100x100 microns' 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             7484 
__diffrn_reflns_av_R_equivalents  0.0447 
_diffrn_reflns_av_sigmaI/netI     0.0697 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        25 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        7 
_diffrn_reflns_limit_l_min        -37 
_diffrn_reflns_limit_l_max        36 
_diffrn_reflns_theta_min          2.29 
_diffrn_reflns_theta_max          27.48 
_reflns_number_total              7484 
_reflns_number_gt                 5037 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'Molecular Structure Corporation (1994)
                                   MSC/AFC Diffractometer Control Software
                                   MSC, 3200 Research Forest Drive, The
                                   Woodlands, TX 77381, USA.'
_computing_cell_refinement        'Molecular Structure Corporation (1994)
                                   MSC/AFC Diffractometer Control Software
                                   MSC, 3200 Research Forest Drive, The
                                   Woodlands, TX 77381 USA.'
_computing_data_reduction         'Sheldrick, G. M. (1997) SHELXS97, Program
                                   for the Solution of Crystal Structure,
                                   University of Gottingen, Germany.'
_computing_structure_solution     'Sheldrick, G. M. (1997) SHELXS97, Program
                                   for the Solution of Crystal Structure,
                                   University of Gottingen, Germany.'
_computing_structure_refinement   'Sheldrick, G. M. (1997) SHELXL97, Program
                                   for the Refinement of Crystal Structure,
                                   University of Gottingen, Germany.'
_computing_molecular_graphics     'Interactive Molecular Graphics XP, Virsion
                                   4.2 for MSDOS (1990), Siemens Analytical
                                   X-ray Instruments Inc., Madison, Wisconsin,
                                   USA.'
_computing_publication_material   'Sheldrick, G. M. (1997) SHELXL97, Program
                                   for the refinement of Crystal Structure,
                                   University of Gottingen, Germany.'
 
 
_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)+(0.0665P)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_number_reflns          7484 
_refine_ls_number_parameters      397 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0626 
_refine_ls_R_factor_gt            0.0384 
_refine_ls_wR_factor_ref          0.1082 
_refine_ls_wR_factor_gt           0.1007 
_refine_ls_goodness_of_fit_ref    0.862 
_refine_ls_restrained_S_all       0.862 
_refine_ls_shift/su_max           0.242 
_refine_ls_shift/su_mean          0.017 
 
