#\#CIF_1.1
 
#  CIF produced by WinGX routine CIF_UPDATE
#  Created on 2004-01-21 at 14:05:42
#  Using CIFtbx version 2.6.2 16 Jun 1998
 
#  Dictionary name : cif_core.dic
#  Dictionary vers : 2.3
#  Request file    : c:\wingx\files\archive.dat
#  CIF files read  : ljf106a sortabs sortav struct
 
 
data_ljf106a
 
_audit_creation_date            2004-01-21T14:05:42-00:00
_audit_creation_method         'WinGX routine CIF_UPDATE'
_audit_conform_dict_name        cif_core.dic
_audit_conform_dict_version     2.3
_audit_conform_dict_location    ftp://ftp.iucr.org/pub/cif_core.dic
_publ_requested_category        FO
 
#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#
 
_chemical_name_systematic
;
 ?
;
_chemical_formula_moiety                'C17 H21 N O3 S'
_chemical_formula_sum                   'C17 H21 N O3 S'
_chemical_formula_weight                319.41
_chemical_compound_source               'synthesis as described'
_chemical_absolute_configuration        ad
 
#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#
 
_space_group_crystal_system             triclinic
_space_group_name_H-M_alt               'P 1'
_space_group_name_Hall                  'P 1'
_space_group_IT_number                  1
loop_
    _space_group_symop_operation_xyz
'x, y, z'
 
_cell_length_a                          6.1954(2)
_cell_length_b                          7.5986(4)
_cell_length_c                          9.8236(5)
_cell_angle_alpha                       102.559(2)
_cell_angle_beta                        101.707(2)
_cell_angle_gamma                       109.160(2)
_cell_volume                            407.09(3)
_cell_formula_units_Z                   1
_cell_measurement_temperature           100(2)
_cell_measurement_reflns_used           7940
_cell_measurement_theta_max             29.99
_cell_measurement_theta_min             2.2
_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                 0.4
_exptl_crystal_size_min                 0.2
_exptl_crystal_density_diffrn           1.303
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    170
_exptl_special_details
;
 ?
;
 
#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#
 
_exptl_absorpt_coefficient_mu           0.211
_exptl_absorpt_correction_type          multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_absorpt_correction_T_min         0.88
_exptl_absorpt_correction_T_max         0.969
 
#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#
 
_diffrn_ambient_temperature             100(2)
_diffrn_radiation_wavelength            0.71073
_diffrn_radiation_type                  MoK\a
_diffrn_radiation_monochromator         graphite
_diffrn_radiation_probe                 x-ray
_diffrn_reflns_av_R_equivalents         0.0333
_diffrn_reflns_av_unetI/netI            0.0353
_diffrn_reflns_number                   8945
_diffrn_reflns_limit_h_min              -8
_diffrn_reflns_limit_h_max              8
_diffrn_reflns_limit_k_min              -10
_diffrn_reflns_limit_k_max              10
_diffrn_reflns_limit_l_min              -13
_diffrn_reflns_limit_l_max              13
_diffrn_reflns_theta_min                2.22
_diffrn_reflns_theta_max                30.07
_diffrn_reflns_theta_full               30.07
_diffrn_measured_fraction_theta_full
                                        0.979
_diffrn_measured_fraction_theta_max
                                        0.979
_reflns_number_total                    4110
_reflns_number_gt                       3975
_reflns_threshold_expression            >2sigma(I)
_diffrn_reflns_reduction_process
;
 Data were integrated using Eval-14. Crystal was twinned about (0 0 1)
 Twin Matrix :  -1 0 0 0 -1 0 0.975 0.823 1
 About 15% of secondary lattice from SHELXL refinement

 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               'Eval-14 (Duisenberg et al, 2003)'
_computing_structure_solution           'SIR92 (Cascarano et al, 1993)'
_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.

 Twin refinement using hkl5.hkl prepared by the TwinRotMat option in Platon.
 This brings the residuals from R1=0.071 to 0.042 and e-density from 1.8 to
 0.6. The non-merohedral twinning has the apparent effect of doubling the c
 axis in some zones, which led to an initial incorrect cell. Reciprocal
 lattice points in the planes perpendicular to c* are in perfect registry.
;
_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)+(0.0724P)²+0.2876P] 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                4110
_refine_ls_number_parameters            203
_refine_ls_number_restraints            3
_refine_ls_R_factor_all                 0.045
_refine_ls_R_factor_gt                  0.0419
_refine_ls_wR_factor_ref                0.1271
_refine_ls_wR_factor_gt                 0.1231
_refine_ls_goodness_of_fit_ref          1.101
_refine_ls_restrained_S_all             1.101
_refine_ls_shift/su_max                 0.001
_refine_ls_shift/su_mean                0
_refine_ls_abs_structure_details
                                    'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack          0.07(8)
_refine_diff_density_max                0.564
_refine_diff_density_min                -0.441
_refine_diff_density_rms                0.073
 
