 
#  CIF produced by WinGX routine CIF_UPDATE
#  Created on 2000-11-05 at 12:41:35
#  Using CIFtbx version 2.6.2 16 Jun 1998
 
#  Dictionary name : cif_core.dic
#  Dictionary vers : 2.1
#  Request file    : c:\wingx\files\archive.dat
#  CIF files read  : ljf027 dreduc sortav gaussian struct
 
 
data_ljf027
 
_audit_creation_date            2000-11-05T12:41:35-00:00
_audit_creation_method         'WinGX routine CIF_UPDATE'
_audit_conform_dict_name        cif_core.dic
_audit_conform_dict_version     2.1
_audit_conform_dict_location    ftp://ftp.iucr.org/pub/cif_core.dic
_publ_requested_category        FO
 
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#
 
_chemical_name_systematic
;
 ?
;
_chemical_formula_moiety                'C20 H22 N2 O S4'
_chemical_formula_structural            'C20 H22 N2 O S4'
_chemical_formula_sum                   'C20 H22 N2 O S4'
_chemical_formula_weight                434.64
_chemical_compound_source               'synthesis as described'
 
#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#
 
_symmetry_cell_setting                  monoclinic
_symmetry_space_group_name_H-M          'P 21/n'
_symmetry_space_group_name_Hall         '-P 2yn'
_symmetry_Int_Tables_number             14
loop_
    _symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
 
_cell_length_a                          10.2666(2)
_cell_length_b                          19.2594(5)
_cell_length_c                          10.7649(2)
_cell_angle_alpha                       90
_cell_angle_beta                        102.115(1)
_cell_angle_gamma                       90
_cell_volume                            2081.12(8)
_cell_formula_units_Z                   4
_cell_measurement_temperature           293(2)
_cell_measurement_reflns_used           10059
_cell_measurement_theta_min             3.395
_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                 0.31
_exptl_crystal_size_mid                 0.16
_exptl_crystal_size_min                 0.1
_exptl_crystal_density_diffrn           1.387
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    912
loop_
    _exptl_crystal_face_index_h
    _exptl_crystal_face_index_k
    _exptl_crystal_face_index_l
    _exptl_crystal_face_perp_dist
1 1 0 0.09
-1 -1 0 0.07
0 0 1 0.05
0 0 -1 0.05
-1 1 1 0.19
1 -1 -1 0.12
 
_exptl_special_details
;
 UB matrix and faces refer to cell used for data collection 
 10.267 10.765 19.259 90 90 77.89
;
 
#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#
 
_exptl_absorpt_coefficient_mu           0.47
_exptl_absorpt_correction_type          gaussian
_exptl_absorpt_process_details
;
   P. Coppens, L. Leiserowitz, D Rabinovich, Acta Cryst.
   (1965), 18, 1035-1038
;
_exptl_absorpt_correction_T_min         0.894
_exptl_absorpt_correction_T_max         0.963
 