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 
S11 S -0.08419(4) 0.47596(13) 0.07244(2) 0.02636(16) Uani 1 1 d . . . 
S12 S -0.01506(4) 0.89117(12) 0.11993(2) 0.02501(16) Uani 1 1 d . . . 
S13 S 0.02800(3) 0.72475(13) 0.03737(2) 0.02479(16) Uani 1 1 d . . . 
S14 S 0.08486(4) 1.28445(12) 0.13605(2) 0.02632(16) Uani 1 1 d . . . 
S15 S 0.13053(3) 1.10341(13) 0.03416(2) 0.02648(17) Uani 1 1 d . . . 
S21 S 0.37352(4) 1.73559(14) 0.02474(2) 0.02800(17) Uani 1 1 d . . . 
S22 S 0.27260(4) 1.40800(13) -0.03053(2) 0.02540(16) Uani 1 1 d . . . 
S23 S 0.41894(4) 1.34528(13) -0.02753(3) 0.02714(17) Uani 1 1 d . . . 
S24 S 0.22827(4) 1.00924(13) -0.09529(3) 0.02796(17) Uani 1 1 d . . . 
S25 S 0.39830(4) 0.92837(13) -0.09023(3) 0.03294(19) Uani 1 1 d . . . 
N11 N 0.25209(13) 0.5969(4) 0.15558(9) 0.0315(6) Uani 1 1 d . . . 
N12 N 0.06218(17) 1.0408(6) 0.28254(11) 0.0535(8) Uani 1 1 d . . . 
N21 N 0.56539(15) 0.5480(5) -0.14109(10) 0.0436(7) Uani 1 1 d . . . 
N22 N 0.33760(16) 1.5275(6) -0.18960(11) 0.0486(8) Uani 1 1 d . . . 
C11 C -0.02698(13) 0.6842(5) 0.07638(9) 0.0210(6) Uani 1 1 d . . . 
C12 C 0.05170(14) 1.0438(5) 0.10239(9) 0.0223(6) Uani 1 1 d . . . 
C13 C 0.07141(13) 0.9688(5) 0.06343(9) 0.0225(6) Uani 1 1 d . . . 
C14 C 0.19742(14) 0.8818(5) 0.03749(9) 0.0264(6) Uani 1 1 d . . . 
H14A H 0.1758 0.7406 0.0247 0.032 Uiso 1 1 calc R . . 
H14B H 0.2306 0.9280 0.0191 0.032 Uiso 1 1 calc R . . 
C15 C 0.23592(13) 0.8396(5) 0.08725(9) 0.0214(6) Uani 1 1 d . . . 
C16 C 0.22269(14) 0.6456(5) 0.11036(10) 0.0261(6) Uani 1 1 d . . . 
H16 H 0.1917 0.5397 0.0943 0.031 Uiso 1 1 calc R . . 
C17 C 0.29830(14) 0.7493(6) 0.17777(10) 0.0291(7) Uani 1 1 d . . . 
H17 H 0.3195 0.7202 0.2082 0.035 Uiso 1 1 calc R . . 
C18 C 0.31575(14) 0.9485(6) 0.15717(10) 0.0296(7) Uani 1 1 d . . . 
H18 H 0.3480 1.0498 0.1736 0.036 Uiso 1 1 calc R . . 
C19 C 0.28390(13) 0.9947(5) 0.11120(10) 0.0250(6) Uani 1 1 d . . . 
H19 H 0.2947 1.1275 0.0969 0.030 Uiso 1 1 calc R . . 
C20 C 0.15204(14) 1.1508(5) 0.18077(10) 0.0258(6) Uani 1 1 d . . . 
H20A H 0.1767 1.0379 0.1662 0.031 Uiso 1 1 calc R . . 
H20B H 0.1853 1.2673 0.1939 0.031 Uiso 1 1 calc R . . 
C21 C 0.12499(13) 1.0354(5) 0.21970(9) 0.0221(6) Uani 1 1 d . . . 
