#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/47/7114730.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_7114730
loop_
_publ_author_name
'Cameron, T. Stanley'
'Decken, Andreas'
'Fang, Min'
'Passmore, Jack'
_publ_section_title
;
 Synthesis and characterization of the heteroaromatic MF6− (M = As,
 Sb) salts of the 1,2,4-trithiolanylium dication
 [PhCSSC(Ph)S]2+
;
_journal_issue                   15
_journal_name_full               'Chemical Communications'
_journal_page_first              1370
_journal_paper_doi               10.1039/b100001m
_journal_year                    2001
_chemical_formula_sum            'C14 H10 F12 S3 Sb2'
_chemical_formula_weight         745.89
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 104.56(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.359(5)
_cell_length_b                   15.148(2)
_cell_length_c                   15.762(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      19.9
_cell_measurement_theta_min      18.8
_cell_volume                     2162.8(12)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan for Windows (MSC, 1997)'
_computing_publication_material  'teXsan for Windows (MSC, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
SHELXS86 (Sheldrick, 1985)
;
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC5R'
_diffrn_measurement_method       ω-2θ
_diffrn_orient_matrix_UB_11      0.00991
_diffrn_orient_matrix_UB_12      0.06211
_diffrn_orient_matrix_UB_13      0.02220
_diffrn_orient_matrix_UB_21      -0.01147
_diffrn_orient_matrix_UB_22      0.02212
_diffrn_orient_matrix_UB_23      -0.06113
_diffrn_orient_matrix_UB_31      -0.10935
_diffrn_orient_matrix_UB_32      0.00331
_diffrn_orient_matrix_UB_33      -0.00821
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.06174
_diffrn_reflns_av_sigmaI/netI    0.130
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            6923
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         2.62
_diffrn_standards_decay_%        -1.66
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.885
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.883
_exptl_absorpt_correction_type
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.291
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1408.00
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.38
_refine_diff_density_min         -1.08
_refine_ls_extinction_coef       0.00000024(2)
_refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.'
_refine_ls_extinction_method     'Zachariasen (1967)'
_refine_ls_goodness_of_fit_all   2.910
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     281
_refine_ls_number_reflns         2263
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.0006
_refine_ls_shift/su_mean         0.0004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(Fo) + 0.00001|Fo|²]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.2080
_refine_ls_wR_factor_ref         0.2020
_reflns_number_gt                2263
_reflns_number_total             6564
_reflns_threshold_expression     I>3.00σ(I)
_cod_data_source_file            b100001m.txt
_cod_data_source_block           pass7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2162.8(9)
