##############################################################################
###                                                                        ###
###           Full Paper (Acta Crystallographica Section C)                ###
###                                                                        ###
##############################################################################
#                                                                            #
# This CIF contains the data in a paper accepted for publication in Acta     #
# Crystallographica Section C. It conforms to the editorial and technical    #
# requirements of Notes for Authors for Section C, and has been peer         #
# reviewed under the auspices of the IUCr Commission on Journals.            #
#                                                                            #
# Full details of the Crystallographic Information File format               #
# are given in the paper "The Crystallographic Information File (CIF):       #
# a New Standard Archive File for Crystallography" by S. R. Hall, F. H.      #
# Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685].                  #
#                                                                            #
# The current version of the core CIF dictionary is obtainable from          #
# ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.1.    #
#                                                                            #
# Software is freely available for graphical display of the structure(s) in  #
# this CIF.  For information consult the CIF home page http://www.iucr.org/  #
# cif/home.html                                                              #
#                                                                            #
#            Copyright International Union of Crystallography                #
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data_global
_audit_creation_method     'form.cif (version 2.0)'
_journal_data_validation_number     ?
_journal_date_recd_electronic     2001-02-22
_journal_date_accepted     2001-03-13
_journal_name_full     'Acta Crystallographica, Section C'
_journal_year     2001
_journal_volume     57
_journal_issue      7
_journal_page_first     787
_journal_page_last     789
_journal_paper_category     FM
_publ_contact_author_name     'Dr J. M. S. Skakle'
_publ_contact_author_address
;
Department of Chemistry
University of Aberdeen
Meston Walk
Aberdeen
AB24 3UE
Scotland
;
_publ_contact_author_email     j.skakle@abdn.ac.uk
_publ_contact_author_fax      0E*****
_publ_contact_author_phone      0E*****
_publ_section_title
;
(2-Thioxo-1,3-dithiole-4,5-dithiolato-S,S')diphenylplumbane at 295 K and
(2-thioxo-1,3-dithiole-4,5-dithiolato-S,S')diphenylstannane at 150 K
;
loop_
    _publ_author_name
    _publ_author_footnote
    _publ_author_address
    'Skakle, Janet M. S.' ?
;
Department of Chemistry
University of Aberdeen
Meston Walk
Aberdeen AB24 3UE
Scotland
;
    'Wardell, James L.'
;
also at: Instituto de Quimica
Departamento de Quimica Inorganica
Universidade Federal do Rio de Janeiro
21945-970 RJ
Brazil
;
;
Department of Chemistry
University of Aberdeen
Meston Walk
Aberdeen AB24 3UE
Scotland
;
    'Wardell, Solange M. S. V.' ?
;
Instituto de Quimica
Departamento de Quimica Organica
Universidade Federal Fluminense
24020-150 Niteroi
RJ
Brazil
;
data_III
_audit_creation_method     SHELXL97
_chemical_name_systematic
;
(2-thioxo-1,3-dithiole-4,5-dithiolato-S,S')diphenylplumbane
;
_chemical_name_common     ?
_chemical_formula_moiety     'C15 H10 Pb S5'
_chemical_formula_sum     'C15 H10 Pb S5'
_chemical_formula_iupac     '[Pb (C3 S5) (C6 H5)2]'
_chemical_formula_weight     557.73
_symmetry_cell_setting     orthorhombic
_symmetry_space_group_name_H-M     'Pna21'
_symmetry_space_group_name_Hall     'P 2c -2n'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, -y, z+1/2'
    'x+1/2, -y+1/2, z'
    '-x+1/2, y+1/2, z+1/2'
_cell_length_a     17.5109(9)
_cell_length_b     9.5222(5)
_cell_length_c     10.3232(5)
_cell_angle_alpha     90
_cell_angle_beta     90
_cell_angle_gamma     90
_cell_volume     1721.31(15)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     4683
_cell_measurement_theta_min     2.3
_cell_measurement_theta_max     30.1
_cell_measurement_temperature     295(2)
_exptl_crystal_description     plate
_exptl_crystal_colour     'dark red'
_exptl_crystal_size_max      .25
_exptl_crystal_size_mid      .18
_exptl_crystal_size_min      .02
_exptl_crystal_density_diffrn     2.152
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     1048
_exptl_absorpt_coefficient_mu     10.40
_exptl_absorpt_correction_type     'multi-scan'
_exptl_absorpt_process_details     '(SADABS; Bruker, 1999)'
_exptl_absorpt_correction_T_min      .181
_exptl_absorpt_correction_T_max      .819
_exptl_special_details
;
 ?
