 
#  CIF produced by WinGX routine CIF_UPDATE
#  Created on 2003-01-08 at 12:25:19
#  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  : ljf077 dreduc struct
 
 
data_ljf077
 
_audit_creation_date            2003-01-08T12:25:19-00:00
_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                'C7 H13 S2, C7 H7 O3 S'
_chemical_formula_sum                   'C14 H20 O3 S3'
_chemical_formula_weight                332.48
_chemical_compound_source               'synthesis as described'
 
#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#
 
_symmetry_cell_setting                  triclinic
_symmetry_space_group_name_H-M          'P -1'
_symmetry_space_group_name_Hall         '-P 1'
_symmetry_Int_Tables_number             2
loop_
    _symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
 
_cell_length_a                          9.1968(2)
_cell_length_b                          9.2085(2)
_cell_length_c                          10.0820(2)
_cell_angle_alpha                       108.8810(10)
_cell_angle_beta                        109.7780(10)
_cell_angle_gamma                       90.1870(10)
_cell_volume                            754.11(3)
_cell_formula_units_Z                   2
_cell_measurement_temperature           150(2)
_cell_measurement_reflns_used           3886
_cell_measurement_theta_min             2
_cell_measurement_theta_max             30.034
_cell_measurement_wavelength            0.71073
 
#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#
 
_exptl_crystal_description              prism
_exptl_crystal_colour                   colourless
_exptl_crystal_size_max                 0.6
_exptl_crystal_size_mid                 0.45
_exptl_crystal_size_min                 0.25
_exptl_crystal_density_diffrn           1.464
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    352
_exptl_special_details
;
 ?
;
 
#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#
 
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_coefficient_mu      0.495
_exptl_absorpt_correction_T_min    0.767
_exptl_absorpt_correction_T_max    0.835
 
#----------------------------------------------------------------------------#
#                   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             0.935294E-1
_diffrn_orient_matrix_ub_12             0.86244E-2
_diffrn_orient_matrix_ub_13             -0.276437E-1
_diffrn_orient_matrix_ub_21             0.689271E-1
_diffrn_orient_matrix_ub_22             -0.10155E-2
_diffrn_orient_matrix_ub_23             0.100496
_diffrn_orient_matrix_ub_31             -0.84103E-2
_diffrn_orient_matrix_ub_32             -0.115376
_diffrn_orient_matrix_ub_33             -0.418126E-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         0.0111
_diffrn_reflns_av_unetI/netI            0.0236
_diffrn_reflns_number                   7144
_diffrn_reflns_limit_h_min              -12
_diffrn_reflns_limit_h_max              10
_diffrn_reflns_limit_k_min              -12
_diffrn_reflns_limit_k_max              12
_diffrn_reflns_limit_l_min              -14
_diffrn_reflns_limit_l_max              14
_diffrn_reflns_theta_min                2.29
_diffrn_reflns_theta_max                30.04
_diffrn_reflns_theta_full               30.04
_diffrn_measured_fraction_theta_full
                                        0.992
_diffrn_measured_fraction_theta_max
                                        0.992
_reflns_number_total                    4364
_reflns_number_gt                       4217
_reflns_threshold_expression            >2sigma(I)
 
#----------------------------------------------------------------------------#
#                   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_solution           'SHELXS-97 (Sheldrick, 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)+(0.0413P)²+0.6492P] 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                4364
_refine_ls_number_parameters            182
_refine_ls_number_restraints            0
_refine_ls_R_factor_all                 0.0361
_refine_ls_R_factor_gt                  0.0351
_refine_ls_wR_factor_ref                0.0968
_refine_ls_wR_factor_gt                 0.0961
_refine_ls_goodness_of_fit_ref          1.069
_refine_ls_restrained_S_all             1.069
_refine_ls_shift/su_max                 0.001
_refine_ls_shift/su_mean                0
_refine_diff_density_max                1.157
_refine_diff_density_min                -0.459
_refine_diff_density_rms                0.064
 