_cod_original_sg_symbol_H-M      'P 21/n     '
_cod_original_formula_sum        'C14 H10 F12 S3 Sb2 '
_cod_database_code               7114730
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
1/2-x,1/2+y,1/2-z
'   -x,   -y,   -z'
1/2+x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_calc_flag
Sb(1) 0.12149(7) 0.36430(4) 0.12854(4) 0.0568(2) 1.000 Uani d
Sb(2) 0.22980(7) 0.39590(4) 0.50209(4) 0.0631(2) 1.000 Uani d
S(1) 0.3532(2) 0.1081(1) 0.1746(1) 0.0569(7) 1.000 Uani d
S(2) 0.1600(2) 0.0570(1) 0.1886(1) 0.0583(7) 1.000 Uani d
S(3) 0.3013(2) 0.1627(1) 0.3425(1) 0.0530(7) 1.000 Uani d
F(1) 0.212(1) 0.2866(5) 0.0680(5) 0.159(4) 1.000 Uani d
F(2) 0.0395(7) 0.4448(4) 0.1899(4) 0.112(3) 1.000 Uani d
F(3) 0.0721(6) 0.2702(4) 0.1901(4) 0.100(2) 1.000 Uani d
F(4) 0.1887(9) 0.4593(4) 0.0756(4) 0.135(3) 1.000 Uani d
F(5) 0.2989(5) 0.3707(4) 0.2132(4) 0.110(2) 1.000 Uani d
F(6) -0.0556(8) 0.3593(4) 0.0450(5) 0.170(3) 1.000 Uani d
F(7) 0.355(2) 0.3647(7) 0.450(1) 0.47(1) 1.000 Uani d
F(8) 0.092(1) 0.4196(9) 0.551(1) 0.385(9) 1.000 Uani d
F(9) 0.346(1) 0.3934(7) 0.6077(5) 0.225(5) 1.000 Uani d
F(10) 0.100(2) 0.409(1) 0.4008(6) 0.45(1) 1.000 Uani d
F(11) 0.2739(8) 0.5084(4) 0.4750(4) 0.135(3) 1.000 Uani d
F(12) 0.190(1) 0.2813(5) 0.5248(7) 0.273(6) 1.000 Uani d
C(1) 0.4077(8) 0.1661(5) 0.2693(5) 0.043(2) 1.000 Uani d
C(2) 0.5375(9) 0.2172(5) 0.2872(5) 0.051(3) 1.000 Uani d
C(3) 0.628(1) 0.2148(6) 0.2281(6) 0.080(4) 1.000 Uani d
C(4) 0.759(1) 0.2639(7) 0.2446(7) 0.095(4) 1.000 Uani d
C(5) 0.798(1) 0.3126(6) 0.3191(7) 0.081(4) 1.000 Uani d
C(6) 0.709(1) 0.3157(6) 0.3773(6) 0.076(3) 1.000 Uani d
C(7) 0.5807(9) 0.2668(6) 0.3612(6) 0.068(3) 1.000 Uani d
C(8) 0.1591(8) 0.0972(5) 0.2890(5) 0.048(2) 1.000 Uani d
C(9) 0.0420(9) 0.0786(5) 0.3279(5) 0.051(3) 1.000 Uani d
C(10) 0.0322(9) 0.1195(6) 0.4061(6) 0.075(3) 1.000 Uani d
C(11) -0.083(1) 0.1048(7) 0.4398(6) 0.088(4) 1.000 Uani d
C(12) -0.190(1) 0.0439(7) 0.4024(8) 0.077(4) 1.000 Uani d
C(13) -0.186(1) 0.0018(8) 0.3249(7) 0.093(5) 1.000 Uani d
C(14) -0.071(1) 0.0188(7) 0.2888(6) 0.079(4) 1.000 Uani d
H(1) 0.6000 0.1804 0.1762 0.093 1.000 Uiso c
H(2) 0.8186 0.2622 0.2038 0.118 1.000 Uiso c
H(3) 0.8885 0.3438 0.3304 0.093 1.000 Uiso c
H(4) 0.7382 0.3521 0.4274 0.093 1.000 Uiso c
H(5) 0.5219 0.2670 0.4026 0.083 1.000 Uiso c
H(6) 0.1089 0.1577 0.4373 0.091 1.000 Uiso c
H(7) -0.0934 0.1365 0.4886 0.107 1.000 Uiso c
H(8) -0.2709 0.0338 0.4281 0.092 1.000 Uiso c
H(9) -0.2562 -0.0418 0.3031 0.110 1.000 Uiso c
H(10) -0.0685 -0.0062 0.2343 0.096 1.000 Uiso c
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 56 0.002 0.002
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
H 0 40 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
S 0 12 0.110 0.124
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
F 0 48 0.014 0.010
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
Sb 0 8 -0.816 1.546
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-2 1 1
-1 2 0
-1 3 1
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
F(1) Sb(1) F(2) 176.7(6) ?
F(1) Sb(1) F(3) 88.0(5) ?
F(1) Sb(1) F(4) 90.6(6) ?
F(1) Sb(1) F(5) 86.2(6) ?
F(1) Sb(1) F(6) 94.0(7) ?
F(2) Sb(1) F(3) 93.0(5) ?