;
_diffrn_ambient_temperature     295(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength      .71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Bruker SMART CCD area-detector'
_diffrn_measurement_method     φ/ω
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     16869
_diffrn_reflns_av_R_equivalents      .10
_diffrn_reflns_av_sigmaI/netI      .081
_diffrn_reflns_theta_min     2.3
_diffrn_reflns_theta_max     32.5
_diffrn_reflns_theta_full     32.5
_diffrn_measured_fraction_theta_max     1.00
_diffrn_measured_fraction_theta_full     1.00
_diffrn_reflns_limit_h_min     -26
_diffrn_reflns_limit_h_max     26
_diffrn_reflns_limit_k_min     -14
_diffrn_reflns_limit_k_max     12
_diffrn_reflns_limit_l_min     -12
_diffrn_reflns_limit_l_max     15
_diffrn_standards_number     ?
_diffrn_standards_interval_count     ?
_diffrn_standards_interval_time     ?
_diffrn_standards_decay_%     negligible
_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.
;
_reflns_number_total     5088
_reflns_number_gt     3310
_reflns_threshold_expression     'I>2σ(I)'
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all      .106
_refine_ls_R_factor_gt      .055
_refine_ls_wR_factor_ref      .140
_refine_ls_goodness_of_fit_ref     1.01
_refine_ls_restrained_S_all     1.01
_refine_ls_number_reflns     5088
_refine_ls_number_parameters     190
_refine_ls_number_restraints     1
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
            'w = 1/[σ²(Fo²)+(0.0573P)²+8.9418P] where P=(Fo²+2Fc²)/3'
_refine_ls_shift/su_max     <0.001
_refine_ls_shift/su_mean      .000
_refine_diff_density_max     1.89
_refine_diff_density_min     -2.04
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
_refine_ls_abs_structure_details     '(Flack, 1983)'
_refine_ls_abs_structure_Flack      .015(14)
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'C' 'C'  .0033  .0016
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'H' 'H'  .0000  .0000
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Pb' 'Pb' -3.3944 10.1111
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'S' 'S'  .1246  .1234
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection     'SMART (Bruker, 1999)'
_computing_cell_refinement     'SAINT (Bruker, 1999)'
_computing_data_reduction     'SAINT'
_computing_structure_solution     'SHELXS86 (Sheldrick, 1990)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics
;
ORTEX in OSCAIL (McArdle, 1994, 2000) and ORTEP-3 for Windows (Farrugia, 1997)
;
_computing_publication_material     'CIFTAB (Sheldrick, 1997)'
loop_
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    Pb1  .08628(2)  .13212(3)  -.00325(8)  .03829(13) Uani d . 1 . . Pb
    S1  .1517(2)  .2027(4)  .2122(3)  .0436(7) Uani d . 1 . . S
    S2  .1990(2)  .2470(4)  -.1204(4)  .0467(8) Uani d . 1 . . S
    C1  .2274(7)  .2957(11)  .1439(12)  .032(2) Uani d . 1 . . C
    C2  .2460(7)  .3119(12)  .0162(17)  .038(3) Uani d . 1 . . C
    S3  .28893(19)  .3763(3)  .2535(3)  .0410(7) Uani d . 1 . . S
    S4  .32587(17)  .4180(3)  -.0129(5)  .0431(7) Uani d . 1 . . S
    C3  .3496(7)  .4526(13)  .1441(14)  .042(3) Uani d . 1 . . C
    S5  .4263(2)  .5511(5)  .1844(4)  .0575(10) Uani d . 1 . . S
    C4  .1033(6)  -.0949(10)  .009(2)  .033(3) Uani d . 1 . . C