#----------------------------------------------------------------------------#
#                   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'
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 0.31266(16) 0.77020(15) -0.24183(15) 0.0171(2) Uani 1 1 d . . .
H1 H 0.3852 0.7603 -0.2956 0.02 Uiso 1 1 calc R . .
C3 C 0.2699(2) 0.75582(19) 0.01728(18) 0.0256(3) Uani 1 1 d . . .
H3A H 0.1687 0.6969 -0.047 0.031 Uiso 1 1 calc R . .
H3B H 0.3068 0.7259 0.1057 0.031 Uiso 1 1 calc R . .
C4 C 0.2535(2) 0.92806(19) 0.06443(17) 0.0261(3) Uani 1 1 d . . .
H4A H 0.1967 0.9515 0.1327 0.031 Uiso 1 1 calc R . .
H4B H 0.3563 0.9869 0.118 0.031 Uiso 1 1 calc R . .
C5 C 0.16916(18) 0.97831(17) -0.06857(17) 0.0220(3) Uani 1 1 d . . .
H5A H 0.1462 1.0834 -0.0316 0.026 Uiso 1 1 calc R . .
H5B H 0.0709 0.9121 -0.128 0.026 Uiso 1 1 calc R . .
C7 C 0.17097(17) 0.64676(18) -0.34519(17) 0.0226(3) Uani 1 1 d . . .
H7A H 0.088 0.6598 -0.3048 0.027 Uiso 1 1 calc R . .
H7B H 0.1315 0.6532 -0.4451 0.027 Uiso 1 1 calc R . .
C8 C 0.23330(19) 0.49215(19) -0.34903(19) 0.0280(3) Uani 1 1 d . . .
H8A H 0.2903 0.4654 -0.4171 0.034 Uiso 1 1 calc R . .
H8B H 0.1472 0.4112 -0.3852 0.034 Uiso 1 1 calc R . .
C9 C 0.34129(19) 0.50476(18) -0.19056(19) 0.0253(3) Uani 1 1 d . . .
H9A H 0.4304 0.4501 -0.1953 0.03 Uiso 1 1 calc R . .
H9B H 0.286 0.4598 -0.1437 0.03 Uiso 1 1 calc R . .
C013 C 0.35017(19) 0.84680(17) 0.46467(17) 0.0226(3) Uani 1 1 d . . .
H013 H 0.4358 0.9119 0.5417 0.027 Uiso 1 1 calc R . .
C101 C 0.23414(15) 0.59256(15) 0.28826(15) 0.0155(2) Uani 1 1 d . . .
C102 C 0.36198(16) 0.68971(16) 0.40410(15) 0.0182(2) Uani 1 1 d . . .
H102 H 0.4544 0.6505 0.4408 0.022 Uiso 1 1 calc R . .
C104 C 0.2129(2) 0.90790(17) 0.41206(18) 0.0242(3) Uani 1 1 d . . .
C105 C 0.08479(19) 0.80710(18) 0.29789(18) 0.0246(3) Uani 1 1 d . . .
H105 H -0.0088 0.8454 0.2635 0.029 Uiso 1 1 calc R . .
C106 C 0.09469(16) 0.65122(17) 0.23513(16) 0.0200(3) Uani 1 1 d . . .
H106 H 0.009 0.5861 0.1581 0.024 Uiso 1 1 calc R . .
C107 C 0.2023(3) 1.07899(19) 0.4729(2) 0.0359(4) Uani 1 1 d . . .
H10A H 0.2784 1.1234 0.5724 0.054 Uiso 1 1 calc R . .
H10B H 0.1 1.0938 0.4759 0.054 Uiso 1 1 calc R . .
H10C H 0.2217 1.1284 0.409 0.054 Uiso 1 1 calc R . .
O1 O 0.24972(15) 0.38791(15) 0.05120(13) 0.0302(3) Uani 1 1 d . . .
O2 O 0.11045(15) 0.30773(14) 0.18640(18) 0.0376(3) Uani 1 1 d . . .
O3 O 0.39347(14) 0.36126(14) 0.28995(14) 0.0292(3) Uani 1 1 d . . .
S1 S 0.24781(4) 0.39530(4) 0.19787(4) 0.01653(9) Uani 1 1 d . . .
S2 S 0.40516(4) 0.71004(4) -0.08251(4) 0.02042(9) Uani 1 1 d . . .
S6 S 0.28057(5) 0.97024(4) -0.18751(4) 0.02383(10) 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 C7 1.543(2) . ?
C1 S6 1.8001(14) . ?
C1 S2 1.8069(14) . ?
C1 H1 0.98 . ?
C3 C4 1.525(2) . ?
C3 S2 1.8203(16) . ?
C3 H3A 0.97 . ?
C3 H3B 0.97 . ?
C4 C5 1.521(2) . ?
C4 H4A 0.97 . ?
C4 H4B 0.97 . ?
C5 S6 1.8076(15) . ?
C5 H5A 0.97 . ?
C5 H5B 0.97 . ?
C7 C8 1.530(2) . ?
C7 H7A 0.97 . ?
C7 H7B 0.97 . ?
C8 C9 1.535(2) . ?
C8 H8A 0.97 . ?
C8 H8B 0.97 . ?
C9 S2 1.8254(16) . ?
C9 H9A 0.97 . ?
C9 H9B 0.97 . ?
C013 C104 1.392(2) . ?
C013 C102 1.397(2) . ?
C013 H013 0.93 . ?
C101 C102 1.3908(19) . ?
C101 C106 1.3966(18) . ?
C101 S1 1.7758(13) . ?
C102 H102 0.93 . ?
C104 C105 1.399(2) . ?
C104 C107 1.511(2) . ?
C105 C106 1.386(2) . ?
C105 H105 0.93 . ?
C106 H106 0.93 . ?
C107 H10A 0.96 . ?
C107 H10B 0.96 . ?
C107 H10C 0.96 . ?
O1 S1 1.4642(12) . ?
O2 S1 1.4470(12) . ?
O3 S1 1.4505(11) . ?
 