F(2) Sb(1) F(4) 88.1(5) ?
F(2) Sb(1) F(5) 90.6(4) ?
F(2) Sb(1) F(6) 89.2(6) ?
F(3) Sb(1) F(4) 173.1(5) ?
F(3) Sb(1) F(5) 88.2(4) ?
F(3) Sb(1) F(6) 91.7(5) ?
F(4) Sb(1) F(5) 85.0(5) ?
F(4) Sb(1) F(6) 95.1(6) ?
F(5) Sb(1) F(6) 179.8(6) ?
F(7) Sb(2) F(8) 172(1) ?
F(7) Sb(2) F(9) 86(1) ?
F(7) Sb(2) F(10) 92(2) ?
F(7) Sb(2) F(11) 81.7(7) ?
F(7) Sb(2) F(12) 95.4(9) ?
F(8) Sb(2) F(9) 86(1) ?
F(8) Sb(2) F(10) 96(2) ?
F(8) Sb(2) F(11) 98.3(8) ?
F(8) Sb(2) F(12) 84.6(9) ?
F(9) Sb(2) F(10) 178(1) ?
F(9) Sb(2) F(11) 94.7(7) ?
F(9) Sb(2) F(12) 85.3(8) ?
F(10) Sb(2) F(11) 84.1(9) ?
F(10) Sb(2) F(12) 96(1) ?
F(11) Sb(2) F(12) 177.1(8) ?
S(2) S(1) C(1) 100.4(5) ?
S(1) S(2) C(8) 100.5(5) ?
C(1) S(3) C(8) 101.6(6) ?
S(1) C(1) S(3) 118.4(8) ?
S(1) C(1) C(2) 120.8(9) ?
S(3) C(1) C(2) 121(1) ?
C(1) C(2) C(3) 119(1) ?
C(1) C(2) C(7) 122(1) ?
C(3) C(2) C(7) 119(1) ?
C(2) C(3) C(4) 121(2) ?
C(2) C(3) H(1) 120.5 no
C(4) C(3) H(1) 118.5 no
C(3) C(4) C(5) 119(2) ?
C(3) C(4) H(2) 121.2 no
C(5) C(4) H(2) 119.8 no
C(4) C(5) C(6) 121(2) ?
C(4) C(5) H(3) 117.5 no
C(6) C(5) H(3) 121.7 no
C(5) C(6) C(7) 120(2) ?
C(5) C(6) H(4) 117.2 no
C(7) C(6) H(4) 123.1 no
C(2) C(7) C(6) 121(1) ?
C(2) C(7) H(5) 119.5 no
C(6) C(7) H(5) 119.5 no
S(2) C(8) S(3) 119.0(8) ?
S(2) C(8) C(9) 122(1) ?
S(3) C(8) C(9) 119(1) ?
C(8) C(9) C(10) 121(1) ?
C(8) C(9) C(14) 121(1) ?
C(10) C(9) C(14) 119(1) ?
C(9) C(10) C(11) 121(1) ?
C(9) C(10) H(6) 123.2 no
C(11) C(10) H(6) 115.5 no
C(10) C(11) C(12) 117(2) ?
C(10) C(11) H(7) 118.2 no
C(12) C(11) H(7) 124.0 no
C(11) C(12) C(13) 122(2) ?
C(11) C(12) H(8) 113.4 no
C(13) C(12) H(8) 124.5 no
C(12) C(13) C(14) 120(2) ?
C(12) C(13) H(9) 113.8 no
C(14) C(13) H(9) 125.6 no
C(9) C(14) C(13) 121(2) ?
C(9) C(14) H(10) 119.8 no
C(13) C(14) H(10) 118.8 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Sb(1) F(1) 1.85(1) ?
Sb(1) F(2) 1.845(9) ?
Sb(1) F(3) 1.842(8) ?
Sb(1) F(4) 1.86(1) ?