    C5  .1673(9)  -.1433(14)  .0732(14)  .047(3) Uani d . 1 . . C
    H5  .1994  -.0808  .1160  .056 Uiso calc R 1 . . H
    C6  .1832(10)  -.2850(15)  .0733(16)  .057(4) Uani d . 1 . . C
    H6  .2267  -.3184  .1148  .068 Uiso calc R 1 . . H
    C7  .1343(12)  -.3775(13)  .012(3)  .073(6) Uani d . 1 . . C
    H7  .1465  -.4724  .0069  .087 Uiso calc R 1 . . H
    C8  .0685(9)  -.3300(13)  -.0422(15)  .053(4) Uani d . 1 . . C
    H8  .0337  -.3943  -.0753  .063 Uiso calc R 1 . . H
    C9  .0520(8)  -.1884(12)  -.0489(14)  .044(3) Uani d . 1 . . C
    H9  .0082  -.1564  -.0905  .053 Uiso calc R 1 . . H
    C10  -.0077(6)  .2859(10)  -.0212(14)  .033(3) Uani d . 1 . . C
    C11  -.0379(10)  .3305(17)  -.1341(19)  .045(4) Uani d . 1 . . C
    H11  -.0197  .2943  -.2119  .054 Uiso calc R 1 . . H
    C12  -.0940(9)  .427(2)  -.135(2)  .057(5) Uani d . 1 . . C
    H12  -.1150  .4542  -.2142  .069 Uiso calc R 1 . . H
    C13  -.1208(8)  .4854(15)  -.023(2)  .059(5) Uani d . 1 . . C
    H13  -.1591  .5530  -.0271  .070 Uiso calc R 1 . . H
    C14  -.0919(10)  .445(2)  .094(2)  .064(6) Uani d . 1 . . C
    H14  -.1097  .4852  .1706  .077 Uiso calc R 1 . . H
    C15  -.0335(11)  .3404(19)  .096(2)  .052(4) Uani d . 1 . . C
    H15  -.0131  .3092  .1740  .063 Uiso calc R 1 . . H
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    Pb1  .03712(19)  .02808(14)  .0497(2)  .00494(15)  -.0089(3)  -.0037(4)
    S1  .0466(18)  .0458(15)  .0383(18)  -.0138(14)  -.0006(14)  -.0028(13)
    S2  .049(2)  .058(2)  .0335(18)  -.0018(16)  .0024(15)  -.0090(15)
    C1  .034(6)  .033(5)  .030(6)  -.001(5)  .000(5)  -.003(4)
    C2  .032(5)  .045(5)  .038(9)  -.002(4)  .000(6)  -.012(6)
    S3  .0404(16)  .0501(16)  .0326(16)  -.0116(14)  -.0012(12)  -.0051(13)
    S4  .0383(13)  .0511(13)  .040(2)  -.0023(11)  .0042(18)  -.0010(19)
    C3  .037(7)  .041(6)  .049(8)  -.003(5)  .001(6)  -.002(5)
    S5  .050(2)  .067(2)  .056(2)  -.0265(18)  .0096(17)  -.0075(18)
    C4  .031(5)  .033(4)  .035(7)  .007(3)  .008(7)  -.001(6)
    C5  .051(8)  .048(7)  .042(8)  .008(6)  -.004(6)  .001(6)
    C6  .058(9)  .052(7)  .060(10)  .028(7)  -.010(7)  -.009(7)
    C7  .113(14)  .034(5)  .071(13)  .012(7)  .027(14)  .004(8)
    C8  .067(9)  .031(5)  .060(11)  -.007(6)  .013(7)  -.010(5)
    C9  .041(7)  .035(5)  .057(9)  -.003(5)  .006(6)  -.006(5)
    C10  .034(5)  .031(4)  .034(8)  .006(4)  -.001(5)  -.002(5)
    C11  .040(8)  .040(7)  .055(10)  .008(6)  -.001(7)  .003(6)
    C12  .048(10)  .052(9)  .072(14)  .003(7)  -.012(9)  -.005(8)
    C13  .043(7)  .053(7)  .079(15)  .017(6)  -.001(9)  -.001(9)
    C14  .066(12)  .059(11)  .068(14)  .028(9)  .015(9)  -.012(10)
    C15  .054(10)  .052(9)  .051(10)  .005(7)  .007(7)  -.002(7)
_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_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Pb1 C4 . 2.185(10) ?
    Pb1 C10 . 2.210(10) ?
    Pb1 S2 . 2.561(4) ?
    Pb1 S1 . 2.591(4) ?
    Pb1 S5 4_544 3.322(4) ?
    Pb1 S5 3_455 3.827(4) ?
    S1 C1 . 1.742(12) ?
    S2 C2 . 1.746(16) ?
    C1 C2 . 1.37(2) ?
    C1 S3 . 1.741(13) ?
    C2 S4 . 1.752(12) ?
    S3 C3 . 1.713(14) ?
    S4 C3 . 1.706(15) ?
    C3 S5 . 1.690(13) ?
    C4 C5 . 1.384(19) ?
    C4 C9 . 1.397(18) ?
    C5 C6 . 1.378(19) ?
