#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:48:47 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179816 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/12/7011261.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7011261
loop_
_publ_author_name
'Vasile Berceanc'
'Crina Crainic'
'Ionel Haiduc'
'Mary F. Mahon'
'Kieran C. Molloy'
'Monica M. Venter'
'Paul J. Wilson'
_publ_section_title
;
 The structural chemistry of organotin derivatives of
 5-mercapto-3-phenyl-1,3,4-thiadiazoline-2-thione: supramolecular
 structures involving intermolecular SnS, N--HS or SS interactions
;
_journal_issue                   6
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1036
_journal_page_last               1045
_journal_paper_doi               10.1039/b109726a
_journal_year                    2002
_chemical_formula_sum            'C28 H20 N4 S6 Sn'
_chemical_formula_weight         723.53
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.340(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9240(10)
_cell_length_b                   21.975(2)
_cell_length_c                   11.2550(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     2931.1(5)
_computing_data_reduction
'Denzo and Scalepack (otwinowski & Minor, 1997'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'scintillation counter'
_diffrn_measurement_method       'Enraf(Nonius CAD4 4(circle diffractometer'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0121
_diffrn_reflns_av_sigmaI/netI    0.0189
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2760
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    1.326
_exptl_absorpt_correction_T_max  0.7774
_exptl_absorpt_correction_T_min  0.7774
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.210
_refine_diff_density_min         -0.833
_refine_diff_density_rms         0.148
_refine_ls_extinction_coef       0.0012(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.221
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         2572
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.221
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0636P)²+72.7872P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1682
_refine_ls_wR_factor_ref         0.1687
_reflns_number_gt                2502
_reflns_number_total             2572
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b109726a.txt
_cod_data_source_block           99kcm6
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/adriana/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_cell_volume        2931.1(4)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7011261
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'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Sn1 Sn 0.5000 0.71174(3) 0.2500 0.0145(3) Uani 1 2 d S . .
S1 S 0.35784(15) 0.79237(8) 0.20194(17) 0.0216(4) Uani 1 1 d . A .
S2 S 0.10876(15) 0.76611(9) 0.13211(17) 0.0215(4) Uani 1 1 d . A .
S3 S -0.06689(15) 0.66956(9) 0.07111(18) 0.0257(5) Uani 1 1 d . . .
N1 N 0.2614(5) 0.6841(3) 0.1642(5) 0.0182(13) Uani 1 1 d . A .
N2 N 0.1590(5) 0.6545(3) 0.1320(5) 0.0176(12) Uani 1 1 d . . .
C1 C 0.2462(6) 0.7416(4) 0.1667(6) 0.0200(15) Uani 1 1 d . . .
C2 C 0.0665(6) 0.6900(3) 0.1109(6) 0.0184(15) Uani 1 1 d . A .
C3 C 0.5395(6) 0.6619(3) 0.0992(6) 0.0190(15) Uani 1 1 d . . .
C4 C 0.4763(7) 0.6115(4) 0.0616(7) 0.0269(17) Uani 1 1 d . . .
H4 H 0.4176 0.5982 0.1060 0.032 Uiso 1 1 calc R . .
C5 C 0.4977(8) 0.5800(5) -0.0409(10) 0.050(3) Uani 1 1 d . . .
H5 H 0.4535 0.5456 -0.0673 0.059 Uiso 1 1 calc R . .
C6 C 0.5858(8) 0.5999(6) -0.1044(9) 0.052(3) Uani 1 1 d . . .
H6 H 0.6014 0.5790 -0.1746 0.062 Uiso 1 1 calc R . .
C7 C 0.6489(6) 0.6491(4) -0.0655(7) 0.0288(18) Uani 1 1 d . . .
H7 H 0.7088 0.6620 -0.1086 0.035 Uiso 1 1 calc R . .
C8 C 0.6272(6) 0.6804(4) 0.0349(7) 0.0211(16) Uani 1 1 d . . .
H8 H 0.6720 0.7147 0.0607 0.025 Uiso 1 1 calc R . .