Sb(1) F(5) 1.857(9) ?
Sb(1) F(6) 1.82(1) ?
Sb(2) F(7) 1.80(2) ?
Sb(2) F(8) 1.68(1) ?
Sb(2) F(9) 1.76(1) ?
Sb(2) F(10) 1.68(1) ?
Sb(2) F(11) 1.826(9) ?
Sb(2) F(12) 1.82(1) ?
S(1) S(2) 2.036(5) ?
S(1) C(1) 1.70(1) ?
S(2) C(8) 1.67(1) ?
S(3) C(1) 1.70(1) ?
S(3) C(8) 1.72(1) ?
C(1) C(2) 1.41(2) ?
C(2) C(3) 1.39(2) ?
C(2) C(7) 1.35(2) ?
C(3) C(4) 1.36(2) ?
C(3) H(1) 0.97 no
C(4) C(5) 1.35(2) ?
C(4) H(2) 0.99 no
C(5) C(6) 1.37(2) ?
C(5) H(3) 0.98 no
C(6) C(7) 1.36(2) ?
C(6) H(4) 0.95 no
C(7) H(5) 0.95 no
C(8) C(9) 1.42(2) ?
C(9) C(10) 1.39(2) ?
C(9) C(14) 1.37(2) ?
C(10) C(11) 1.39(2) ?
C(10) H(6) 0.98 no
C(11) C(12) 1.38(2) ?
C(11) H(7) 0.93 no
C(12) C(13) 1.36(2) ?
C(12) H(8) 0.99 no
C(13) C(14) 1.34(2) ?
C(13) H(9) 0.96 no
C(14) H(10) 0.93 no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Sb(1) F(6) 1.82(1) . no
Sb(1) F(3) 1.842(8) . no
Sb(1) F(2) 1.845(9) . no
Sb(1) F(1) 1.85(1) . no
Sb(1) F(4) 1.86(1) . no
Sb(1) F(5) 1.857(9) . no
Sb(2) F(10) 1.68(1) . no
Sb(2) F(8) 1.68(1) . no
Sb(2) F(9) 1.76(1) . no
Sb(2) F(7) 1.80(2) . no
Sb(2) F(12) 1.82(1) . no
Sb(2) F(11) 1.826(9) . no
S(1) F(11) 2.83(1) 2_545 no
S(1) F(2) 3.24(1) 2_545 no
S(1) F(1) 3.26(1) . no
S(1) F(8) 3.36(1) 4_554 no
S(1) F(10) 3.44(3) 2_545 no
S(2) F(11) 2.92(1) 2_545 no
S(2) F(9) 2.99(1) 4_454 no
S(2) F(5) 3.22(1) 2_545 no
S(2) F(3) 3.32(1) . no
S(2) F(2) 3.41(1) 2_545 no
S(3) F(6) 3.20(1) 4 no
S(3) F(3) 3.22(1) . no
S(3) F(4) 3.35(1) 2_545 no
F(1) H(7) 2.7391 4_554 no
F(1) H(5) 2.8864 4_454 no
F(1) C(7) 3.31(2) 4_454 no
F(1) C(6) 3.37(2) 4_454 no
F(1) C(11) 3.54(2) 4_554 no
F(2) H(9) 2.7055 2_455 no
F(2) F(10) 3.24(2) . no
F(2) C(13) 3.44(2) 2_455 no
F(2) C(1) 3.45(2) 2 no
F(2) C(12) 3.57(2) 2_455 no
F(2) C(8) 3.58(2) 2 no
F(3) H(2) 2.4594 1_455 no
F(3) C(8) 3.04(1) . no
F(3) C(4) 3.32(2) 1_455 no
F(3) F(9) 3.36(2) 4_454 no
F(3) C(1) 3.41(2) . no
F(4) H(8) 2.4371 4_554 no
F(4) C(8) 3.08(2) 2 no
F(4) C(9) 3.15(2) 2 no
F(4) C(12) 3.24(2) 4_554 no
F(4) F(6) 3.44(2) 3_565 no