    C5 H5 .  .9300 ?
    C6 C7 . 1.38(3) ?
    C6 H6 .  .9300 ?
    C7 C8 . 1.36(3) ?
    C7 H7 .  .9300 ?
    C8 C9 . 1.380(17) ?
    C8 H8 .  .9300 ?
    C9 H9 .  .9300 ?
    C10 C11 . 1.35(2) ?
    C10 C15 . 1.39(2) ?
    C11 C12 . 1.34(3) ?
    C11 H11 .  .9300 ?
    C12 C13 . 1.37(3) ?
    C12 H12 .  .9300 ?
    C13 C14 . 1.37(3) ?
    C13 H13 .  .9300 ?
    C14 C15 . 1.43(3) ?
    C14 H14 .  .9300 ?
    C15 H15 .  .9300 ?
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    C4 Pb1 C10 . . 139.6(4) ?
    C4 Pb1 S2 . . 110.2(4) ?
    C10 Pb1 S2 . . 104.5(3) ?
    C4 Pb1 S1 . . 98.5(5) ?
    C10 Pb1 S1 . . 103.3(3) ?
    S2 Pb1 S1 . . 87.33(11) ?
    C4 Pb1 S5 . 4_544 80.5(5) ?
    C10 Pb1 S5 . 4_544 91.3(4) ?
    S2 Pb1 S5 . 4_544 72.07(12) ?
    S1 Pb1 S5 . 4_544 157.32(11) ?
    C4 Pb1 S5 . 3_455 67.7(4) ?
    C10 Pb1 S5 . 3_455 78.5(3) ?
    S2 Pb1 S5 . 3_455 176.61(11) ?
    S1 Pb1 S5 . 3_455 90.44(11) ?
    S5 Pb1 S5 4_544 3_455 109.68(6) ?
    C1 S1 Pb1 . . 96.9(4) ?
    C2 S2 Pb1 . . 97.6(5) ?
    C2 C1 S3 . . 115.5(9) ?
    C2 C1 S1 . . 129.0(10) ?
    S3 C1 S1 . . 115.6(7) ?
    C1 C2 S2 . . 128.9(10) ?
    C1 C2 S4 . . 114.9(11) ?
    S2 C2 S4 . . 116.2(10) ?
    C3 S3 C1 . . 98.2(6) ?
    C3 S4 C2 . . 98.2(7) ?
    S5 C3 S4 . . 122.3(8) ?
    S5 C3 S3 . . 124.5(9) ?
    S4 C3 S3 . . 113.1(7) ?
    C5 C4 C9 . . 120.9(11) ?
    C5 C4 Pb1 . . 117.8(9) ?
    C9 C4 Pb1 . . 121.3(10) ?
    C6 C5 C4 . . 119.4(14) ?
    C6 C5 H5 . . 120.3 ?
    C4 C5 H5 . . 120.3 ?
    C5 C6 C7 . . 119.9(15) ?
    C5 C6 H6 . . 120.1 ?
    C7 C6 H6 . . 120.1 ?
    C8 C7 C6 . . 120.1(11) ?
    C8 C7 H7 . . 120.0 ?
    C6 C7 H7 . . 120.0 ?
    C7 C8 C9 . . 121.7(14) ?
    C7 C8 H8 . . 119.2 ?
    C9 C8 H8 . . 119.2 ?
    C8 C9 C4 . . 117.8(14) ?
    C8 C9 H9 . . 121.1 ?
    C4 C9 H9 . . 121.1 ?
    C11 C10 C15 . . 120.5(11) ?
    C11 C10 Pb1 . . 124.9(11) ?
    C15 C10 Pb1 . . 114.6(11) ?
    C12 C11 C10 . . 120.7(18) ?
    C12 C11 H11 . . 119.7 ?
    C10 C11 H11 . . 119.7 ?
    C11 C12 C13 . . 121(2) ?
    C11 C12 H12 . . 119.3 ?
    C13 C12 H12 . . 119.3 ?
    C12 C13 C14 . . 120.5(13) ?
    C12 C13 H13 . . 119.7 ?
    C14 C13 H13 . . 119.7 ?
    C13 C14 C15 . . 118.1(18) ?
    C13 C14 H14 . . 120.9 ?
    C15 C14 H14 . . 120.9 ?
    C10 C15 C14 . . 118.8(18) ?
    C10 C15 H15 . . 120.6 ?