#----------------------------------------------------------------------------#
#                   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
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
 
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 0.89433(7) 0.08989(6) -0.09569(5) 0.01200(13) Uani 1 1 d . . .
O1 O 1.1335(3) 0.0933(3) -0.0735(2) 0.0192(4) Uani 1 1 d . . .
O2 O 0.8214(4) 0.2079(3) -0.1782(2) 0.0177(4) Uani 1 1 d . . .
O3 O 0.6467(4) -0.4989(3) -0.1736(3) 0.0300(5) Uani 1 1 d . . .
H3 H 0.6745 -0.6012 -0.1839 0.045 Uiso 1 1 calc R . .
N1 N 0.7166(4) -0.1349(3) -0.1793(2) 0.0116(4) Uani 1 1 d . . .
H1A H 0.7487 -0.2059 -0.1204 0.014 Uiso 1 1 d R . .
C1 C 0.4537(5) -0.1932(4) -0.2244(3) 0.0128(4) Uani 1 1 d . . .
H1 H 0.4191 -0.0841 -0.1687 0.015 Uiso 1 1 calc R . .
C2 C 0.3312(5) -0.3781(4) -0.1811(3) 0.0163(5) Uani 1 1 d . . .
H2 H 0.1547 -0.422 -0.2251 0.02 Uiso 1 1 calc R . .
C3 C 0.3986(5) -0.5491(4) -0.2421(3) 0.0188(5) Uani 1 1 d . . .
H3A H 0.3004 -0.6678 -0.2228 0.023 Uiso 1 1 calc R . .
H3B H 0.3675 -0.5773 -0.3491 0.023 Uiso 1 1 calc R . .
C4 C 0.3793(6) -0.3299(5) -0.0150(3) 0.0260(7) Uani 1 1 d . . .
H4A H 0.2945 -0.4477 0.0085 0.039 Uiso 1 1 calc R . .
H4B H 0.3227 -0.2274 0.0202 0.039 Uiso 1 1 calc R . .
H4C H 0.5516 -0.2838 0.0325 0.039 Uiso 1 1 calc R . .
C11 C 0.8496(5) 0.1580(4) 0.0768(3) 0.0141(5) Uani 1 1 d . . .
C12 C 0.9738(5) 0.1175(4) 0.1935(3) 0.0176(5) Uani 1 1 d . . .
H12 H 1.0904 0.0641 0.1827 0.021 Uiso 1 1 calc R . .
C13 C 0.9233(6) 0.1571(4) 0.3263(3) 0.0211(6) Uani 1 1 d . . .
H13 H 1.0099 0.1334 0.4071 0.025 Uiso 1 1 calc R . .
C14 C 0.7481(5) 0.2307(4) 0.3430(3) 0.0197(5) Uani 1 1 d . . .
C15 C 0.6289(5) 0.2711(4) 0.2247(3) 0.0188(5) Uani 1 1 d . . .
H15 H 0.5108 0.3229 0.235 0.023 Uiso 1 1 calc R . .
C16 C 0.6787(5) 0.2373(4) 0.0921(3) 0.0158(5) Uani 1 1 d . . .
H16 H 0.5979 0.2677 0.0131 0.019 Uiso 1 1 calc R . .
C17 C 0.6885(7) 0.2655(5) 0.4853(3) 0.0296(7) Uani 1 1 d . . .
H17A H 0.7833 0.223 0.5538 0.044 Uiso 1 1 calc R . .
H17B H 0.5178 0.1907 0.4678 0.044 Uiso 1 1 calc R . .
H17C H 0.7257 0.4053 0.5268 0.044 Uiso 1 1 calc R . .
C21 C 0.3539(4) -0.2227(3) -0.3857(3) 0.0126(4) Uani 1 1 d . . .
C22 C 0.4663(5) -0.2767(4) -0.4881(3) 0.0179(5) Uani 1 1 d . . .
H22 H 0.6136 -0.2905 -0.4564 0.022 Uiso 1 1 calc R . .
C23 C 0.3635(5) -0.3107(4) -0.6369(3) 0.0196(6) Uani 1 1 d . . .
H23 H 0.4408 -0.348 -0.7056 0.024 Uiso 1 1 calc R . .
C24 C 0.1491(5) -0.2900(4) -0.6844(3) 0.0194(5) Uani 1 1 d . . .
H24 H 0.0801 -0.312 -0.7853 0.023 Uiso 1 1 calc R . .
C25 C 0.0362(5) -0.2373(4) -0.5838(3) 0.0195(5) Uani 1 1 d . . .
H25 H -0.1123 -0.2256 -0.6161 0.023 Uiso 1 1 calc R . .
C26 C 0.1404(5) -0.2010(4) -0.4347(3) 0.0173(5) Uani 1 1 d . . .
H26 H 0.064 -0.161 -0.3663 0.021 Uiso 1 1 calc R . .
 
