 
#  CIF produced by WinGX routine CIF_UPDATE
#  Created on 2000-09-03 at 23:40:10
#  Using CIFtbx version 2.6.2 16 Jun 1998
 
#  Dictionary name : cif_core.dic
#  Dictionary vers : 2.1beta3
#  Request file    : c:\wingx\files\archive.dat
#  CIF files read  : ljf011 dreduc struct sortav
 
 
data_ljf011
 
_audit_creation_date            2000-09-03T23:40:10-00:00
_audit_creation_method         'WinGX routine CIF_UPDATE'
_audit_conform_dict_name        cif_core.dic
_audit_conform_dict_version     2.1beta3
_audit_conform_dict_location    ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic
_publ_requested_category        FO
 
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#
 
_chemical_name_systematic
;
 ?
;
_chemical_formula_moiety                'C19 H15 Br O S2'
_chemical_formula_structural            'C19 H15 Br O S2'
_chemical_formula_sum                   'C19 H15 Br O S2'
_chemical_formula_weight                403.34
_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                          6.41200(10)
_cell_length_b                          17.7776(4)
_cell_length_c                          15.6695(3)
_cell_angle_alpha                       90
_cell_angle_beta                        101.8430(10)
_cell_angle_gamma                       90
_cell_volume                            1748.14(6)
_cell_formula_units_Z                   4
_cell_measurement_temperature           291(2)
_cell_measurement_reflns_used           16192
_cell_measurement_theta_min             3.395
_cell_measurement_theta_max             30.999
_cell_measurement_wavelength            0.71073
 
#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#
 
_exptl_crystal_description              prism
_exptl_crystal_colour                   colourless
_exptl_crystal_size_max                 0.5
_exptl_crystal_size_mid                 0.15
_exptl_crystal_size_min                 0.1
_exptl_crystal_density_diffrn           1.533
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    816
_exptl_special_details
;
 ?
;
 
#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#
 
_exptl_absorpt_coefficient_mu           2.591
_exptl_absorpt_correction_type          multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_correction_T_min         0.515
_exptl_absorpt_correction_T_max         0.621
 
#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#
 
_diffrn_source                          'Enraf Nonius FR590'
_diffrn_ambient_temperature             291(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
        Matrix refers to original P21/c cell
;
_diffrn_orient_matrix_ub_11             0.155451E-1
_diffrn_orient_matrix_ub_12             0.129339
_diffrn_orient_matrix_ub_13             -0.917021E-1
_diffrn_orient_matrix_ub_21             0.281755E-1
_diffrn_orient_matrix_ub_22             0.25859E-1
_diffrn_orient_matrix_ub_23             0.412485E-1
_diffrn_orient_matrix_ub_31             0.561936E-1
_diffrn_orient_matrix_ub_32             -0.121706E-1
_diffrn_orient_matrix_ub_33             -0.307542E-1
_diffrn_measurement_device              '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type         KappaCCD
_diffrn_measurement_method              CCD
_diffrn_reflns_number                   9206
_diffrn_reflns_av_R_equivalents         0.031
_diffrn_reflns_av_unetI/netI            0.048
_diffrn_reflns_limit_h_min              -9
_diffrn_reflns_limit_h_max              9
_diffrn_reflns_limit_k_min              -25
_diffrn_reflns_limit_k_max              25
_diffrn_reflns_limit_l_min              -8
_diffrn_reflns_limit_l_max              21
_diffrn_reflns_theta_min                4.35
_diffrn_reflns_theta_max                30.96
_diffrn_reflns_theta_full               27
_diffrn_measured_fraction_theta_full
                                        0.977
_diffrn_measured_fraction_theta_max
                                        0.905
_reflns_number_total                    5035
_reflns_number_gt                       3564
_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)+(0.0478P)²+0.8697P] 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                5035
_refine_ls_number_parameters            209
_refine_ls_number_restraints            0
_refine_ls_R_factor_all                 0.0705
_refine_ls_R_factor_gt                  0.0419
_refine_ls_wR_factor_ref                0.1098
_refine_ls_wR_factor_gt                 0.0973
_refine_ls_goodness_of_fit_ref          1.018
_refine_ls_restrained_S_all             1.018
_refine_ls_shift/su_max                 0.001
_refine_ls_shift/su_mean                0
_refine_diff_density_max                0.589
_refine_diff_density_min                -0.794
_refine_diff_density_rms                0.069
 