#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#
 
_diffrn_source                          'Enraf Nonius FR590'
_diffrn_ambient_temperature             293(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             0.881576E-1
_diffrn_orient_matrix_ub_12             0.463338E-1
_diffrn_orient_matrix_ub_13             -0.24344E-2
_diffrn_orient_matrix_ub_21             -0.194118E-1
_diffrn_orient_matrix_ub_22             -0.107918E-1
_diffrn_orient_matrix_ub_23             -0.92378E-1
_diffrn_orient_matrix_ub_31             -0.241577E-1
_diffrn_orient_matrix_ub_32             0.459597E-1
_diffrn_orient_matrix_ub_33             -0.2869E-3
_diffrn_measurement_device              '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type         KappaCCD
_diffrn_measurement_method              'CCD rotation images, thick slices'
_diffrn_reflns_number                   11736
_diffrn_reflns_av_R_equivalents         0.0401
_diffrn_reflns_av_unetI/netI            0.0481
_diffrn_reflns_limit_h_min              -13
_diffrn_reflns_limit_h_max              13
_diffrn_reflns_limit_k_min              -25
_diffrn_reflns_limit_k_max              16
_diffrn_reflns_limit_l_min              -13
_diffrn_reflns_limit_l_max              13
_diffrn_reflns_theta_min                3.72
_diffrn_reflns_theta_max                27.5
_diffrn_reflns_theta_full               27.5
_diffrn_measured_fraction_theta_full
                                        0.993
_diffrn_measured_fraction_theta_max
                                        0.993
_reflns_number_total                    4752
_reflns_number_gt                       3268
_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)+(0.0421P)²+0.4252P] 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                4752
_refine_ls_number_parameters            244
_refine_ls_number_restraints            0
_refine_ls_R_factor_all                 0.071
_refine_ls_R_factor_gt                  0.0408
_refine_ls_wR_factor_ref                0.1031
_refine_ls_wR_factor_gt                 0.0922
_refine_ls_goodness_of_fit_ref          1.028
_refine_ls_restrained_S_all             1.028
_refine_ls_shift/su_max                 0.001
_refine_ls_shift/su_mean                0
_refine_diff_density_max                0.342
_refine_diff_density_min                -0.349
_refine_diff_density_rms                0.044
 
#----------------------------------------------------------------------------#
#                   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'
S S 0.1246 0.1234 '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'
 
