 
#  CIF produced by WinGX routine CIF_UPDATE
#  Created on 2002-08-09 at 17:54:42
#  Using CIFtbx version 2.6.2 16 Jun 1998
 
#  Dictionary name : cif_core.dic
#  Dictionary vers : 2.2
#  Request file    : c:\wingx\files\archive.dat
#  CIF files read  : ljf029 dreduc sortav struct
 
 
data_ljf029
 
_audit_creation_date            2002-08-09T17:54:42-00:00
_audit_creation_method         'WinGX routine CIF_UPDATE'
_audit_conform_dict_name        cif_core.dic
_audit_conform_dict_version     2.2
_audit_conform_dict_location    ftp://ftp.iucr.org/pub/cif_core.dic
_publ_requested_category        FO
 
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#
 
_chemical_name_systematic
;
 ?
;
_chemical_formula_moiety                'C15 H21 N O2 S2'
_chemical_formula_sum                   'C15 H21 N O2 S2'
_chemical_formula_weight                311.45
_chemical_compound_source               'synthesis as described'
 
#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#
 
_symmetry_cell_setting                  monoclinic
_symmetry_space_group_name_H-M          'P 21/a'
_symmetry_space_group_name_Hall         '-P 2yab'
_symmetry_Int_Tables_number             14
loop_
    _symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'
 
_cell_length_a                          12.9071(5)
_cell_length_b                          6.4873(2)
_cell_length_c                          19.0794(8)
_cell_angle_alpha                       90
_cell_angle_beta                        99.5470(10)
_cell_angle_gamma                       90
_cell_volume                            1575.43(10)
_cell_formula_units_Z                   4
_cell_measurement_temperature           150(2)
_cell_measurement_reflns_used           84145
_cell_measurement_theta_min             2.91
_cell_measurement_theta_max             27.485
_cell_measurement_wavelength            0.71073
 
#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#
 
_exptl_crystal_description              prism
_exptl_crystal_colour                   colourless
_exptl_crystal_size_max                 0.35
_exptl_crystal_size_mid                 0.25
_exptl_crystal_size_min                 0.03
_exptl_crystal_density_diffrn           1.313
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    664
_exptl_special_details
;
 ?
;
 
#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#
 
_exptl_absorpt_coefficient_mu           0.339
_exptl_absorpt_correction_type          multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_correction_T_min         0.814
_exptl_absorpt_correction_T_max         1.156
 
#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#
 
_diffrn_source                          'Enraf Nonius FR590'
_diffrn_ambient_temperature             150(2)
_diffrn_radiation_wavelength            0.71073
_diffrn_radiation_type                  MoK\a
_diffrn_radiation_monochromator         graphite
_diffrn_radiation_probe                 x-ray
_diffrn_detector                        'CCD plate'
_diffrn_orient_matrix_type              'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_ub_11             0.138019E-1
_diffrn_orient_matrix_ub_12             -0.401958E-1
_diffrn_orient_matrix_ub_13             -0.660776E-1
_diffrn_orient_matrix_ub_21             0.147092
_diffrn_orient_matrix_ub_22             0.460204E-1
_diffrn_orient_matrix_ub_23             0.2729E-2
_diffrn_orient_matrix_ub_31             0.142345E-1
_diffrn_orient_matrix_ub_32             -0.467374E-1
_diffrn_orient_matrix_ub_33             0.209231E-1
_diffrn_measurement_device              '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type         KappaCCD
_diffrn_measurement_method              'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents         0.0873
_diffrn_reflns_av_unetI/netI            0.0555
_diffrn_reflns_number                   3606
_diffrn_reflns_limit_h_min              -16
_diffrn_reflns_limit_h_max              16
_diffrn_reflns_limit_k_min              -8
_diffrn_reflns_limit_k_max              8
_diffrn_reflns_limit_l_min              -24
_diffrn_reflns_limit_l_max              24
_diffrn_reflns_theta_min                3.25
_diffrn_reflns_theta_max                27.5
_diffrn_reflns_theta_full               27.5
_diffrn_measured_fraction_theta_full
                                        0.994
_diffrn_measured_fraction_theta_max
                                        0.994
_reflns_number_total                    3606
_reflns_number_gt                       2942
_reflns_threshold_expression            >2sigma(I)
_diffrn_reflns_reduction_process
;
 Scaled and merged with SORTAV
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
 
