#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:16:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179102 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/64/4306439.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_4306439
loop_
_publ_author_name
'Carsten Knapp'
'Paul G. Watson'
'Enno Lork'
'Daniel H. Friese'
'Rüdiger Mews'
'Andreas Decken'
_publ_contact_author_address
;
Institut für Anorganische und Analytische Chemie
Albert-Ludwigs Universität Freiburg
Albertstr. 21
79104 Freiburg i. Br.
Germany
;
_publ_contact_author_email       carsten.knapp@ac.uni-freiburg.de
_publ_contact_author_fax         +49-761-203-6150
_publ_contact_author_name        'Carsten Knapp'
_publ_contact_author_phone       +49-761-203-6001
_publ_section_title
;
Trithiatetrazocine Cations, [RCN4S3]+; Planar Sulfur-Nitrogen 10π
Aromatics
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10618
_journal_page_last               10625
_journal_paper_doi               10.1021/ic801253f
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C7 H3 F2 N4 S3, As F6'
_chemical_formula_sum            'C7 H3 As F8 N4 S3'
_chemical_formula_weight         466.23
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.892(7)
_cell_angle_beta                 83.377(9)
_cell_angle_gamma                66.603(9)
_cell_formula_units_Z            2
_cell_length_a                   6.6569(8)
_cell_length_b                   7.9782(7)
_cell_length_c                   14.3271(10)
_cell_measurement_reflns_used    31
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      11.42
_cell_measurement_theta_min      1.435
_cell_volume                     693.41(12)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '2θ/ω scans'
_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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6418
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.78
_diffrn_standards_decay_%        'random varaition +/-2.0'
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.996
_exptl_absorpt_correction_T_max  0.3004
_exptl_absorpt_correction_T_min  0.2105
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
N. Walker and D. Stuart, Acta Cryst., A39 (1983) 158-166
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       0.0171(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         3190
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0255
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0256P)²+0.4351P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0690
_reflns_number_gt                2960
_reflns_number_total             3190
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801253f_si_002_2.cif
_cod_data_source_block           2c
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'refdelF' changed to
'refdelf' according to
'/home/saulius/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 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        693.41(11)
_cod_database_code               4306439
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
C1 C 0.2241(3) 0.2432(3) 0.69258(14) 0.0224(4) Uani 1 1 d . . .
N1 N 0.0408(3) 0.3209(3) 0.74809(12) 0.0262(4) Uani 1 1 d . . .
S1 S -0.05416(9) 0.36578(8) 0.85087(4) 0.02857(13) Uani 1 1 d . . .
N2 N 0.0911(3) 0.3266(3) 0.93400(12) 0.0282(4) Uani 1 1 d . . .
S2 S 0.32604(10) 0.24941(8) 0.96800(4) 0.03125(14) Uani 1 1 d . . .
N3 N 0.5275(3) 0.1547(3) 0.89439(13) 0.0290(4) Uani 1 1 d . . .
S3 S 0.59382(9) 0.10319(8) 0.78819(4) 0.02729(13) Uani 1 1 d . . .
N4 N 0.4293(3) 0.1585(3) 0.71382(12) 0.0248(4) Uani 1 1 d . . .
C2 C 0.1947(3) 0.2509(3) 0.59079(14) 0.0246(4) Uani 1 1 d . . .
C3 C 0.0285(4) 0.2148(3) 0.55786(15) 0.0294(5) Uani 1 1 d . . .
F1 F -0.1060(2) 0.1673(2) 0.62050(10) 0.0413(4) Uani 1 1 d . . .
C4 C 0.0003(4) 0.2214(3) 0.46328(16) 0.0358(5) Uani 1 1 d . . .
H4 H -0.1148 0.1952 0.4429 0.055(5) Uiso 1 1 calc R . .
C5 C 0.1435(5) 0.2669(4) 0.39912(16) 0.0381(6) Uani 1 1 d . . .
H5 H 0.1273 0.2706 0.3339 0.055(5) Uiso 1 1 calc R . .
C6 C 0.3095(5) 0.3069(4) 0.42808(17) 0.0414(6) Uani 1 1 d . . .
H6 H 0.4061 0.3399 0.3838 0.055(5) Uiso 1 1 calc R . .
C7 C 0.3316(4) 0.2979(3) 0.52295(16) 0.0341(5) Uani 1 1 d . . .
F2 F 0.4879(3) 0.3436(3) 0.55220(11) 0.0534(5) Uani 1 1 d . . .
As1 As 0.72802(3) 0.25686(3) 0.170479(13) 0.02099(8) Uani 1 1 d . . .
F3 F 0.6660(3) 0.3575(2) 0.06200(10) 0.0416(4) Uani 1 1 d . . .
F4 F 0.7944(3) 0.0463(2) 0.12524(12) 0.0523(4) Uani 1 1 d . . .
F5 F 0.7876(3) 0.1563(2) 0.27850(10) 0.0438(4) Uani 1 1 d . . .
F6 F 0.6576(3) 0.4679(2) 0.21574(12) 0.0546(5) Uani 1 1 d . . .
F7 F 0.9932(2) 0.2389(2) 0.14592(11) 0.0467(4) Uani 1 1 d . . .