#----------------------------------------------------------------------------#
#                   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'
Br Br -0.2901 2.4595 '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
C1 C 0.4652(4) 0.19071(12) 0.29590(14) 0.0320(4) Uani 1 1 d . . .
H1 H 0.339 0.177 0.2519 0.038 Uiso 1 1 calc R . .
C101 C 0.4522(4) 0.31319(13) 0.49384(14) 0.0365(5) Uani 1 1 d . . .
C102 C 0.5175(4) 0.28395(13) 0.42173(15) 0.0340(5) Uani 1 1 d . . .
H102 H 0.6427 0.301 0.407 0.041 Uiso 1 1 calc R . .
C103 C 0.3959(3) 0.22925(12) 0.37141(14) 0.0314(4) Uani 1 1 d . . .
C104 C 0.2090(3) 0.20384(14) 0.39533(16) 0.0365(5) Uani 1 1 d . . .
C105 C 0.1445(4) 0.23467(15) 0.46740(17) 0.0427(6) Uani 1 1 d . . .
H105 H 0.0189 0.2182 0.4823 0.051 Uiso 1 1 calc R . .
C106 C 0.2654(4) 0.28939(15) 0.51686(16) 0.0425(5) Uani 1 1 d . . .
H106 H 0.2222 0.31 0.565 0.051 Uiso 1 1 calc R . .
C111 C 0.4921(4) 0.31509(14) 0.18403(15) 0.0385(5) Uani 1 1 d . . .
C112 C 0.2759(5) 0.31012(16) 0.14928(19) 0.0520(7) Uani 1 1 d . . .
H112 H 0.1984 0.2689 0.1622 0.062 Uiso 1 1 calc R . .
C113 C 0.1749(6) 0.36682(19) 0.0950(2) 0.0613(8) Uani 1 1 d . . .
H113 H 0.0298 0.3631 0.0715 0.074 Uiso 1 1 calc R . .
C114 C 0.2857(6) 0.42770(18) 0.0759(2) 0.0647(9) Uani 1 1 d . . .
H114 H 0.2168 0.4652 0.0393 0.078 Uiso 1 1 calc R . .
C115 C 0.4993(7) 0.43346(18) 0.1109(2) 0.0682(9) Uani 1 1 d . . .
H115 H 0.5755 0.4749 0.0977 0.082 Uiso 1 1 calc R . .
C116 C 0.6022(5) 0.37791(17) 0.1658(2) 0.0559(7) Uani 1 1 d . . .
H116 H 0.7463 0.3829 0.1905 0.067 Uiso 1 1 calc R . .
C211 C 0.5702(4) 0.04484(12) 0.24807(15) 0.0339(4) Uani 1 1 d . . .
C212 C 0.3927(4) -0.00170(15) 0.23051(18) 0.0457(6) Uani 1 1 d . . .
H212 H 0.2907 0.0004 0.2649 0.055 Uiso 1 1 calc R . .
C213 C 0.3696(6) -0.05145(18) 0.1608(2) 0.0616(8) Uani 1 1 d . . .
H213 H 0.2512 -0.0829 0.1487 0.074 Uiso 1 1 calc R . .
C214 C 0.5183(6) -0.05479(18) 0.1098(2) 0.0634(8) Uani 1 1 d . . .
H214 H 0.5014 -0.0885 0.0635 0.076 Uiso 1 1 calc R . .
C215 C 0.6926(6) -0.00839(18) 0.1270(2) 0.0598(8) Uani 1 1 d . . .
H215 H 0.7927 -0.0103 0.0917 0.072 Uiso 1 1 calc R . .
C216 C 0.7207(4) 0.04120(16) 0.19644(18) 0.0466(6) Uani 1 1 d . . .
H216 H 0.8404 0.072 0.2084 0.056 Uiso 1 1 calc R . .
Br1 Br 0.62551(5) 0.386866(16) 0.562376(18) 0.05453(11) Uani 1 1 d . . .
O1 O 0.1011(3) 0.14779(12) 0.34589(14) 0.0516(5) Uani 1 1 d . . .
H1A H -0.0158 0.1422 0.3586 0.077 Uiso 1 1 calc R . .
S1 S 0.64839(10) 0.24287(4) 0.24427(4) 0.04040(15) Uani 1 1 d . . .
S2 S 0.60506(9) 0.10473(3) 0.34085(4) 0.03410(13) 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 C103 1.511(3) . ?
C1 S1 1.812(2) . ?
C1 S2 1.838(2) . ?
C101 C102 1.384(3) . ?
C101 C106 1.386(4) . ?
C101 Br1 1.901(2) . ?
C102 C103 1.387(3) . ?
C103 C104 1.402(3) . ?
C104 O1 1.361(3) . ?
C104 C105 1.392(3) . ?
C105 C106 1.379(4) . ?
C111 C116 1.382(4) . ?
C111 C112 1.385(4) . ?
C111 S1 1.776(3) . ?
C112 C113 1.390(4) . ?
C113 C114 1.361(5) . ?
C114 C115 1.371(5) . ?
C115 C116 1.384(5) . ?
C211 C216 1.382(3) . ?
C211 C212 1.388(3) . ?
C211 S2 1.779(2) . ?
C212 C213 1.390(4) . ?
C213 C214 1.365(5) . ?
C214 C215 1.371(5) . ?
C215 C216 1.384(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
C103 C1 S1 116.07(16) . . ?
C103 C1 S2 106.00(15) . . ?
S1 C1 S2 106.67(11) . . ?
C102 C101 C106 121.3(2) . . ?
C102 C101 Br1 118.71(18) . . ?
C106 C101 Br1 119.97(18) . . ?
C101 C102 C103 119.9(2) . . ?
C102 C103 C104 119.0(2) . . ?
C102 C103 C1 122.8(2) . . ?
C104 C103 C1 117.9(2) . . ?
O1 C104 C105 123.3(2) . . ?
O1 C104 C103 116.5(2) . . ?
C105 C104 C103 120.2(2) . . ?
C106 C105 C104 120.5(2) . . ?
C105 C106 C101 119.0(2) . . ?
C116 C111 C112 118.9(3) . . ?
C116 C111 S1 116.0(2) . . ?
C112 C111 S1 125.0(2) . . ?
C111 C112 C113 119.8(3) . . ?
C114 C113 C112 120.8(3) . . ?
C113 C114 C115 119.7(3) . . ?
C114 C115 C116 120.3(3) . . ?
C111 C116 C115 120.4(3) . . ?
C216 C211 C212 119.9(2) . . ?
C216 C211 S2 121.37(18) . . ?
C212 C211 S2 118.65(19) . . ?
C211 C212 C213 119.1(3) . . ?
C214 C213 C212 120.9(3) . . ?
C213 C214 C215 119.9(3) . . ?
C214 C215 C216 120.5(3) . . ?
C211 C216 C215 119.8(3) . . ?
C111 S1 C1 105.10(11) . . ?
C211 S2 C1 102.42(10) . . ?
 