    C14 C15 H15 . . 120.6 ?
data_IV
_audit_creation_method     SHELXL97
_chemical_name_systematic
;
(2-thioxo-1,3-dithiole-4,5-dithiolato-S,S')diphenylstannane
;
_chemical_name_common     ?
_chemical_formula_moiety     'C15 H10 S5 Sn'
_chemical_formula_sum     'C15 H10 S5 Sn'
_chemical_formula_iupac     '[Sn (C3 S5) (C6 H5)2]'
_chemical_formula_weight     469.23
_symmetry_cell_setting     orthorhombic
_symmetry_space_group_name_H-M     'Pna21'
_symmetry_space_group_name_Hall     'P 2c -2n'
loop_
    _symmetry_equiv_pos_as_xyz
    'x, y, z'
    '-x, -y, z+1/2'
    'x+1/2, -y+1/2, z'
    '-x+1/2, y+1/2, z+1/2'
_cell_length_a     17.3574(5)
_cell_length_b     9.2270(2)
_cell_length_c     10.3775(2)
_cell_angle_alpha     90
_cell_angle_beta     90
_cell_angle_gamma     90
_cell_volume     1662.03(7)
_cell_formula_units_Z     4
_cell_measurement_reflns_used     6500
_cell_measurement_theta_min     2.9
_cell_measurement_theta_max     27.5
_cell_measurement_temperature     150(2)
_exptl_crystal_description     needle
_exptl_crystal_colour     'orange-red'
_exptl_crystal_size_max      .48
_exptl_crystal_size_mid      .10
_exptl_crystal_size_min      .06
_exptl_crystal_density_diffrn     1.875
_exptl_crystal_density_meas     ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000     920
_exptl_absorpt_coefficient_mu     2.15
_exptl_absorpt_correction_type     empirical
_exptl_absorpt_process_details     '(SORTAV; Blessing, 1995, 1997)'
_exptl_absorpt_correction_T_min      .425
_exptl_absorpt_correction_T_max      .882
_exptl_special_details
;
 ?
;
_diffrn_ambient_temperature     150(2)
_diffrn_radiation_type     MoK\a
_diffrn_radiation_wavelength      .71073
_diffrn_radiation_source     'fine-focus sealed tube'
_diffrn_radiation_monochromator     graphite
_diffrn_measurement_device_type     'Nonius KappaCCD area-detector'
_diffrn_measurement_method     φ/ω
_diffrn_detector_area_resol_mean     ?
_diffrn_reflns_number     11483
_diffrn_reflns_av_R_equivalents      .039
_diffrn_reflns_av_sigmaI/netI      .046
_diffrn_reflns_theta_min     3.2
_diffrn_reflns_theta_max     27.5
_diffrn_reflns_theta_full     27.5
_diffrn_measured_fraction_theta_max     1.00
_diffrn_measured_fraction_theta_full     1.00
_diffrn_reflns_limit_h_min     -22
_diffrn_reflns_limit_h_max     19
_diffrn_reflns_limit_k_min     -11
_diffrn_reflns_limit_k_max     11
_diffrn_reflns_limit_l_min     -13
_diffrn_reflns_limit_l_max     13
_diffrn_standards_number     ?
_diffrn_standards_interval_count     ?
_diffrn_standards_interval_time     ?
_diffrn_standards_decay_%     ?
_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.
;
_reflns_number_total     3622
_reflns_number_gt     3405
_reflns_threshold_expression     I>2σ(I)
_refine_ls_structure_factor_coef     Fsqd
_refine_ls_matrix_type     full
_refine_ls_R_factor_all      .032
_refine_ls_R_factor_gt      .028
_refine_ls_wR_factor_ref      .061
_refine_ls_goodness_of_fit_ref     1.08
_refine_ls_restrained_S_all     1.08
_refine_ls_number_reflns     3622
_refine_ls_number_parameters     190
_refine_ls_number_restraints     1
_refine_ls_hydrogen_treatment     constr
_refine_ls_weighting_scheme     calc
_refine_ls_weighting_details
                    'w = 1/[σ²(Fo²)+(0.0284P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_shift/su_max     <0.001
_refine_ls_shift/su_mean      .000
_refine_diff_density_max      .68
_refine_diff_density_min     -1.25
_refine_ls_extinction_method     none
_refine_ls_extinction_coef     ?
