#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:16:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179102 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/64/4306442.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_4306442
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         'C14 H10 N3 S, As F6'
_chemical_formula_sum            'C14 H10 As F6 N3 S'
_chemical_formula_weight         441.24
_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                 110.77(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.107(2)
_cell_length_b                   12.1940(10)
_cell_length_c                   7.844(3)
_cell_measurement_reflns_used    29
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.350
_cell_measurement_theta_min      3.117
_cell_volume                     1619.4(7)
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '2θ/ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-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    0.0362
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4370
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.10
_diffrn_standards_decay_%        'random variation +/- 2.0'
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.294
_exptl_absorpt_correction_T_max  0.6306
_exptl_absorpt_correction_T_min  0.2847
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
N. Walker and D. Stuart, Acta Cryst., A39 (1983) 158-166
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.267
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         1842
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0654P)²+1.3095P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1075
_reflns_number_gt                1589
_reflns_number_total             1842
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801253f_si_002_5.cif
_cod_data_source_block           3b
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_database_code               4306442
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
N1 N 0.5000 0.1173(3) 0.2500 0.0306(7) Uani 1 2 d S . .
C1 C 0.43264(18) 0.1705(2) 0.2232(4) 0.0315(6) Uani 1 1 d . . .
N2 N 0.42471(17) 0.2826(2) 0.2140(4) 0.0376(6) Uani 1 1 d . . .
S1 S 0.5000 0.35296(8) 0.2500 0.0374(3) Uani 1 2 d S . .
C2 C 0.36131(17) 0.1074(2) 0.2003(4) 0.0336(6) Uani 1 1 d . . .
C3 C 0.3624(2) -0.0068(3) 0.1866(5) 0.0411(7) Uani 1 1 d . . .
H3 H 0.4094 -0.0434 0.1925 0.059(5) Uiso 1 1 d R . .
C4 C 0.2948(2) -0.0654(3) 0.1650(6) 0.0519(9) Uani 1 1 d . . .
H4 H 0.2953 -0.1429 0.1543 0.059(5) Uiso 1 1 d R . .
C5 C 0.2264(2) -0.0126(4) 0.1604(6) 0.0554(10) Uani 1 1 d . . .
H5 H 0.1802 -0.0538 0.1466 0.059(5) Uiso 1 1 d R . .
C6 C 0.2253(2) 0.1000(4) 0.1753(5) 0.0526(9) Uani 1 1 d . . .
H6 H 0.1782 0.1359 0.1718 0.059(5) Uiso 1 1 d R . .
C7 C 0.2919(2) 0.1608(3) 0.1941(5) 0.0438(7) Uani 1 1 d . . .
H7 H 0.2908 0.2383 0.2038 0.059(5) Uiso 1 1 d R . .
As1 As 0.0000 0.19334(3) 0.2500 0.03204(16) Uani 1 2 d S . .
F1 F -0.02113(17) 0.29125(17) 0.3811(3) 0.0623(7) Uani 1 1 d . . .
F2 F -0.02299(19) 0.09513(18) 0.3783(3) 0.0735(8) Uani 1 1 d . . .
F3 F 0.09478(15) 0.1951(3) 0.3979(4) 0.0805(9) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0282(16) 0.0278(16) 0.0352(18) 0.000 0.0105(14) 0.000
C1 0.0362(15) 0.0297(14) 0.0291(14) 0.0020(11) 0.0120(12) 0.0049(11)
N2 0.0432(15) 0.0297(13) 0.0413(15) 0.0041(10) 0.0169(12) 0.0044(10)
S1 0.0517(7) 0.0244(5) 0.0399(6) 0.000 0.0211(5) 0.000
C2 0.0291(14) 0.0370(16) 0.0335(15) 0.0017(12) 0.0098(12) 0.0021(12)
C3 0.0321(16) 0.0384(16) 0.0512(19) 0.0016(14) 0.0126(14) -0.0002(12)
C4 0.0444(19) 0.044(2) 0.066(2) -0.0015(17) 0.0173(18) -0.0080(15)
C5 0.0338(18) 0.071(3) 0.058(2) -0.0025(19) 0.0130(16) -0.0141(17)
C6 0.0309(16) 0.070(3) 0.058(2) 0.0046(19) 0.0169(16) 0.0064(16)
C7 0.0381(17) 0.0456(18) 0.049(2) 0.0030(15) 0.0175(15) 0.0084(14)
As1 0.0400(3) 0.0263(2) 0.0308(2) 0.000 0.01389(18) 0.000
F1 0.1020(19) 0.0434(11) 0.0435(12) 0.0017(9) 0.0284(13) 0.0274(11)
F2 0.137(2) 0.0382(11) 0.0658(15) 0.0019(10) 0.0619(17) -0.0127(13)
F3 0.0473(13) 0.135(3) 0.0497(15) 0.0078(14) 0.0054(11) 0.0178(14)
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'
As As 0.0499 2.0058 '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'
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'
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
C1 N1 C1 121.7(4) . 2_655 ?