 
 
#----------------------------------------------------------------------------#
#                   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 O1 1.444(2) . ?
S1 O2 1.4489(19) . ?
S1 N1 1.610(2) . ?
S1 C11 1.766(3) . ?
O3 C3 1.430(4) . ?
O3 H3 0.84 . ?
N1 C1 1.481(3) . ?
N1 H1A 0.9077 . ?
C1 C21 1.517(3) . ?
C1 C2 1.556(4) . ?
C1 H1 1 . ?
C2 C3 1.531(4) . ?
C2 C4 1.535(4) . ?
C2 H2 1 . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
C4 H4A 0.98 . ?
C4 H4B 0.98 . ?
C4 H4C 0.98 . ?
C11 C16 1.397(4) . ?
C11 C12 1.397(3) . ?
C12 C13 1.396(4) . ?
C12 H12 0.95 . ?
C13 C14 1.396(4) . ?
C13 H13 0.95 . ?
C14 C15 1.395(4) . ?
C14 C17 1.507(4) . ?
C15 C16 1.388(4) . ?
C15 H15 0.95 . ?
C16 H16 0.95 . ?
C17 H17A 0.98 . ?
C17 H17B 0.98 . ?
C17 H17C 0.98 . ?
C21 C26 1.389(4) . ?
C21 C22 1.399(3) . ?
C22 C23 1.399(4) . ?
C22 H22 0.95 . ?
C23 C24 1.387(4) . ?
C23 H23 0.95 . ?
C24 C25 1.385(4) . ?
C24 H24 0.95 . ?
C25 C26 1.400(4) . ?
C25 H25 0.95 . ?
C26 H26 0.95 . ?
 
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
O1 S1 O2 119.45(12) . . ?
O1 S1 N1 105.82(11) . . ?
O2 S1 N1 107.32(11) . . ?
O1 S1 C11 108.50(12) . . ?
O2 S1 C11 107.19(12) . . ?
N1 S1 C11 108.11(11) . . ?
C3 O3 H3 109.5 . . ?
C1 N1 S1 120.97(16) . . ?
C1 N1 H1A 106.8 . . ?
S1 N1 H1A 106.9 . . ?
N1 C1 C21 112.1(2) . . ?
N1 C1 C2 110.0(2) . . ?
C21 C1 C2 112.0(2) . . ?
N1 C1 H1 107.5 . . ?
C21 C1 H1 107.5 . . ?
C2 C1 H1 107.5 . . ?
C3 C2 C4 111.1(2) . . ?
C3 C2 C1 113.0(2) . . ?
C4 C2 C1 111.4(2) . . ?
C3 C2 H2 107 . . ?
C4 C2 H2 107 . . ?
C1 C2 H2 107 . . ?
O3 C3 C2 109.1(2) . . ?
O3 C3 H3A 109.9 . . ?
C2 C3 H3A 109.9 . . ?
O3 C3 H3B 109.9 . . ?
C2 C3 H3B 109.9 . . ?
H3A C3 H3B 108.3 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C16 C11 C12 121.0(2) . . ?
C16 C11 S1 119.9(2) . . ?
C12 C11 S1 119.0(2) . . ?
C13 C12 C11 118.7(3) . . ?
C13 C12 H12 120.7 . . ?
C11 C12 H12 120.7 . . ?
C12 C13 C14 121.4(3) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
C15 C14 C13 118.4(3) . . ?
C15 C14 C17 120.7(3) . . ?
C13 C14 C17 120.9(3) . . ?
C16 C15 C14 121.6(3) . . ?
C16 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
C15 C16 C11 118.9(3) . . ?
C15 C16 H16 120.5 . . ?
C11 C16 H16 120.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C26 C21 C22 118.6(2) . . ?
C26 C21 C1 119.2(2) . . ?
C22 C21 C1 122.2(2) . . ?
C21 C22 C23 120.6(3) . . ?
C21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C24 C23 C22 120.2(3) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C25 C24 C23 119.6(3) . . ?
C25 C24 H24 120.2 . . ?
C23 C24 H24 120.2 . . ?
C24 C25 C26 120.2(3) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C21 C26 C25 120.8(2) . . ?
C21 C26 H26 119.6 . . ?
C25 C26 H26 119.6 . . ?
 