_refine_ls_abs_structure_details     '(Flack, 1983)'
_refine_ls_abs_structure_Flack      -.004(19)
loop_
    _atom_type_symbol
    _atom_type_description
    _atom_type_scat_dispersion_real
    _atom_type_scat_dispersion_imag
    _atom_type_scat_source
    'C' 'C'  .0033  .0016
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'H' 'H'  .0000  .0000
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'Sn' 'Sn'  -.6537 1.4246
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
    'S' 'S'  .1246  .1234
                         'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_computing_data_collection
                 'DENZO (Otwinowski and Minor, 1997) and COLLECT (Nonius, 1998)'
_computing_cell_refinement     'DENZO and COLLECT'
_computing_data_reduction     'DENZO and COLLECT'
_computing_structure_solution     'SHELXS86 (Sheldrick, 1990)'
_computing_structure_refinement     'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics
;
ORTEX in OSCAIL (McArdle, 1994, 2000), ORTEP-3 for Windows (Farrugia, 1997)
;
_computing_publication_material     'CIFTAB (Sheldrick, 1997)'
loop_
    _atom_site_label
    _atom_site_fract_x
    _atom_site_fract_y
    _atom_site_fract_z
    _atom_site_U_iso_or_equiv
    _atom_site_adp_type
    _atom_site_calc_flag
    _atom_site_refinement_flags
    _atom_site_occupancy
    _atom_site_disorder_assembly
    _atom_site_disorder_group
    _atom_site_type_symbol
    Sn1  .101604(10)  .16708(2)  -.01258(3)  .01963(8) Uani d . 1 . . Sn
    S1  .15889(5)  .22305(10)  .20630(8)  .02618(18) Uani d . 1 . . S
    S2  .20835(5)  .30346(10)  -.10939(9)  .02471(19) Uani d . 1 . . S
    C1  .2330(2)  .3346(3)  .1525(4)  .0195(7) Uani d . 1 . . C
    C2  .25333(18)  .3662(4)  .0302(3)  .0195(7) Uani d . 1 . . C
    S3  .28947(5)  .41349(9)  .27232(7)  .02238(18) Uani d . 1 . . S
    S4  .33083(5)  .48353(9)  .01353(7)  .0260(2) Uani d . 1 . . S
    C3  .34947(19)  .5097(4)  .1743(3)  .0239(7) Uani d . 1 . . C
    S5  .42116(5)  .61976(11)  .22192(8)  .0286(2) Uani d . 1 . . S
    C4  .10113(16)  -.0625(4)  .0153(3)  .0209(8) Uani d . 1 . . C
    C5  .1555(2)  -.1267(4)  .0932(3)  .0237(7) Uani d . 1 . . C
    H5  .1917  -.0683  .1383  .028 Uiso calc R 1 . . H
    C6  .1577(2)  -.2763(4)  .1062(4)  .0328(9) Uani d . 1 . . C
    H6  .1970  -.3205  .1564  .039 Uiso calc R 1 . . H
    C7  .1024(2)  -.3614(5)  .0455(5)  .0368(10) Uani d . 1 . . C
    H7  .1033  -.4638  .0551  .044 Uiso calc R 1 . . H
    C8  .0463(2)  -.2964(4)  -.0288(4)  .0339(9) Uani d . 1 . . C
    H8  .0076  -.3538  -.0687  .041 Uiso calc R 1 . . H
    C9  .0463(2)  -.1474(4)  -.0455(3)  .0260(8) Uani d . 1 . . C
    H9  .0086  -.1032  -.0988  .031 Uiso calc R 1 . . H
    C10  -.00310(17)  .2880(3)  -.0017(4)  .0211(6) Uani d . 1 . . C
    C11  -.0392(2)  .3451(4)  -.1098(4)  .0259(9) Uani d . 1 . . C
    H11  -.0193  .3254  -.1933  .031 Uiso calc R 1 . . H
    C12  -.1045(2)  .4312(5)  -.0957(4)  .0327(10) Uani d . 1 . . C
    H12  -.1289  .4710  -.1697  .039 Uiso calc R 1 . . H
