 
#  CIF produced by WinGX routine CIF_UPDATE
#  Created on 2000-08-27 at 18:28:37
#  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  : ljf016a dreduc struct
 
 
data_ljf016a
 
_audit_creation_date            2000-08-27T18:28:37-00:00
_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                'C25 H29 Br O S2 Si'
_chemical_formula_structural            'C25 H29 Br O S2 Si'
_chemical_formula_sum                   'C25 H29 Br O S2 Si'
_chemical_formula_weight                517.6
_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                          8.93860(10)
_cell_length_b                          31.8060(4)
_cell_length_c                          9.24000(10)
_cell_angle_alpha                       90
_cell_angle_beta                        97.3480(10)
_cell_angle_gamma                       90
_cell_volume                            2605.37(5)
_cell_formula_units_Z                   4
_cell_measurement_temperature           291(2)
_cell_measurement_reflns_used           30412
_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                 0.43
_exptl_crystal_size_mid                 0.33
_exptl_crystal_size_min                 0.32
_exptl_crystal_density_diffrn           1.32
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    1072
_exptl_special_details
;
 ?
;
 
#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#
 
_exptl_absorpt_coefficient_mu           1.798
_exptl_absorpt_correction_type          multi-scan
_exptl_absorpt_process_details          'Blessing (1995)'
_exptl_absorpt_correction_T_min         0.667
_exptl_absorpt_correction_T_max         0.69
 
#----------------------------------------------------------------------------#
#                   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'
_diffrn_orient_matrix_ub_11             0.712692E-1
_diffrn_orient_matrix_ub_12             -0.222715E-1
_diffrn_orient_matrix_ub_13             0.845516E-1
_diffrn_orient_matrix_ub_21             -0.215787E-1
_diffrn_orient_matrix_ub_22             0.96499E-2
_diffrn_orient_matrix_ub_23             0.207307E-1
_diffrn_orient_matrix_ub_31             -0.301691E-1
_diffrn_orient_matrix_ub_32             -0.103516
_diffrn_orient_matrix_ub_33             0.167824E-1
_diffrn_measurement_device              '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type         KappaCCD
_diffrn_measurement_method              CCD
_diffrn_reflns_number                   14325
_diffrn_reflns_av_R_equivalents         0.0309
_diffrn_reflns_av_unetI/netI            0.0431
_diffrn_reflns_limit_h_min              -11
_diffrn_reflns_limit_h_max              11
_diffrn_reflns_limit_k_min              -38
_diffrn_reflns_limit_k_max              41
_diffrn_reflns_limit_l_min              -11
_diffrn_reflns_limit_l_max              11
_diffrn_reflns_theta_min                3.44
_diffrn_reflns_theta_max                27.51
_diffrn_reflns_theta_full               27.51
_diffrn_measured_fraction_theta_full
                                        0.955
_diffrn_measured_fraction_theta_max
                                        0.955
_reflns_number_total                    5719
_reflns_number_gt                       4079
_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)+(0.0350P)²+1.4659P] 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                5719
_refine_ls_number_parameters            276
_refine_ls_number_restraints            0
_refine_ls_R_factor_all                 0.074
_refine_ls_R_factor_gt                  0.0467
_refine_ls_wR_factor_ref                0.1084
_refine_ls_wR_factor_gt                 0.0976
_refine_ls_goodness_of_fit_ref          1.041
_refine_ls_restrained_S_all             1.041
_refine_ls_shift/su_max                 0
_refine_ls_shift/su_mean                0
_refine_diff_density_max                0.5
_refine_diff_density_min                -0.564
_refine_diff_density_rms                0.045
 