#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#
 
_computing_data_collection              'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement
                                       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
                             'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement         'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics           'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
                                   'WinGX publication routines (Farrugia, 1999)'
 
#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#
 
_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)+(0.0398P)²+0.8451P] 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_number_reflns                3606
_refine_ls_number_parameters            188
_refine_ls_number_restraints            0
_refine_ls_R_factor_all                 0.0623
_refine_ls_R_factor_gt                  0.0465
_refine_ls_wR_factor_ref                0.1126
_refine_ls_wR_factor_gt                 0.1076
_refine_ls_goodness_of_fit_ref          1.098
_refine_ls_restrained_S_all             1.098
_refine_ls_shift/su_max                 0
_refine_ls_shift/su_mean                0
_refine_diff_density_max                0.353
_refine_diff_density_min                -0.273
_refine_diff_density_rms                0.057
 
#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#
 
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 0 '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 0.006 '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'
 
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 0.16171(4) 0.46167(8) 0.38065(3) 0.02837(15) Uani 1 1 d . . .
S3 S 0.26462(4) 0.87841(8) 0.40733(3) 0.02574(14) Uani 1 1 d . . .
O1 O 0.28873(13) 0.9464(3) 0.11573(8) 0.0394(4) Uani 1 1 d . . .
O2 O 0.19977(11) 1.1855(2) 0.17053(8) 0.0289(3) Uani 1 1 d . . .
N1 N 0.28168(14) 0.9345(3) 0.23453(10) 0.0278(4) Uani 1 1 d . . .
C1" C 0.25952(16) 1.0163(3) 0.16776(11) 0.0281(5) Uani 1 1 d . . .
C2 C 0.21748(15) 0.6807(3) 0.34128(11) 0.0229(4) Uani 1 1 d . . .
H2 H 0.1614 0.7431 0.305 0.027 Uiso 1 1 calc R . .
C6 C 0.05415(16) 0.5950(3) 0.41140(12) 0.0317(5) Uani 1 1 d . . .
H6A H 0.009 0.658 0.3699 0.038 Uiso 1 1 calc R . .
H6B H 0.0111 0.4925 0.4322 0.038 Uiso 1 1 calc R . .
C5 C 0.08820(16) 0.7622(3) 0.46629(12) 0.0290(5) Uani 1 1 d . . .
H5A H 0.1369 0.7014 0.5065 0.035 Uiso 1 1 calc R . .
H5B H 0.0257 0.8127 0.4849 0.035 Uiso 1 1 calc R . .
C4 C 0.14214(16) 0.9446(3) 0.43710(12) 0.0277(4) Uani 1 1 d . . .
H4A H 0.1565 1.0514 0.4745 0.033 Uiso 1 1 calc R . .
H4B H 0.0935 1.0049 0.3967 0.033 Uiso 1 1 calc R . .
C1' C 0.30793(15) 0.6198(3) 0.30464(11) 0.0234(4) Uani 1 1 d . . .
C2' C 0.33767(15) 0.7484(3) 0.25232(11) 0.0245(4) Uani 1 1 d . . .
C3' C 0.42125(16) 0.6930(3) 0.21821(12) 0.0308(5) Uani 1 1 d . . .
H3' H 0.4423 0.7816 0.1835 0.037 Uiso 1 1 calc R . .
C4' C 0.47338(16) 0.5087(3) 0.23518(12) 0.0333(5) Uani 1 1 d . . .
H4' H 0.5297 0.4707 0.2115 0.04 Uiso 1 1 calc R . .
C5' C 0.44464(17) 0.3792(3) 0.28614(12) 0.0334(5) Uani 1 1 d . . .
H5' H 0.4804 0.2523 0.2971 0.04 Uiso 1 1 calc R . .
C6' C 0.36316(16) 0.4363(3) 0.32104(11) 0.0276(5) Uani 1 1 d . . .
H6' H 0.3445 0.3488 0.3569 0.033 Uiso 1 1 calc R . .
C2" C 0.16004(18) 1.3024(3) 0.10499(12) 0.0317(5) Uani 1 1 d . . .
C3" C 0.0989(2) 1.4748(4) 0.13350(14) 0.0419(6) Uani 1 1 d . . .
H3"1 H 0.0429 1.4155 0.1561 0.063 Uiso 1 1 calc R . .
H3"2 H 0.068 1.5645 0.0942 0.063 Uiso 1 1 calc R . .
H3"3 H 0.1465 1.5554 0.1685 0.063 Uiso 1 1 calc R . .
C5" C 0.2507(2) 1.3875(4) 0.07235(13) 0.0410(6) Uani 1 1 d . . .
H5"1 H 0.2966 1.4696 0.1078 0.062 Uiso 1 1 calc R . .
H5"2 H 0.2232 1.4747 0.0315 0.062 Uiso 1 1 calc R . .
H5"3 H 0.2908 1.2732 0.0566 0.062 Uiso 1 1 calc R . .
C4" C 0.08703(19) 1.1663(4) 0.05378(14) 0.0426(6) Uani 1 1 d . . .
H4"1 H 0.1269 1.0504 0.0388 0.064 Uiso 1 1 calc R . .
H4"2 H 0.0565 1.2472 0.012 0.064 Uiso 1 1 calc R . .
H4"3 H 0.0307 1.1137 0.0775 0.064 Uiso 1 1 calc R . .
H1 H 0.2617(19) 0.999(4) 0.2660(13) 0.031(6) Uiso 1 1 d . . .
 