    C13  -.1338(2)  .4585(4)  .0237(4)  .0330(9) Uani d . 1 . . C
    H13  -.1782  .5179  .0324  .040 Uiso calc R 1 . . H
    C14  -.0995(2)  .4010(5)  .1318(5)  .0418(11) Uani d . 1 . . C
    H14  -.1208  .4187  .2146  .050 Uiso calc R 1 . . H
    C15  -.0337(2)  .3168(4)  .1186(4)  .0313(10) Uani d . 1 . . C
    H15  -.0094  .2785  .1933  .038 Uiso calc R 1 . . H
loop_
    _atom_site_aniso_label
    _atom_site_aniso_U_11
    _atom_site_aniso_U_22
    _atom_site_aniso_U_33
    _atom_site_aniso_U_12
    _atom_site_aniso_U_13
    _atom_site_aniso_U_23
    Sn1  .02078(12)  .01665(12)  .02147(13)  .00217(8)  -.00251(10)  -.00229(10)
    S1  .0325(5)  .0270(4)  .0190(4)  -.0096(4)  -.0022(3)  -.0003(4)
    S2  .0286(5)  .0293(5)  .0162(4)  -.0022(4)  -.0007(3)  -.0030(3)
    C1  .0190(18)  .0171(18)  .0224(18)  .0023(12)  -.0013(14)  -.0032(12)
    C2  .0183(17)  .0192(17)  .0211(17)  -.0005(14)  -.0018(12)  -.0017(13)
    S3  .0245(4)  .0247(4)  .0180(4)  -.0053(3)  .0001(3)  -.0032(3)
    S4  .0270(4)  .0307(5)  .0204(5)  -.0052(4)  .0024(3)  -.0024(3)
    C3  .0237(18)  .0210(18)  .0271(18)  .0003(15)  .0012(13)  -.0017(13)
    S5  .0290(5)  .0344(5)  .0225(4)  -.0116(4)  .0057(4)  -.0064(4)
    C4  .0212(17)  .0141(16)  .027(2)  .0018(11)  .0057(12)  -.0044(13)
    C5  .0240(18)  .0205(18)  .0266(18)  .0004(15)  .0018(14)  -.0021(15)
    C6  .042(2)  .021(2)  .036(2)  .0039(17)  .0010(17)  .0034(17)
    C7  .052(3)  .019(2)  .039(2)  -.0010(16)  .0072(17)  .0031(18)
    C8  .038(2)  .0292(19)  .034(2)  -.0146(16)  .0032(19)  -.0129(19)
    C9  .0253(18)  .0257(18)  .027(2)  -.0032(14)  .0045(13)  -.0054(13)
    C10  .0212(15)  .0152(14)  .0268(18)  -.0008(12)  .0009(14)  .0002(16)
    C11  .025(2)  .029(2)  .023(2)  .0036(15)  -.0013(15)  -.0049(14)
    C12  .028(2)  .028(2)  .042(3)  .0066(15)  -.0080(15)  -.0036(18)
    C13  .0211(18)  .033(2)  .045(3)  .0076(15)  .0022(16)  -.0079(16)
    C14  .035(3)  .047(3)  .043(3)  .0057(18)  .0156(17)  -.005(2)
    C15  .030(2)  .035(2)  .029(2)  .0041(16)  .0048(17)  .0053(16)
_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_site_symmetry_2
    _geom_bond_distance
    _geom_bond_publ_flag
    Sn1 C10 . 2.135(3) ?
    Sn1 C4 . 2.138(3) ?
    Sn1 S2 . 2.4547(10) ?
    Sn1 S1 . 2.5327(9) ?
    Sn1 S5 4_544 2.8174(9) ?
    Sn1 S5 3_455 4.7683(10) ?
    S1 C1 . 1.740(4) ?
    S2 C2 . 1.745(3) ?
    C1 C2 . 1.349(5) ?
    C1 S3 . 1.742(4) ?
    C2 S4 . 1.735(3) ?
    S3 C3 . 1.705(3) ?
    S4 C3 . 1.717(3) ?
    C3 S5 . 1.681(3) ?
    S5 Sn1 4 2.8175(9) ?
    C4 C5 . 1.377(5) ?
    C4 C9 . 1.383(5) ?
    C5 C6 . 1.387(4) ?
    C5 H5 .  .9500 ?
    C6 C7 . 1.392(6) ?
    C6 H6 .  .9500 ?
    C7 C8 . 1.379(6) ?
    C7 H7 .  .9500 ?
    C8 C9 . 1.386(5) ?
    C8 H8 .  .9500 ?
    C9 H9 .  .9500 ?
    C10 C15 . 1.383(6) ?
    C10 C11 . 1.389(5) ?
    C11 C12 . 1.393(5) ?
    C11 H11 .  .9500 ?
    C12 C13 . 1.363(6) ?
    C12 H12 .  .9500 ?
    C13 C14 . 1.375(6) ?
    C13 H13 .  .9500 ?
    C14 C15 . 1.389(6) ?
    C14 H14 .  .9500 ?