#----------------------------------------------------------------------------#
#                   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'
Si Si 0.0817 0.0704 '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'
Br Br -0.2901 2.4595 '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
C2 C 0.2422(3) 0.24926(10) 0.7191(4) 0.0715(8) Uani 1 1 d . . .
H2A H 0.1613 0.2594 0.7688 0.107 Uiso 1 1 calc R . .
H2B H 0.2375 0.2626 0.6255 0.107 Uiso 1 1 calc R . .
H2C H 0.337 0.2556 0.776 0.107 Uiso 1 1 calc R . .
C3 C 0.0659(3) 0.17788(10) 0.5537(3) 0.0665(8) Uani 1 1 d . . .
H3A H -0.0268 0.1881 0.5827 0.1 Uiso 1 1 calc R . .
H3B H 0.0605 0.1479 0.5428 0.1 Uiso 1 1 calc R . .
H3C H 0.0818 0.1905 0.4625 0.1 Uiso 1 1 calc R . .
C4 C 0.2122(3) 0.16523(10) 0.8746(3) 0.0557(7) Uani 1 1 d . . .
C5 C 0.5793(3) 0.10659(8) 0.6007(3) 0.0511(6) Uani 1 1 d . . .
H5 H 0.5083 0.1086 0.673 0.061 Uiso 1 1 calc R . .
C41 C 0.0701(4) 0.18068(13) 0.9367(4) 0.0863(11) Uani 1 1 d . . .
H41A H 0.0754 0.2106 0.9496 0.129 Uiso 1 1 calc R . .
H41B H 0.0641 0.1674 1.029 0.129 Uiso 1 1 calc R . .
H41C H -0.0177 0.1737 0.8701 0.129 Uiso 1 1 calc R . .
C42 C 0.2031(4) 0.11773(11) 0.8559(3) 0.0748(9) Uani 1 1 d . . .
H42A H 0.1171 0.1107 0.7869 0.112 Uiso 1 1 calc R . .
H42B H 0.1931 0.1048 0.9481 0.112 Uiso 1 1 calc R . .
H42C H 0.2931 0.1077 0.8209 0.112 Uiso 1 1 calc R . .
C43 C 0.3516(4) 0.17690(14) 0.9819(4) 0.0919(11) Uani 1 1 d . . .
H43A H 0.3525 0.2067 0.9989 0.138 Uiso 1 1 calc R . .
H43B H 0.4412 0.169 0.9413 0.138 Uiso 1 1 calc R . .
H43C H 0.3483 0.1623 1.0724 0.138 Uiso 1 1 calc R . .
C111 C 0.6389(3) 0.18634(9) 0.3104(3) 0.0533(7) Uani 1 1 d . . .
C112 C 0.5311(3) 0.21560(9) 0.3272(3) 0.0573(7) Uani 1 1 d . . .
H112 H 0.5186 0.2388 0.2658 0.069 Uiso 1 1 calc R . .
C113 C 0.4409(3) 0.21040(9) 0.4362(3) 0.0584(7) Uani 1 1 d . . .
H113 H 0.3666 0.2302 0.4474 0.07 Uiso 1 1 calc R . .
C114 C 0.4593(3) 0.17601(9) 0.5294(3) 0.0480(6) Uani 1 1 d . . .
C115 C 0.5646(2) 0.14527(8) 0.5080(3) 0.0447(5) Uani 1 1 d . . .
C116 C 0.6547(3) 0.15109(9) 0.3971(3) 0.0547(7) Uani 1 1 d . . .
H116 H 0.7262 0.1309 0.3816 0.066 Uiso 1 1 calc R . .
C121 C 0.7428(3) 0.06989(11) 0.8442(3) 0.0629(8) Uani 1 1 d . . .
C122 C 0.6808(5) 0.08488(16) 0.9600(4) 0.1039(14) Uani 1 1 d . . .
H122 H 0.6502 0.1128 0.962 0.125 Uiso 1 1 calc R . .
C123 C 0.6635(7) 0.0584(3) 1.0752(5) 0.150(3) Uani 1 1 d . . .
H123 H 0.6203 0.0685 1.1548 0.18 Uiso 1 1 calc R . .
C124 C 0.7084(10) 0.0186(3) 1.0723(7) 0.175(3) Uani 1 1 d . . .
H124 H 0.6953 0.0008 1.1495 0.209 Uiso 1 1 calc R . .
C125 C 0.7715(11) 0.0041(2) 0.9609(7) 0.198(4) Uani 1 1 d . . .
H125 H 0.805 -0.0236 0.9614 0.238 Uiso 1 1 calc R . .
C126 C 0.7879(7) 0.02945(16) 0.8446(5) 0.1322(19) Uani 1 1 d . . .
H126 H 0.8302 0.0188 0.7654 0.159 Uiso 1 1 calc R . .
C131 C 0.3431(3) 0.06282(9) 0.4472(3) 0.0579(7) Uani 1 1 d . . .
C132 C 0.2844(4) 0.08272(13) 0.3205(4) 0.0815(10) Uani 1 1 d . . .
H132 H 0.3485 0.0945 0.2598 0.098 Uiso 1 1 calc R . .
C133 C 0.1298(5) 0.08526(16) 0.2834(5) 0.1048(13) Uani 1 1 d . . .
H133 H 0.0901 0.0986 0.1975 0.126 Uiso 1 1 calc R . .
C134 C 0.0354(5) 0.06829(15) 0.3720(6) 0.1011(14) Uani 1 1 d . . .
H134 H -0.0685 0.0697 0.3459 0.121 Uiso 1 1 calc R . .
C135 C 0.0930(5) 0.04925(14) 0.4990(5) 0.0962(13) Uani 1 1 d . . .
H135 H 0.0284 0.0384 0.5609 0.115 Uiso 1 1 calc R . .
C136 C 0.2465(4) 0.04606(11) 0.5357(4) 0.0752(9) Uani 1 1 d . . .
H136 H 0.2851 0.0324 0.6214 0.09 Uiso 1 1 calc R . .
O1 O 0.3813(2) 0.17116(7) 0.6452(2) 0.0632(5) Uani 1 1 d . . .
Si1 Si 0.22412(7) 0.19166(2) 0.69450(8) 0.04752(18) Uani 1 1 d . . .
S1 S 0.76946(8) 0.10327(3) 0.69631(10) 0.0787(3) Uani 1 1 d . . .
S2 S 0.54104(9) 0.05794(2) 0.49587(9) 0.0683(2) Uani 1 1 d . . .
Br1 Br 0.76637(4) 0.193415(13) 0.16294(4) 0.07960(14) 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
C2 Si1 1.850(3) . ?
C3 Si1 1.848(3) . ?
C4 C42 1.521(5) . ?
C4 C43 1.535(4) . ?
C4 C41 1.539(4) . ?
C4 Si1 1.880(3) . ?
C5 C115 1.495(4) . ?
C5 S1 1.815(2) . ?
C5 S2 1.834(3) . ?
C111 C112 1.362(4) . ?
C111 C116 1.375(4) . ?
C111 Br1 1.898(2) . ?
C112 C113 1.378(4) . ?
C113 C114 1.389(4) . ?
C114 O1 1.358(3) . ?
C114 C115 1.389(3) . ?
C115 C116 1.394(3) . ?
C121 C126 1.348(5) . ?
C121 C122 1.353(5) . ?
C121 S1 1.770(3) . ?
C122 C123 1.381(8) . ?
C123 C124 1.331(9) . ?
C124 C125 1.318(9) . ?
C125 C126 1.367(7) . ?
C131 C136 1.371(4) . ?
C131 C132 1.375(4) . ?
C131 S2 1.776(3) . ?
C132 C133 1.383(5) . ?
C133 C134 1.360(6) . ?
C134 C135 1.361(6) . ?
C135 C136 1.374(5) . ?
O1 Si1 1.6646(18) . ?
 