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 0.56939(18) 0.22787(10) 0.76254(18) 0.0409(4) Uani 1 1 d ' ' ' ' ' '
H1 H 0.5177 0.271 0.7512 0.049 Uiso 1 1 calc R ' ' ' '
C2 C 0.6317(2) 0.25528(13) 0.5317(2) 0.0565(6) Uani 1 1 d ' ' ' ' ' '
H2A H 0.5785 0.2971 0.5291 0.068 Uiso 1 1 calc R ' ' ' '
H2B H 0.6985 0.2637 0.4818 0.068 Uiso 1 1 calc R ' ' ' '
C3 C 0.5429(2) 0.19686(13) 0.4717(2) 0.0594(6) Uani 1 1 d ' ' ' ' ' '
H3A H 0.5946 0.1543 0.4795 0.071 Uiso 1 1 calc R ' ' ' '
H3B H 0.5125 0.2065 0.3818 0.071 Uiso 1 1 calc R ' ' ' '
C4 C 0.4225(2) 0.18574(13) 0.5305(2) 0.0577(6) Uani 1 1 d ' ' ' ' ' '
H4A H 0.3646 0.1517 0.4802 0.069 Uiso 1 1 calc R ' ' ' '
H4B H 0.3734 0.229 0.5262 0.069 Uiso 1 1 calc R ' ' ' '
C5 C 0.68104(17) 0.44606(10) 0.75057(18) 0.0403(4) Uani 1 1 d ' ' ' ' ' '
H5 H 0.6993 0.3977 0.7766 0.048 Uiso 1 1 calc R ' ' ' '
C6 C 0.8326(2) 0.42500(14) 0.5697(2) 0.0694(7) Uani 1 1 d ' ' ' ' ' '
H6A H 0.8447 0.3774 0.5991 0.083 Uiso 1 1 calc R ' ' ' '
H6B H 0.8395 0.4257 0.4812 0.083 Uiso 1 1 calc R ' ' ' '
C8 C 0.9436(2) 0.46875(13) 0.6455(3) 0.0653(7) Uani 1 1 d ' ' ' ' ' '
H8A H 1.0276 0.4535 0.627 0.078 Uiso 1 1 calc R ' ' ' '
H8B H 0.93 0.5167 0.6182 0.078 Uiso 1 1 calc R ' ' ' '
C9 C 0.9529(2) 0.46531(14) 0.7856(2) 0.0647(7) Uani 1 1 d ' ' ' ' ' '
H9A H 1.0324 0.49 0.8276 0.078 Uiso 1 1 calc R ' ' ' '
H9B H 0.9633 0.4171 0.812 0.078 Uiso 1 1 calc R ' ' ' '
C111 C 0.58116(19) 0.25654(10) 0.99526(18) 0.0411(4) Uani 1 1 d ' ' ' ' ' '
C112 C 0.61492(18) 0.21401(10) 0.90303(18) 0.0406(4) Uani 1 1 d ' ' ' ' ' '
C113 C 0.6913(2) 0.15555(11) 0.9442(2) 0.0497(5) Uani 1 1 d ' ' ' ' ' '
H113 H 0.7152 0.1258 0.8846 0.06 Uiso 1 1 calc R ' ' ' '
C114 C 0.7322(2) 0.14088(12) 1.0716(2) 0.0599(6) Uani 1 1 d ' ' ' ' ' '
H114 H 0.785 0.1021 1.0972 0.072 Uiso 1 1 calc R ' ' ' '
C115 C 0.6955(2) 0.18321(13) 1.1611(2) 0.0622(6) Uani 1 1 d ' ' ' ' ' '
H115 H 0.7228 0.1729 1.247 0.075 Uiso 1 1 calc R ' ' ' '
C116 C 0.6180(2) 0.24102(12) 1.1234(2) 0.0547(6) Uani 1 1 d ' ' ' ' ' '
H116 H 0.5909 0.2692 1.1833 0.066 Uiso 1 1 calc R ' ' ' '
C211 C 0.48790(17) 0.42808(9) 0.86323(17) 0.0362(4) Uani 1 1 d ' ' ' ' ' '
C212 C 0.55242(17) 0.46890(10) 0.78508(18) 0.0381(4) Uani 1 1 d ' ' ' ' ' '
C213 C 0.4981(2) 0.53264(11) 0.7429(2) 0.0500(5) Uani 1 1 d ' ' ' ' ' '
H213 H 0.5401 0.5599 0.6916 0.06 Uiso 1 1 calc R ' ' ' '
C214 C 0.3832(2) 0.55651(12) 0.7752(2) 0.0570(6) Uani 1 1 d ' ' ' ' ' '
H214 H 0.3474 0.5991 0.7447 0.068 Uiso 1 1 calc R ' ' ' '
C215 C 0.32160(19) 0.51736(12) 0.8523(2) 0.0541(6) Uani 1 1 d ' ' ' ' ' '
H215 H 0.2447 0.534 0.8748 0.065 Uiso 1 1 calc R ' ' ' '
C216 C 0.37209(18) 0.45338(11) 0.8971(2) 0.0459(5) Uani 1 1 d ' ' ' ' ' '
H216 H 0.3294 0.4273 0.9494 0.055 Uiso 1 1 calc R ' ' ' '
N1 N 0.50126(15) 0.31916(9) 0.96002(15) 0.0428(4) Uani 1 1 d ' ' ' ' ' '
N2 N 0.55490(15) 0.36563(8) 0.90432(15) 0.0400(4) Uani 1 1 d ' ' ' ' ' '
S1 S 0.71459(5) 0.23893(3) 0.69408(5) 0.05408(17) Uani 1 1 d ' ' ' ' ' '
S2 S 0.46165(5) 0.15679(3) 0.69355(5) 0.05196(16) Uani 1 1 d ' ' ' ' ' '
S3 S 0.66667(6) 0.45319(3) 0.58013(5) 0.05874(18) Uani 1 1 d ' ' ' ' ' '
S4 S 0.81150(5) 0.50115(3) 0.83897(6) 0.05826(18) Uani 1 1 d ' ' ' ' ' '
O10 O 0.39077(17) 0.32037(10) 0.9900(2) 0.0897(6) Uani 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
C1 C112 1.510(3) ' ' ?
C1 S1 1.8088(19) ' ' ?
C1 S2 1.8178(19) ' ' ?
C2 C3 1.506(3) ' ' ?
C2 S1 1.804(2) ' ' ?
C3 C4 1.518(3) ' ' ?
C4 S2 1.804(2) ' ' ?
C5 C212 1.510(3) ' ' ?
C5 S4 1.8139(19) ' ' ?
C5 S3 1.815(2) ' ' ?
C6 C8 1.512(3) ' ' ?
C6 S3 1.814(2) ' ' ?
C8 C9 1.493(3) ' ' ?
C9 S4 1.807(2) ' ' ?
C111 C116 1.384(3) ' ' ?
C111 C112 1.386(3) ' ' ?
C111 N1 1.463(3) ' ' ?
C112 C113 1.390(3) ' ' ?
C113 C114 1.377(3) ' ' ?
C114 C115 1.374(3) ' ' ?
C115 C116 1.379(3) ' ' ?
C211 C216 1.402(3) ' ' ?
C211 N2 1.410(2) ' ' ?
C211 C212 1.414(3) ' ' ?
C212 C213 1.385(3) ' ' ?
C213 C214 1.377(3) ' ' ?
C214 C215 1.370(3) ' ' ?
C215 C216 1.384(3) ' ' ?
N1 O10 1.243(2) ' ' ?
N1 N2 1.266(2) ' ' ?
 