 
 
#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#
 
_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 C2 1.811(2) . ?
S1 C6 1.814(2) . ?
S3 C4 1.818(2) . ?
S3 C2 1.830(2) . ?
O1 C1" 1.207(2) . ?
O2 C1" 1.348(2) . ?
O2 C2" 1.480(2) . ?
N1 C1" 1.366(3) . ?
N1 C2' 1.419(3) . ?
N1 H1 0.81(2) . ?
C2 C1' 1.509(3) . ?
C2 H2 1 . ?
C6 C5 1.521(3) . ?
C6 H6A 0.99 . ?
C6 H6B 0.99 . ?
C5 C4 1.524(3) . ?
C5 H5A 0.99 . ?
C5 H5B 0.99 . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
C1' C6' 1.396(3) . ?
C1' C2' 1.402(3) . ?
C2' C3' 1.396(3) . ?
C3' C4' 1.384(3) . ?
C3' H3' 0.95 . ?
C4' C5' 1.381(3) . ?
C4' H4' 0.95 . ?
C5' C6' 1.385(3) . ?
C5' H5' 0.95 . ?
C6' H6' 0.95 . ?
C2" C5" 1.518(3) . ?
C2" C3" 1.520(3) . ?
C2" C4" 1.522(3) . ?
C3" H3"1 0.98 . ?
C3" H3"2 0.98 . ?
C3" H3"3 0.98 . ?
C5" H5"1 0.98 . ?
C5" H5"2 0.98 . ?
C5" H5"3 0.98 . ?
C4" H4"1 0.98 . ?
C4" H4"2 0.98 . ?
C4" H4"3 0.98 . ?
 