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 C1 S6 118.22(10) . . ?
C7 C1 S2 105.38(9) . . ?
S6 C1 S2 112.68(7) . . ?
C7 C1 H1 106.6 . . ?
S6 C1 H1 106.6 . . ?
S2 C1 H1 106.6 . . ?
C4 C3 S2 111.36(11) . . ?
C4 C3 H3A 109.4 . . ?
S2 C3 H3A 109.4 . . ?
C4 C3 H3B 109.4 . . ?
S2 C3 H3B 109.4 . . ?
H3A C3 H3B 108 . . ?
C5 C4 C3 112.59(13) . . ?
C5 C4 H4A 109.1 . . ?
C3 C4 H4A 109.1 . . ?
C5 C4 H4B 109.1 . . ?
C3 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
C4 C5 S6 113.00(11) . . ?
C4 C5 H5A 109 . . ?
S6 C5 H5A 109 . . ?
C4 C5 H5B 109 . . ?
S6 C5 H5B 109 . . ?
H5A C5 H5B 107.8 . . ?
C8 C7 C1 104.68(12) . . ?
C8 C7 H7A 110.8 . . ?
C1 C7 H7A 110.8 . . ?
C8 C7 H7B 110.8 . . ?
C1 C7 H7B 110.8 . . ?
H7A C7 H7B 108.9 . . ?
C7 C8 C9 109.57(13) . . ?
C7 C8 H8A 109.8 . . ?
C9 C8 H8A 109.8 . . ?
C7 C8 H8B 109.8 . . ?
C9 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?
C8 C9 S2 107.33(10) . . ?
C8 C9 H9A 110.2 . . ?
S2 C9 H9A 110.2 . . ?
C8 C9 H9B 110.2 . . ?
S2 C9 H9B 110.2 . . ?
H9A C9 H9B 108.5 . . ?
C104 C013 C102 121.36(14) . . ?
C104 C013 H013 119.3 . . ?
C102 C013 H013 119.3 . . ?
C102 C101 C106 120.22(13) . . ?
C102 C101 S1 120.99(10) . . ?
C106 C101 S1 118.69(10) . . ?
C101 C102 C013 119.30(13) . . ?
C101 C102 H102 120.3 . . ?
C013 C102 H102 120.3 . . ?
C013 C104 C105 118.23(13) . . ?
C013 C104 C107 121.35(16) . . ?
C105 C104 C107 120.40(15) . . ?
C106 C105 C104 121.27(14) . . ?
C106 C105 H105 119.4 . . ?
C104 C105 H105 119.4 . . ?
C105 C106 C101 119.59(13) . . ?
C105 C106 H106 120.2 . . ?
C101 C106 H106 120.2 . . ?
C104 C107 H10A 109.5 . . ?
C104 C107 H10B 109.5 . . ?
H10A C107 H10B 109.5 . . ?
C104 C107 H10C 109.5 . . ?
H10A C107 H10C 109.5 . . ?
H10B C107 H10C 109.5 . . ?
O2 S1 O3 114.33(8) . . ?
O2 S1 O1 112.66(9) . . ?
O3 S1 O1 111.91(8) . . ?
O2 S1 C101 106.12(7) . . ?
O3 S1 C101 106.39(7) . . ?
O1 S1 C101 104.54(7) . . ?
C1 S2 C3 101.73(7) . . ?
C1 S2 C9 93.86(7) . . ?
C3 S2 C9 101.52(8) . . ?
C1 S6 C5 102.14(6) . . ?
 