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
C112 C1 S1 108.69(13) ' ' ' ' ?
C112 C1 S2 108.05(13) ' ' ' ' ?
S1 C1 S2 113.89(10) ' ' ' ' ?
C3 C2 S1 113.93(17) ' ' ' ' ?
C2 C3 C4 113.50(18) ' ' ' ' ?
C3 C4 S2 114.49(14) ' ' ' ' ?
C212 C5 S4 106.74(13) ' ' ' ' ?
C212 C5 S3 109.69(13) ' ' ' ' ?
S4 C5 S3 112.37(10) ' ' ' ' ?
C8 C6 S3 114.29(17) ' ' ' ' ?
C9 C8 C6 113.70(19) ' ' ' ' ?
C8 C9 S4 114.78(16) ' ' ' ' ?
C116 C111 C112 121.94(19) ' ' ' ' ?
C116 C111 N1 117.23(19) ' ' ' ' ?
C112 C111 N1 120.82(17) ' ' ' ' ?
C111 C112 C113 117.34(18) ' ' ' ' ?
C111 C112 C1 122.78(17) ' ' ' ' ?
C113 C112 C1 119.86(18) ' ' ' ' ?
C114 C113 C112 121.2(2) ' ' ' ' ?
C115 C114 C113 120.4(2) ' ' ' ' ?
C114 C115 C116 119.9(2) ' ' ' ' ?
C115 C116 C111 119.2(2) ' ' ' ' ?
C216 C211 N2 126.84(18) ' ' ' ' ?
C216 C211 C212 119.34(18) ' ' ' ' ?
N2 C211 C212 113.73(15) ' ' ' ' ?
C213 C212 C211 118.79(18) ' ' ' ' ?
C213 C212 C5 119.35(18) ' ' ' ' ?
C211 C212 C5 121.83(16) ' ' ' ' ?
C214 C213 C212 121.4(2) ' ' ' ' ?
C215 C214 C213 119.9(2) ' ' ' ' ?
C214 C215 C216 120.98(19) ' ' ' ' ?
C215 C216 C211 119.7(2) ' ' ' ' ?
O10 N1 N2 128.40(18) ' ' ' ' ?
O10 N1 C111 116.14(16) ' ' ' ' ?
N2 N1 C111 115.45(15) ' ' ' ' ?
N1 N2 C211 121.31(15) ' ' ' ' ?
C2 S1 C1 98.83(10) ' ' ' ' ?
C4 S2 C1 99.03(10) ' ' ' ' ?
C6 S3 C5 99.32(10) ' ' ' ' ?
C9 S4 C5 99.44(11) ' ' ' ' ?
 