    C15 H15 .  .9500 ?
loop_
    _geom_angle_atom_site_label_1
    _geom_angle_atom_site_label_2
    _geom_angle_atom_site_label_3
    _geom_angle_site_symmetry_1
    _geom_angle_site_symmetry_3
    _geom_angle
    _geom_angle_publ_flag
    C10 Sn1 C4 . . 120.47(11) ?
    C10 Sn1 S2 . . 113.34(8) ?
    C4 Sn1 S2 . . 124.49(8) ?
    C10 Sn1 S1 . . 100.38(10) ?
    C4 Sn1 S1 . . 94.72(9) ?
    S2 Sn1 S1 . . 88.06(3) ?
    C10 Sn1 S5 . 4_544 90.77(11) ?
    C4 Sn1 S5 . 4_544 88.74(9) ?
    S2 Sn1 S5 . 4_544 77.59(3) ?
    S1 Sn1 S5 . 4_544 164.51(3) ?
    C10 Sn1 S5 . 3_455 72.77(8) ?
    C4 Sn1 S5 . 3_455 51.58(8) ?
    S2 Sn1 S5 . 3_455 171.57(3) ?
    S1 Sn1 S5 . 3_455 85.03(2) ?
    S5 Sn1 S5 4_544 3_455 108.722(16) ?
    C1 S1 Sn1 . . 97.09(13) ?
    C2 S2 Sn1 . . 99.67(11) ?
    C2 C1 S1 . . 128.5(3) ?
    C2 C1 S3 . . 115.7(3) ?
    S1 C1 S3 . . 115.7(2) ?
    C1 C2 S4 . . 115.6(3) ?
    C1 C2 S2 . . 126.3(3) ?
    S4 C2 S2 . . 118.10(18) ?
    C3 S3 C1 . . 97.78(16) ?
    C3 S4 C2 . . 97.86(16) ?
    S5 C3 S3 . . 126.3(2) ?
    S5 C3 S4 . . 120.7(2) ?
    S3 C3 S4 . . 113.05(19) ?
    C3 S5 Sn1 . 4 106.11(12) ?
    C5 C4 C9 . . 119.7(3) ?
    C5 C4 Sn1 . . 120.2(2) ?
    C9 C4 Sn1 . . 120.1(2) ?
    C4 C5 C6 . . 120.2(3) ?
    C4 C5 H5 . . 119.9 ?
    C6 C5 H5 . . 119.9 ?
    C5 C6 C7 . . 119.9(4) ?
    C5 C6 H6 . . 120.0 ?
    C7 C6 H6 . . 120.0 ?
    C8 C7 C6 . . 119.6(4) ?
    C8 C7 H7 . . 120.2 ?
    C6 C7 H7 . . 120.2 ?
    C7 C8 C9 . . 120.1(4) ?
    C7 C8 H8 . . 120.0 ?
    C9 C8 H8 . . 120.0 ?
    C4 C9 C8 . . 120.3(4) ?
    C4 C9 H9 . . 119.8 ?
    C8 C9 H9 . . 119.8 ?
    C15 C10 C11 . . 118.9(3) ?
    C15 C10 Sn1 . . 118.4(3) ?
    C11 C10 Sn1 . . 122.6(3) ?
    C10 C11 C12 . . 119.9(4) ?
    C10 C11 H11 . . 120.1 ?
    C12 C11 H11 . . 120.1 ?
    C13 C12 C11 . . 120.3(4) ?
    C13 C12 H12 . . 119.8 ?
    C11 C12 H12 . . 119.8 ?
    C12 C13 C14 . . 120.6(3) ?
    C12 C13 H13 . . 119.7 ?
    C14 C13 H13 . . 119.7 ?
    C13 C14 C15 . . 119.4(4) ?
    C13 C14 H14 . . 120.3 ?
    C15 C14 H14 . . 120.3 ?
    C10 C15 C14 . . 120.8(4) ?
    C10 C15 H15 . . 119.6 ?
    C14 C15 H15 . . 119.6 ?
loop_
    _geom_hbond_atom_site_label_D
    _geom_hbond_atom_site_label_H
    _geom_hbond_atom_site_label_A
    _geom_hbond_site_symmetry_A
    _geom_hbond_distance_DH
    _geom_hbond_distance_HA
    _geom_hbond_distance_DA
    _geom_hbond_angle_DHA
    C5 H5 S1 .  .95 2.84 3.434(4) 122
    C11 H11 S5 4_544  .95 2.70 3.401(4) 131
