#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/01/2240146.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2240146
loop_
_publ_author_name
'Baughman, Russell G.'
'Delanty, Molly C.'
'Ortwerth, Michael F.'
_publ_section_title
;
 Crystal structure of 1,6-dithiacyclodeca-cis-3,cis-8-diene
 (DTCDD)
;
_journal_coeditor_code           HB7285
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1218
_journal_paper_doi               10.1107/S1600536814023319
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C8 H12 S2'
_chemical_formula_moiety         'C8 H12 S2'
_chemical_formula_sum            'C8 H12 S2'
_chemical_formula_weight         172.31
_chemical_name_common            DTCDD
_chemical_name_systematic
;
1,6-Dithiacyclodeca-cis-3,cis-8-diene
;
_space_group_IT_number           64
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5706(6)
_cell_length_b                   7.5329(4)
_cell_length_c                   8.4303(4)
_cell_measurement_reflns_used    100
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.18
_cell_measurement_theta_min      10.83
_cell_volume                     861.80(7)
_computing_cell_refinement
;
XSCANS  (Bruker, 1996)
;
_computing_data_collection
;
XSCANS (Bruker, 1996)
;
_computing_data_reduction
;
XSCANS (Bruker, 1996)
;
_computing_molecular_graphics
;
SHELXTL/PC (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL/PC and SHELXL97  (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS86 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'Bruker P4 diffractometer'
_diffrn_measurement_method       θ/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            707
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        1.0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.540
_exptl_absorpt_correction_T_max  0.845
_exptl_absorpt_correction_T_min  0.676
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(XSHELL; Bruker, 1999)
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.193
_refine_diff_density_min         -0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     24
_refine_ls_number_reflns         509
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0314P)²+0.6276P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0899
_reflns_number_gt                398
_reflns_number_total             509
_reflns_threshold_expression     'I > 2σ(I)'
_iucr_refine_instructions_details
;
TITL mfo02b in Cmca    BEST LATTS!!
CELL 0.71073  13.5706   7.5329   8.4303  90.00  90.00  90.00
ZERR    4.00   0.0006   0.0004   0.0004   0.00   0.00   0.00
LATT  7
SYMM -X, .5-Y, .5+Z
SYMM -X, .5+Y, .5-Z
SYMM X, -Y, -Z
SFAC C H S
UNIT 32 48 8
MERG 2
OMIT 9 7 4
OMIT 2 4 5
OMIT 15 3 4
OMIT 4 8 3
L.S. 10
BOND 0.5
CONF
BOND $H
ACTA
FMAP 2
PLAN 3
REM WGHT    0.200000
REM WGHT    0.031900    0.701300
REM WGHT    0.025400    0.761200
REM  mfo02b in Cmca    BEST LATTS
REM R1 =  0.0340 for    398 Fo > 4sig(Fo)  and  0.0504 for all    513 data
REM     25 parameters refined using      0 restraints
REM WGHT    0.025100    0.767200
REM WGHT    0.025100    0.767200
REM WGHT    0.030700    0.637600
REM WGHT    0.031200    0.629800
REM WGHT    0.031400    0.626900
REM WGHT    0.031400    0.627600
REM WGHT    0.031400    0.627600
WGHT    0.031400    0.627600
FVAR       0.45220
S1    3    0.300066    0.500000    0.500000    10.50000    0.02526    0.07658 =
         0.07671    0.03295    0.00000    0.00000
C1    1    0.384790    0.610012    0.365003    11.00000    0.03163    0.05210 =
         0.04552    0.01130   -0.00243    0.00095
AFIX  23
H1A   2    0.424555    0.521007    0.311932    11.00000   -1.20000
H1B   2    0.347176    0.672418    0.284608    11.00000   -1.20000
AFIX   0
C2    1    0.450872    0.737969    0.446208    11.00000    0.04603    0.03333 =
         0.04059    0.00550    0.00494    0.00757
AFIX  43
H2    2    0.420391    0.828120    0.503420    11.00000   -1.20000
HKLF 4
REM  mfo02 in Cmca    BEST LATTS
REM R1 =  0.0341 for    398 Fo > 4sig(Fo)  and  0.0487 for all    509 data
REM     24 parameters refined using      0 restraints
END
WGHT      0.0316      0.6276
REM Highest difference peak  0.193,  deepest hole -0.220,  1-sigma level  0.042
Q1    1   0.3273  0.4238  0.4420  11.00000  0.05    0.19
Q2    1   0.3330  0.5580  0.4148  11.00000  0.05    0.17
Q3    1   0.3012  0.3934  0.3714  11.00000  0.05    0.14
;
_cod_data_source_file            hb7285sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               2240146
_cod_database_fobs_code          2240146
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'x+1/2, -y, z-1/2'
'-x+1/2, y+1/2, z'
loop_
_atom_site_type_symbol
_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_symmetry_multiplicity
S S1 0.30007(4) 0.5000 0.5000 0.0595(3) Uani d S 1 2
C C1 0.38479(12) 0.6100(3) 0.3650(2) 0.0431(5) Uani d . 1 1
H H1A 0.4246 0.5210 0.3119 0.052 Uiso calc R 1 1
H H1B 0.3472 0.6724 0.2846 0.052 Uiso calc R 1 1
C C2 0.45087(12) 0.7380(2) 0.4462(2) 0.0400(4) Uani d . 1 1
H H2 0.4204 0.8281 0.5034 0.048 Uiso calc R 1 1
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
S1 0.0253(3) 0.0766(6) 0.0767(6) 0.000 0.000 0.0329(5)
C1 0.0316(8) 0.0521(11) 0.0455(9) 0.0009(8) -0.0024(7) 0.0113(8)
C2 0.0460(10) 0.0333(8) 0.0406(8) 0.0076(8) 0.0049(8) 0.0055(7)
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
0 0 -2
-3 1 -1
-2 2 0
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
C1 S1 C1 . 4_566 101.52(11)
C2 C1 S1 . . 112.93(13)
C2 C1 H1A . . 109.0
S1 C1 H1A . . 109.0
C2 C1 H1B . . 109.0
S1 C1 H1B . . 109.0
H1A C1 H1B . . 107.8
C2 C2 C1 12_655 . 127.18(9)
C2 C2 H2 12_655 . 116.4
C1 C2 H2 . . 116.4
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
S1 C1 . 1.8177(18)
S1 C1 4_566 1.8177(18)
C1 C2 . 1.484(3)
C1 H1A . 0.9700
C1 H1B . 0.9700
C2 C2 12_655 1.333(3)
C2 H2 . 0.9300
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C1 S1 C1 C2 4_566 . -59.88(11) n
S1 C1 C2 C2 . 12_655 122.76(9) n