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
C42 C4 C43 109.9(3) . . ?
C42 C4 C41 108.9(3) . . ?
C43 C4 C41 108.8(3) . . ?
C42 C4 Si1 110.59(19) . . ?
C43 C4 Si1 109.3(2) . . ?
C41 C4 Si1 109.3(2) . . ?
C115 C5 S1 109.56(17) . . ?
C115 C5 S2 113.23(18) . . ?
S1 C5 S2 107.93(14) . . ?
C112 C111 C116 120.8(2) . . ?
C112 C111 Br1 119.9(2) . . ?
C116 C111 Br1 119.3(2) . . ?
C111 C112 C113 119.3(3) . . ?
C112 C113 C114 120.9(3) . . ?
O1 C114 C115 117.2(2) . . ?
O1 C114 C113 123.1(2) . . ?
C115 C114 C113 119.7(2) . . ?
C114 C115 C116 118.5(2) . . ?
C114 C115 C5 120.6(2) . . ?
C116 C115 C5 120.9(2) . . ?
C111 C116 C115 120.7(2) . . ?
C126 C121 C122 119.1(4) . . ?
C126 C121 S1 120.3(3) . . ?
C122 C121 S1 120.5(3) . . ?
C121 C122 C123 119.5(5) . . ?
C124 C123 C122 120.0(5) . . ?
C125 C124 C123 120.6(6) . . ?
C124 C125 C126 120.5(6) . . ?
C121 C126 C125 120.2(5) . . ?
C136 C131 C132 119.1(3) . . ?
C136 C131 S2 119.9(2) . . ?
C132 C131 S2 121.0(2) . . ?
C131 C132 C133 119.9(4) . . ?
C134 C133 C132 120.3(4) . . ?
C133 C134 C135 120.0(4) . . ?
C134 C135 C136 120.1(4) . . ?
C131 C136 C135 120.6(4) . . ?
C114 O1 Si1 135.02(17) . . ?
O1 Si1 C3 108.13(13) . . ?
O1 Si1 C2 111.00(13) . . ?
C3 Si1 C2 111.61(15) . . ?
O1 Si1 C4 102.27(11) . . ?
C3 Si1 C4 113.09(14) . . ?
C2 Si1 C4 110.35(15) . . ?
C121 S1 C5 101.56(13) . . ?
C131 S2 C5 99.95(12) . . ?
 