C22 C 0.08388(15) 1.1504(5) 0.24605(10) 0.0287(6) Uani 1 1 d . . . 
H22 H 0.0709 1.3013 0.2391 0.034 Uiso 1 1 calc R . . 
C23 C 0.08436(17) 0.8170(6) 0.29233(12) 0.0391(8) Uani 1 1 d . . . 
H23 H 0.0719 0.7438 0.3173 0.047 Uiso 1 1 calc R . . 
C24 C 0.12216(14) 0.7042(5) 0.26787(11) 0.0284(7) Uani 1 1 d . . . 
H24 H 0.1354 0.5538 0.2752 0.034 Uiso 1 1 calc R . . 
C25 C 0.14152(15) 0.8104(5) 0.23196(11) 0.0314(7) Uani 1 1 d . . . 
H25 H 0.1674 0.7279 0.2145 0.038 Uiso 1 1 calc R . . 
C31 C 0.35563(14) 1.5101(5) -0.00914(9) 0.0228(6) Uani 1 1 d . . . 
C32 C 0.29485(14) 1.1809(5) -0.06392(9) 0.0239(6) Uani 1 1 d . . . 
C33 C 0.36374(14) 1.1537(5) -0.06245(9) 0.0236(6) Uani 1 1 d . . . 
C34 C 0.46834(14) 1.0711(5) -0.11173(10) 0.0264(6) Uani 1 1 d . . . 
H34A H 0.4500 1.1968 -0.1319 0.032 Uiso 1 1 calc R . . 
H34B H 0.5027 1.1309 -0.0863 0.032 Uiso 1 1 calc R . . 
C35 C 0.50069(13) 0.8922(5) -0.13793(9) 0.0211(6) Uani 1 1 d . . . 
C36 C 0.53987(14) 0.7130(5) -0.11513(9) 0.0254(6) Uani 1 1 d . . . 
H36 H 0.5488 0.7038 -0.0831 0.030 Uiso 1 1 calc R . . 
C37 C 0.54980(15) 0.5673(5) -0.18996(10) 0.0267(6) Uani 1 1 d . . . 
H37 H 0.5654 0.4529 -0.2071 0.032 Uiso 1 1 calc R . . 
C38 C 0.51412(12) 0.7401(5) -0.21236(8) 0.0175(5) Uani 1 1 d . . . 
H38 H 0.5060 0.7503 -0.2443 0.021 Uiso 1 1 calc R . . 
C39 C 0.49044(14) 0.8991(5) -0.18683(9) 0.0254(6) Uani 1 1 d . . . 
H39 H 0.4657 1.0217 -0.2020 0.031 Uiso 1 1 calc R . . 
C40 C 0.19663(14) 1.1960(5) -0.14592(10) 0.0281(6) Uani 1 1 d . . . 
H40A H 0.1599 1.1170 -0.1669 0.034 Uiso 1 1 calc R . . 
H40B H 0.1768 1.3335 -0.1356 0.034 Uiso 1 1 calc R . . 
C41 C 0.25247(13) 1.2641(5) -0.17184(9) 0.0227(6) Uani 1 1 d . . . 
C42 C 0.28480(15) 1.4744(5) -0.16511(10) 0.0293(7) Uani 1 1 d . . . 
H42 H 0.2721 1.5797 -0.1448 0.035 Uiso 1 1 calc R . . 
C43 C 0.35485(15) 1.3619(5) -0.21926(9) 0.0281(6) Uani 1 1 d . . . 
H43 H 0.3897 1.3960 -0.2352 0.034 Uiso 1 1 calc R . . 
C44 C 0.32454(13) 1.1587(5) -0.22608(8) 0.0189(5) Uani 1 1 d . . . 
H44 H 0.3377 1.0524 -0.2460 0.023 Uiso 1 1 calc R . . 
C45 C 0.27424(15) 1.1135(5) -0.20301(10) 0.0296(7) Uani 1 1 d . . . 
H45 H 0.2521 0.9725 -0.2080 0.036 Uiso 1 1 calc R . . 
 