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 S1 C6 97.95(9) . . ?
C4 S3 C2 100.00(10) . . ?
C1" O2 C2" 120.32(16) . . ?
C1" N1 C2' 124.97(18) . . ?
C1" N1 H1 116.7(17) . . ?
C2' N1 H1 118.3(17) . . ?
O1 C1" O2 126.7(2) . . ?
O1 C1" N1 125.1(2) . . ?
O2 C1" N1 108.21(18) . . ?
C1' C2 S1 112.20(14) . . ?
C1' C2 S3 107.94(13) . . ?
S1 C2 S3 111.96(11) . . ?
C1' C2 H2 108.2 . . ?
S1 C2 H2 108.2 . . ?
S3 C2 H2 108.2 . . ?
C5 C6 S1 114.42(14) . . ?
C5 C6 H6A 108.7 . . ?
S1 C6 H6A 108.7 . . ?
C5 C6 H6B 108.7 . . ?
S1 C6 H6B 108.7 . . ?
H6A C6 H6B 107.6 . . ?
C6 C5 C4 113.54(18) . . ?
C6 C5 H5A 108.9 . . ?
C4 C5 H5A 108.9 . . ?
C6 C5 H5B 108.9 . . ?
C4 C5 H5B 108.9 . . ?
H5A C5 H5B 107.7 . . ?
C5 C4 S3 113.86(14) . . ?
C5 C4 H4A 108.8 . . ?
S3 C4 H4A 108.8 . . ?
C5 C4 H4B 108.8 . . ?
S3 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
C6' C1' C2' 118.47(18) . . ?
C6' C1' C2 121.66(18) . . ?
C2' C1' C2 119.87(17) . . ?
C3' C2' C1' 120.18(19) . . ?
C3' C2' N1 120.63(19) . . ?
C1' C2' N1 119.19(17) . . ?
C4' C3' C2' 119.8(2) . . ?
C4' C3' H3' 120.1 . . ?
C2' C3' H3' 120.1 . . ?
C5' C4' C3' 120.9(2) . . ?
C5' C4' H4' 119.6 . . ?
C3' C4' H4' 119.6 . . ?
C4' C5' C6' 119.3(2) . . ?
C4' C5' H5' 120.3 . . ?
C6' C5' H5' 120.3 . . ?
C5' C6' C1' 121.4(2) . . ?
C5' C6' H6' 119.3 . . ?
C1' C6' H6' 119.3 . . ?
O2 C2" C5" 110.51(18) . . ?
O2 C2" C3" 101.67(17) . . ?
C5" C2" C3" 111.1(2) . . ?
O2 C2" C4" 109.63(18) . . ?
C5" C2" C4" 112.6(2) . . ?
C3" C2" C4" 110.71(19) . . ?
C2" C3" H3"1 109.5 . . ?
C2" C3" H3"2 109.5 . . ?
H3"1 C3" H3"2 109.5 . . ?
C2" C3" H3"3 109.5 . . ?
H3"1 C3" H3"3 109.5 . . ?
H3"2 C3" H3"3 109.5 . . ?
C2" C5" H5"1 109.5 . . ?
C2" C5" H5"2 109.5 . . ?
H5"1 C5" H5"2 109.5 . . ?
C2" C5" H5"3 109.5 . . ?
H5"1 C5" H5"3 109.5 . . ?
H5"2 C5" H5"3 109.5 . . ?
C2" C4" H4"1 109.5 . . ?
C2" C4" H4"2 109.5 . . ?
H4"1 C4" H4"2 109.5 . . ?
C2" C4" H4"3 109.5 . . ?
H4"1 C4" H4"3 109.5 . . ?
H4"2 C4" H4"3 109.5 . . ?
 
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
C2" O2 C1" O1 2.1(3) . . . . ?
C2" O2 C1" N1 -177.63(17) . . . . ?
C2' N1 C1" O1 -3.6(3) . . . . ?
C2' N1 C1" O2 176.08(17) . . . . ?
C6 S1 C2 C1' -175.92(15) . . . . ?
C6 S1 C2 S3 62.54(12) . . . . ?
C4 S3 C2 C1' 174.50(14) . . . . ?
C4 S3 C2 S1 -61.54(12) . . . . ?
C2 S1 C6 C5 -62.20(17) . . . . ?
S1 C6 C5 C4 66.4(2) . . . . ?
C6 C5 C4 S3 -63.2(2) . . . . ?
C2 S3 C4 C5 57.61(17) . . . . ?
S1 C2 C1' C6' -20.8(2) . . . . ?
S3 C2 C1' C6' 103.02(19) . . . . ?
S1 C2 C1' C2' 158.72(15) . . . . ?
S3 C2 C1' C2' -77.5(2) . . . . ?
C6' C1' C2' C3' -0.5(3) . . . . ?
C2 C1' C2' C3' -179.99(18) . . . . ?
C6' C1' C2' N1 179.39(18) . . . . ?
C2 C1' C2' N1 -0.1(3) . . . . ?
C1" N1 C2' C3' 36.3(3) . . . . ?
C1" N1 C2' C1' -143.6(2) . . . . ?
C1' C2' C3' C4' 1.3(3) . . . . ?
N1 C2' C3' C4' -178.57(19) . . . . ?
C2' C3' C4' C5' -0.7(3) . . . . ?
C3' C4' C5' C6' -0.6(3) . . . . ?
C4' C5' C6' C1' 1.5(3) . . . . ?
C2' C1' C6' C5' -0.9(3) . . . . ?
C2 C1' C6' C5' 178.59(19) . . . . ?
C1" O2 C2" C5" -61.8(2) . . . . ?
C1" O2 C2" C3" -179.87(18) . . . . ?
C1" O2 C2" C4" 62.9(2) . . . . ?
 