F8 F 0.4616(2) 0.2758(2) 0.19561(11) 0.0442(4) Uani 1 1 d . . .
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'
F F 0.0171 0.0103 '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'
As As 0.0499 2.0058 '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
N4 C1 N1 129.90(19) . . ?
N4 C1 C2 115.00(18) . . ?
N1 C1 C2 115.10(18) . . ?
C1 N1 S1 144.23(16) . . ?
N1 S1 N2 123.41(10) . . ?
S1 N2 S2 148.09(13) . . ?
N2 S2 N3 118.21(10) . . ?
S2 N3 S3 143.39(13) . . ?
N4 S3 N3 123.62(10) . . ?
C1 N4 S3 148.66(16) . . ?
C3 C2 C7 116.0(2) . . ?
C3 C2 C1 122.5(2) . . ?
C7 C2 C1 121.5(2) . . ?
F1 C3 C4 119.0(2) . . ?
F1 C3 C2 118.14(19) . . ?
C4 C3 C2 122.8(2) . . ?
C5 C4 C3 118.4(2) . . ?
C5 C4 H4 120.8 . . ?
C3 C4 H4 120.8 . . ?
C6 C5 C4 121.2(2) . . ?
C6 C5 H5 119.4 . . ?
C4 C5 H5 119.4 . . ?
C7 C6 C5 118.3(2) . . ?
C7 C6 H6 120.9 . . ?
C5 C6 H6 120.9 . . ?
F2 C7 C6 118.7(2) . . ?
F2 C7 C2 118.0(2) . . ?
C6 C7 C2 123.3(2) . . ?
F5 As1 F7 90.22(8) . . ?
F5 As1 F6 90.46(8) . . ?
F7 As1 F6 89.77(9) . . ?
F5 As1 F3 179.47(7) . . ?
F7 As1 F3 90.28(8) . . ?
F6 As1 F3 89.70(8) . . ?
F5 As1 F4 89.71(9) . . ?
F7 As1 F4 91.07(9) . . ?
F6 As1 F4 179.14(9) . . ?
F3 As1 F4 90.12(8) . . ?
F5 As1 F8 89.65(8) . . ?
F7 As1 F8 179.67(9) . . ?
F6 As1 F8 89.93(9) . . ?
F3 As1 F8 89.84(8) . . ?
F4 As1 F8 89.23(9) . . ?
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
C1 N4 1.322(3) . ?
C1 N1 1.323(3) . ?
C1 C2 1.487(3) . ?
N1 S1 1.5419(18) . ?
S1 N2 1.5570(19) . ?
N2 S2 1.559(2) . ?
S2 N3 1.570(2) . ?
N3 S3 1.5716(19) . ?
S3 N4 1.5322(18) . ?
C2 C3 1.386(3) . ?
C2 C7 1.390(3) . ?
C3 F1 1.337(3) . ?
C3 C4 1.384(3) . ?
C4 C5 1.382(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.379(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.378(3) . ?
C6 H6 0.9500 . ?
C7 F2 1.347(3) . ?
As1 F5 1.7049(14) . ?
As1 F7 1.7101(15) . ?
As1 F6 1.7133(15) . ?
As1 F3 1.7137(13) . ?
As1 F4 1.7141(15) . ?
As1 F8 1.7167(15) . ?
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N4 C1 N1 S1 1.4(5) . . . . ?
C2 C1 N1 S1 -179.2(2) . . . . ?
C1 N1 S1 N2 5.0(4) . . . . ?
N1 S1 N2 S2 -0.9(3) . . . . ?
S1 N2 S2 N3 -4.6(3) . . . . ?
N2 S2 N3 S3 1.1(3) . . . . ?
S2 N3 S3 N4 4.0(3) . . . . ?
N1 C1 N4 S3 -6.3(5) . . . . ?
C2 C1 N4 S3 174.3(3) . . . . ?
N3 S3 N4 C1 0.3(4) . . . . ?
N4 C1 C2 C3 135.5(2) . . . . ?
N1 C1 C2 C3 -43.9(3) . . . . ?
N4 C1 C2 C7 -45.5(3) . . . . ?
N1 C1 C2 C7 135.0(2) . . . . ?
C7 C2 C3 F1 179.3(2) . . . . ?
C1 C2 C3 F1 -1.7(3) . . . . ?
C7 C2 C3 C4 1.1(3) . . . . ?
C1 C2 C3 C4 -179.9(2) . . . . ?
F1 C3 C4 C5 -178.6(2) . . . . ?
C2 C3 C4 C5 -0.4(4) . . . . ?
C3 C4 C5 C6 -0.7(4) . . . . ?
C4 C5 C6 C7 1.0(4) . . . . ?
C5 C6 C7 F2 -177.5(2) . . . . ?
C5 C6 C7 C2 -0.2(4) . . . . ?
C3 C2 C7 F2 176.5(2) . . . . ?
C1 C2 C7 F2 -2.5(3) . . . . ?
C3 C2 C7 C6 -0.9(4) . . . . ?
C1 C2 C7 C6 -179.8(2) . . . . ?