 
_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 
S11 C11 1.645(3) . ? 
S12 C11 1.751(3) . ? 
S12 C12 1.750(3) . ? 
S13 C11 1.751(3) . ? 
S13 C13 1.759(3) . ? 
S14 C12 1.772(3) . ? 
S14 C20 1.845(3) . ? 
S15 C13 1.769(3) . ? 
S15 C14 1.834(3) . ? 
S21 C31 1.652(3) . ? 
S22 C31 1.732(3) . ? 
S22 C32 1.764(3) . ? 
S23 C31 1.746(3) . ? 
S23 C33 1.746(3) . ? 
S24 C32 1.758(3) . ? 
S24 C40 1.859(3) . ? 
S25 C33 1.761(3) . ? 
S25 C34 1.831(3) . ? 
N11 C17 1.345(4) . ? 
N11 C16 1.378(4) . ? 
N12 C23 1.392(5) . ? 
N12 C22 1.396(4) . ? 
N21 C36 1.390(4) . ? 
N21 C37 1.423(4) . ? 
N22 C42 1.416(4) . ? 
N22 C43 1.395(4) . ? 
C12 C13 1.363(4) . ? 
C14 C15 1.536(4) . ? 
C15 C16 1.377(4) . ? 
C15 C19 1.395(4) . ? 
C17 C18 1.390(4) . ? 
C18 C19 1.406(4) . ? 
C20 C21 1.522(4) . ? 
C21 C22 1.404(4) . ? 
C21 C25 1.386(4) . ? 
C23 C24 1.315(5) . ? 
C24 C25 1.352(4) . ? 
C32 C33 1.355(4) . ? 
C34 C35 1.517(4) . ? 
C35 C36 1.392(4) . ? 
C35 C39 1.423(4) . ? 
C37 C38 1.329(4) . ? 
C38 C39 1.340(4) . ? 
C40 C41 1.514(4) . ? 
C41 C42 1.380(4) . ? 
C41 C45 1.404(4) . ? 
C43 C44 1.326(4) . ? 
C44 C45 1.337(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 
C11 S12 C12 97.47(13) . . ? 
C11 S13 C13 97.41(13) . . ? 
C12 S14 C20 101.32(13) . . ? 
C13 S15 C14 101.16(13) . . ? 
C31 S22 C32 98.23(13) . . ? 
C31 S23 C33 98.23(13) . . ? 
C32 S24 C40 100.54(14) . . ? 
C33 S25 C34 102.09(13) . . ? 
C17 N11 C16 116.6(3) . . ? 
C23 N12 C22 117.5(3) . . ? 
C36 N21 C37 118.8(3) . . ? 
C42 N22 C43 117.9(3) . . ? 
S11 C11 S12 123.48(16) . . ? 
S11 C11 S13 123.87(17) . . ? 
S12 C11 S13 112.64(15) . . ? 
C13 C12 S12 116.5(2) . . ? 
C13 C12 S14 126.7(2) . . ? 
S12 C12 S14 116.75(16) . . ? 
C12 C13 S13 115.9(2) . . ? 
C12 C13 S15 126.9(2) . . ? 
S13 C13 S15 116.99(16) . . ? 
C15 C14 S15 111.95(19) . . ? 
C16 C15 C19 117.3(3) . . ? 
C16 C15 C14 120.3(3) . . ? 
C19 C15 C14 122.4(3) . . ? 
N11 C16 C15 124.8(3) . . ? 
N11 C17 C18 122.9(3) . . ? 
C17 C18 C19 119.1(3) . . ? 
C15 C19 C18 119.4(3) . . ? 
C21 C20 S14 115.08(19) . . ? 
C22 C21 C25 116.1(3) . . ? 
C22 C21 C20 122.5(3) . . ? 
C25 C21 C20 121.4(3) . . ? 
C21 C22 N12 120.7(3) . . ? 
C24 C23 N12 123.0(3) . . ? 
C23 C24 C25 118.9(3) . . ? 
C24 C25 C21 123.7(3) . . ? 
S21 C31 S22 124.50(16) . . ? 
S21 C31 S23 123.60(17) . . ? 
S22 C31 S23 111.90(16) . . ? 
C33 C32 S24 125.6(2) . . ? 
C33 C32 S22 115.5(2) . . ? 
S24 C32 S22 118.99(16) . . ? 
C32 C33 S23 116.1(2) . . ? 
C32 C33 S25 123.4(2) . . ? 
S23 C33 S25 120.36(16) . . ? 
C35 C34 S25 106.62(19) . . ? 
C36 C35 C39 117.8(2) . . ? 
C36 C35 C34 121.2(2) . . ? 
C39 C35 C34 121.0(3) . . ? 
N21 C36 C35 118.7(3) . . ? 
C38 C37 N21 123.5(3) . . ? 
C37 C38 C39 117.0(2) . . ? 
C38 C39 C35 124.2(3) . . ? 
C41 C40 S24 113.95(19) . . ? 
C42 C41 C45 117.5(3) . . ? 
C42 C41 C40 121.4(3) . . ? 
C45 C41 C40 121.1(3) . . ? 
C41 C42 N22 119.0(3) . . ? 
C44 C43 N22 124.0(3) . . ? 
C43 C44 C45 117.1(3) . . ? 
C44 C45 C41 124.6(3) . . ? 
 