F(4) C(11) 3.44(2) 4_554 no
F(4) C(10) 3.50(2) 2 no
F(5) C(2) 3.21(2) . no
F(5) C(1) 3.28(2) . no
F(5) C(14) 3.33(2) 2 no
F(5) C(7) 3.42(2) . no
F(5) C(8) 3.45(2) 2 no
F(5) C(9) 3.57(2) 2 no
F(6) F(12) 3.12(2) 4_454 no
F(7) H(5) 2.3816 . no
F(7) C(7) 3.14(2) . no
F(7) F(11) 3.47(3) 3_666 no
F(8) H(1) 2.5101 4_455 no
F(8) F(8) 3.13(3) 3_566 no
F(8) C(3) 3.47(2) 4_455 no
F(8) F(11) 3.51(2) 3_566 no
F(9) H(10) 2.5363 4 no
F(9) H(2) 2.8720 4_455 no
F(9) H(1) 2.9761 4_455 no
F(9) C(14) 3.02(2) 4 no
F(9) C(4) 3.47(2) 4_455 no
F(9) C(9) 3.48(2) 4 no
F(9) C(8) 3.51(2) 4 no
F(9) C(3) 3.54(2) 4_455 no
F(10) H(3) 2.3560 1_455 no
F(10) C(5) 3.30(3) 1_455 no
F(11) H(4) 2.6104 3_666 no
F(11) C(6) 3.50(2) 3_666 no
F(12) H(6) 2.3432 . no
F(12) H(1) 2.7943 4_455 no
F(12) H(2) 2.8456 4_455 no
F(12) C(10) 3.25(2) . no
F(12) C(3) 3.43(2) 4_455 no
F(12) C(4) 3.44(3) 4_455 no
C(4) H(9) 3.0559 2 no
C(5) H(9) 2.9030 2 no
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
_geom_torsion_publ_flag
S(1) S(2) C(8) S(3) 0.7(8) no
S(1) S(2) C(8) C(9) -179(1) no
S(1) C(1) S(3) C(8) -3.6(9) no
S(1) C(1) C(2) C(3) -2(2) no
S(1) C(1) C(2) C(7) 178(1) no
S(2) S(1) C(1) S(3) 3.9(8) no
S(2) S(1) C(1) C(2) -179(1) no
S(2) C(8) S(3) C(1) 1.4(9) no
S(2) C(8) C(9) C(10) -172(1) no
S(2) C(8) C(9) C(14) 6(2) no
S(3) C(1) C(2) C(3) 176(1) no
S(3) C(1) C(2) C(7) -5(2) no
S(3) C(8) C(9) C(10) 8(2) no
S(3) C(8) C(9) C(14) -174(1) no
C(1) S(1) S(2) C(8) -2.5(6) no
C(1) S(3) C(8) C(9) -179(1) no
C(1) C(2) C(3) C(4) -180(2) no
C(1) C(2) C(7) C(6) 180(1) no
C(2) C(1) S(3) C(8) 179(1) no
C(2) C(3) C(4) C(5) -0(3) no
C(2) C(7) C(6) C(5) -0(3) no
C(3) C(2) C(7) C(6) -1(2) no
C(3) C(4) C(5) C(6) -0(3) no
C(4) C(3) C(2) C(7) 1(3) no
C(4) C(5) C(6) C(7) 1(3) no
C(8) C(9) C(10) C(11) 179(1) no
C(8) C(9) C(14) C(13) -177(2) no
C(9) C(10) C(11) C(12) -1(3) no
C(9) C(14) C(13) C(12) -2(3) no
C(10) C(9) C(14) C(13) 1(3) no
C(10) C(11) C(12) C(13) -0(3) no
C(11) C(10) C(9) C(14) 0(2) no
C(11) C(12) C(13) C(14) 2(3) no