C9 C 0.1559(10) 0.5870(3) 0.1235(9) 0.0240(14) Uani 0.50 1 d PG A 1
C10 C 0.1999(9) 0.5580(4) 0.0292(8) 0.0240(14) Uani 0.50 1 d PG A 1
H10 H 0.2288 0.5814 -0.0316 0.029 Uiso 0.50 1 calc PR A 1
C11 C 0.2016(8) 0.4948(4) 0.0238(7) 0.0240(14) Uani 0.50 1 d PG A 1
H11 H 0.2316 0.4750 -0.0407 0.029 Uiso 0.50 1 calc PR A 1
C12 C 0.1593(9) 0.4607(3) 0.1128(9) 0.0240(14) Uani 0.50 1 d PG A 1
H12 H 0.1605 0.4175 0.1091 0.029 Uiso 0.50 1 calc PR A 1
C13 C 0.1153(9) 0.4897(4) 0.2072(8) 0.0240(14) Uani 0.50 1 d PG A 1
H13 H 0.0865 0.4663 0.2680 0.029 Uiso 0.50 1 calc PR A 1
C14 C 0.1136(9) 0.5529(4) 0.2125(7) 0.0240(14) Uani 0.50 1 d PG A 1
H14 H 0.0836 0.5727 0.2770 0.029 Uiso 0.50 1 calc PR A 1
C901 C 0.1597(9) 0.5933(3) 0.1396(8) 0.0221(14) Uani 0.50 1 d PG A 2
C902 C 0.1086(8) 0.5592(4) 0.0447(7) 0.0221(14) Uani 0.50 1 d PG A 2
H902 H 0.0770 0.5789 -0.0264 0.027 Uiso 0.50 1 calc PR A 2
C903 C 0.1037(8) 0.4962(4) 0.0537(7) 0.0221(14) Uani 0.50 1 d PG A 2
H903 H 0.0687 0.4728 -0.0112 0.027 Uiso 0.50 1 calc PR A 2
C904 C 0.1499(9) 0.4673(3) 0.1576(8) 0.0221(14) Uani 0.50 1 d PG A 2
H904 H 0.1466 0.4242 0.1638 0.027 Uiso 0.50 1 calc PR A 2
C905 C 0.2011(8) 0.5014(4) 0.2525(7) 0.0221(14) Uani 0.50 1 d PG A 2
H905 H 0.2327 0.4817 0.3236 0.027 Uiso 0.50 1 calc PR A 2
C906 C 0.2060(8) 0.5645(4) 0.2435(7) 0.0221(14) Uani 0.50 1 d PG A 2
H906 H 0.2409 0.5878 0.3084 0.027 Uiso 0.50 1 calc PR A 2
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 0.0000 0.0000 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C3 Sn1 C3 117.7(4) . 2_655 ?
C3 Sn1 S1 109.8(2) . 2_655 ?
C3 Sn1 S1 113.81(19) 2_655 2_655 ?
C3 Sn1 S1 113.81(19) . . ?
C3 Sn1 S1 109.8(2) 2_655 . ?
S1 Sn1 S1 88.35(9) 2_655 . ?
C1 S1 Sn1 94.5(3) . . ?
C1 S2 C2 89.1(4) . . ?
C1 N1 N2 110.1(6) . . ?
C2 N2 C901 125.9(7) . . ?
C2 N2 N1 116.8(6) . . ?
C901 N2 N1 116.7(7) . . ?
C2 N2 C9 123.4(7) . . ?
C901 N2 C9 7.3(6) . . ?
N1 N2 C9 119.7(7) . . ?
N1 C1 S2 115.9(6) . . ?
N1 C1 S1 122.0(6) . . ?
S2 C1 S1 122.1(4) . . ?
N2 C2 S3 129.0(6) . . ?
N2 C2 S2 108.0(5) . . ?
S3 C2 S2 123.0(4) . . ?
C4 C3 C8 119.3(7) . . ?
C4 C3 Sn1 119.9(5) . . ?
C8 C3 Sn1 120.8(6) . . ?
C5 C4 C3 120.6(8) . . ?
C4 C5 C6 118.8(9) . . ?
C7 C6 C5 120.1(8) . . ?
C6 C7 C8 121.0(8) . . ?
C7 C8 C3 120.1(7) . . ?
C10 C9 C14 120.0 . . ?
C10 C9 N2 119.9(6) . . ?
C14 C9 N2 120.1(6) . . ?
C9 C10 C11 120.0 . . ?
C12 C11 C10 120.0 . . ?
C13 C12 C11 120.0 . . ?
C14 C13 C12 120.0 . . ?
C13 C14 C9 120.0 . . ?
N2 C901 C902 119.4(7) . . ?
N2 C901 C906 120.5(7) . . ?
C902 C901 C906 120.0 . . ?
C903 C902 C901 120.0 . . ?
C902 C903 C904 120.0 . . ?
C903 C904 C905 120.0 . . ?
C906 C905 C904 120.0 . . ?
C905 C906 C901 120.0 . . ?
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
Sn1 C3 2.116(7) . ?
Sn1 C3 2.116(7) 2_655 ?
Sn1 S1 2.4704(19) 2_655 ?
Sn1 S1 2.4704(19) . ?
S1 C1 1.748(8) . ?
S2 C1 1.728(7) . ?
S2 C2 1.756(8) . ?
S3 C2 1.666(7) . ?
N1 C1 1.278(10) . ?
N1 N2 1.395(8) . ?
N2 C2 1.350(9) . ?
N2 C901 1.347(9) . ?
N2 C9 1.486(9) . ?
C3 C4 1.380(11) . ?
C3 C8 1.396(10) . ?
C4 C5 1.394(12) . ?
C5 C6 1.404(14) . ?
C6 C7 1.361(14) . ?
C7 C8 1.371(11) . ?
C9 C10 1.3900 . ?
C9 C14 1.3900 . ?
C10 C11 1.3900 . ?
C11 C12 1.3900 . ?
C12 C13 1.3900 . ?
C13 C14 1.3900 . ?
C901 C902 1.3900 . ?
C901 C906 1.3900 . ?
C902 C903 1.3900 . ?
C903 C904 1.3900 . ?
C904 C905 1.3900 . ?
C905 C906 1.3900 . ?