_diffrn_measured_fraction_theta_max    0.975 
_diffrn_reflns_theta_full              27.48 
_diffrn_measured_fraction_theta_full   0.975 
_refine_diff_density_max    0.737 
_refine_diff_density_min   -0.717 
_refine_diff_density_rms    0.078 

 
data_compound 3a 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C9 H7 N S4' 
_chemical_formula_weight          257.40 
 
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' 
 'S'  'S'   0.1246   0.1234 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Monoclinic
_symmetry_space_group_name_H-M    C2/c 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y, -z+1/2' 
 'x+1/2, y+1/2, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y, z-1/2' 
 '-x+1/2, -y+1/2, -z' 
 'x+1/2, -y+1/2, z-1/2' 
 
_cell_length_a                    12.996(3) 
_cell_length_b                    7.934(2) 
_cell_length_c                    22.205(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  109.62(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      2156.6(8) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     2434 
_cell_measurement_theta_min       3.04 
_cell_measurement_theta_max       27.48 
 
_exptl_crystal_description        'block' 
_exptl_crystal_colour             'yellow' 
_exptl_crystal_size_max           0.1 mm 
_exptl_crystal_size_mid           0.1 mm  
_exptl_crystal_size_min           0.1 mm 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.585 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1056 
_exptl_absorpt_coefficient_mu     0.837 
_exptl_absorpt_correction_type    'ABSOR by T. Higashi'
_exptl_absorpt_correction_T_min   0.8490
_exptl_absorpt_correction_T_max   1.0957 

_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(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   'Rigaku RAXIS RIPAD IP' 
_diffrn_measurement_method        'Oscillation' 
_diffrn_detector_area_resol_mean  '100x100 microns' 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             2434 
_diffrn_reflns_av_R_equivalents   0.02563 
_diffrn_reflns_av_sigmaI/netI     0.0232 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        16 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        10 
_diffrn_reflns_limit_l_min        -28 
_diffrn_reflns_limit_l_max        26 
_diffrn_reflns_theta_min          3.04 
_diffrn_reflns_theta_max          27.48 
_reflns_number_total              2434 
_reflns_number_gt                 2152 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'Molecular Structure Corporation (1994)
                                   MSC/AFC Diffractometer Control Software
                                   MSC, 3200 Research Forest Drive, The
                                   Woodlands, TX 77381, USA.'
_computing_cell_refinement        'Molecular Structure Corporation (1994)
                                   MSC/AFC Diffractometer Control Software
                                   MSC, 3200 Research Forest Drive, The
                                   Woodlands, TX 77381 USA.'
_computing_data_reduction         'Sheldrick, G. M. (1997) SHELXS97, Program
                                   for the Solution of Crystal Structure,
                                   University of Gottingen, Germany.'
_computing_structure_solution     'Sheldrick, G. M. (1997) SHELXS97, Program
                                   for the Solution of Crystal Structure,
                                   University of Gottingen, Germany.'
_computing_structure_refinement   'Sheldrick, G. M. (1997) SHELXL97, Program
                                   for the Refinement of Crystal Structure,
                                   University of Gottingen, Germany.'
_computing_molecular_graphics     'Interactive Molecular Graphics XP, Virsion
                                   4.2 for MSDOS (1990), Siemens Analytical
                                   X-ray Instruments Inc., Madison, Wisconsin,
                                   USA.'
_computing_publication_material   'Sheldrick, G. M. (1997) SHELXL97, Program
                                   for the refinement of Crystal Structure,
                                   University of Gottingen, Germany.'
 
_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)+(0.0610P)²+4.0078P] 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          2434 
_refine_ls_number_parameters      130 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0409 
_refine_ls_R_factor_gt            0.0357 
_refine_ls_wR_factor_ref          0.1099 
_refine_ls_wR_factor_gt           0.1062 
_refine_ls_goodness_of_fit_ref    1.132 
_refine_ls_restrained_S_all       1.132 
_refine_ls_shift/su_max           0.072 
_refine_ls_shift/su_mean          0.007 
 