N1 C1 N2 124.5(3) . . ?
N1 C1 C2 119.0(3) . . ?
N2 C1 C2 116.5(3) . . ?
C1 N2 S1 118.2(2) . . ?
N2 S1 N2 112.8(2) . 2_655 ?
C3 C2 C7 119.9(3) . . ?
C3 C2 C1 119.9(3) . . ?
C7 C2 C1 120.2(3) . . ?
C4 C3 C2 119.4(3) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C3 C4 C5 120.6(3) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.8 . . ?
C6 C5 C4 120.0(3) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 120.4(3) . . ?
C5 C6 H6 119.7 . . ?
C7 C6 H6 119.8 . . ?
C6 C7 C2 119.6(3) . . ?
C6 C7 H7 120.0 . . ?
C2 C7 H7 120.4 . . ?
F3 As1 F3 178.5(2) 2 . ?
F3 As1 F1 90.84(14) 2 . ?
F3 As1 F1 88.13(14) . . ?
F3 As1 F1 88.13(14) 2 2 ?
F3 As1 F1 90.84(14) . 2 ?
F1 As1 F1 91.15(16) . 2 ?
F3 As1 F2 90.27(15) 2 2 ?
F3 As1 F2 90.76(15) . 2 ?
F1 As1 F2 178.89(14) . 2 ?
F1 As1 F2 88.96(12) 2 2 ?
F3 As1 F2 90.76(15) 2 . ?
F3 As1 F2 90.27(15) . . ?
F1 As1 F2 88.96(12) . . ?
F1 As1 F2 178.89(14) 2 . ?
F2 As1 F2 90.96(16) 2 . ?
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
N1 C1 1.330(3) . ?
N1 C1 1.330(3) 2_655 ?
C1 N2 1.374(4) . ?
C1 C2 1.459(4) . ?
N2 S1 1.550(3) . ?
S1 N2 1.550(3) 2_655 ?
C2 C3 1.397(4) . ?
C2 C7 1.400(4) . ?
C3 C4 1.376(5) . ?
C3 H3 0.9471 . ?
C4 C5 1.386(5) . ?
C4 H4 0.9485 . ?
C5 C6 1.378(6) . ?
C5 H5 0.9491 . ?
C6 C7 1.379(5) . ?
C6 H6 0.9498 . ?
C7 H7 0.9485 . ?
As1 F3 1.697(3) 2 ?
As1 F3 1.697(3) . ?
As1 F1 1.706(2) . ?
As1 F1 1.706(2) 2 ?
As1 F2 1.708(2) 2 ?
As1 F2 1.708(2) . ?
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
C1 N1 C1 N2 2.4(2) 2_655 . . . ?
C1 N1 C1 C2 -178.1(3) 2_655 . . . ?
N1 C1 N2 S1 -4.3(4) . . . . ?
C2 C1 N2 S1 176.1(2) . . . . ?
C1 N2 S1 N2 1.98(18) . . . 2_655 ?
N1 C1 C2 C3 -7.1(4) . . . . ?
N2 C1 C2 C3 172.5(3) . . . . ?
N1 C1 C2 C7 172.2(3) . . . . ?
N2 C1 C2 C7 -8.2(4) . . . . ?
C7 C2 C3 C4 0.7(5) . . . . ?
C1 C2 C3 C4 -180.0(3) . . . . ?
C2 C3 C4 C5 -1.3(6) . . . . ?
C3 C4 C5 C6 0.8(6) . . . . ?
C4 C5 C6 C7 0.2(6) . . . . ?
C5 C6 C7 C2 -0.8(6) . . . . ?
C3 C2 C7 C6 0.3(5) . . . . ?
C1 C2 C7 C6 -179.0(3) . . . . ?