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 0.42355(5) 0.35936(7) 0.33499(3) 0.02110(16) Uani 1 1 d . . . 
S2 S 0.40664(4) 0.07857(7) 0.42260(3) 0.01863(16) Uani 1 1 d . . . 
S3 S 0.34947(5) -0.17331(7) 0.32283(3) 0.02018(16) Uani 1 1 d . . . 
S4 S 0.35079(5) -0.26616(8) 0.45400(3) 0.02653(18) Uani 1 1 d . . . 
N1 N 0.64905(19) 0.8187(3) 0.42516(12) 0.0341(5) Uani 1 1 d . . . 
C1 C 0.65237(16) 0.7890(3) 0.31776(10) 0.0131(4) Uani 1 1 d . . . 
H1 H 0.6632 0.8350 0.2818 0.016 Uiso 1 1 calc R . . 
C2 C 0.62348(18) 0.6281(3) 0.31951(11) 0.0187(4) Uani 1 1 d . . . 
H2 H 0.6147 0.5622 0.2835 0.022 Uiso 1 1 calc R . . 
C3 C 0.60548(17) 0.5521(3) 0.37178(11) 0.0183(4) Uani 1 1 d . . . 
C4 C 0.61790(19) 0.6509(3) 0.42580(11) 0.0214(5) Uani 1 1 d . . . 
H4 H 0.6057 0.6056 0.4614 0.026 Uiso 1 1 calc R . . 
C5 C 0.66491(19) 0.8808(3) 0.37040(12) 0.0217(5) Uani 1 1 d . . . 
H5 H 0.6855 0.9930 0.3703 0.026 Uiso 1 1 calc R . . 
C6 C 0.57277(19) 0.3698(3) 0.36848(13) 0.0232(5) Uani 1 1 d . . . 
H6A H 0.5981 0.3203 0.4109 0.028 Uiso 1 1 calc R . . 
H6B H 0.6050 0.3079 0.3416 0.028 Uiso 1 1 calc R . . 
C7 C 0.40269(18) 0.1450(3) 0.34673(11) 0.0174(4) Uani 1 1 d . . . 
C8 C 0.37664(19) 0.0267(3) 0.30119(11) 0.0194(4) Uani 1 1 d . . . 
C9 C 0.36835(18) -0.1284(3) 0.40265(11) 0.0189(4) Uani 1 1 d . . . 
H11 H 0.372(4) 0.043(7) 0.260(2) 0.080 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 
S1 C7 1.756(2) . ? 
S1 C6 1.831(2) . ? 
S2 C9 1.730(2) . ? 
S2 C7 1.749(2) . ? 
S3 C8 1.728(2) . ? 
S3 C9 1.743(2) . ? 
S4 C9 1.650(2) . ? 
N1 C4 1.393(4) . ? 
N1 C5 1.390(4) . ? 
C1 C2 1.335(3) . ? 
C1 C5 1.340(3) . ? 
C2 C3 1.396(3) . ? 
C3 C4 1.396(3) . ? 
C3 C6 1.502(3) . ? 
C7 C8 1.337(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 
C7 S1 C6 100.30(11) . . ? 
C9 S2 C7 97.26(11) . . ? 
C8 S3 C9 97.05(11) . . ? 
C4 N1 C5 118.5(2) . . ? 
C2 C1 C5 116.6(2) . . ? 
C1 C2 C3 124.4(2) . . ? 
C2 C3 C4 118.0(2) . . ? 
C2 C3 C6 119.9(2) . . ? 
C4 C3 C6 122.1(2) . . ? 
N1 C4 C3 118.6(2) . . ? 
C1 C5 N1 124.1(2) . . ? 
C3 C6 S1 107.89(15) . . ? 
C8 C7 S2 115.78(18) . . ? 
C8 C7 S1 125.47(19) . . ? 
S2 C7 S1 118.60(13) . . ? 
C7 C8 S3 117.24(19) . . ? 
S4 C9 S2 123.14(15) . . ? 
S4 C9 S3 124.23(14) . . ? 
S2 C9 S3 112.63(13) . . ? 
 
_diffrn_measured_fraction_theta_max    0.988 
_diffrn_reflns_theta_full              27.48 
_diffrn_measured_fraction_theta_full   0.988 
_refine_diff_density_max    0.828 
_refine_diff_density_min   -0.895 
_refine_diff_density_rms    0.091 
