#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:16:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179102 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/64/4306441.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_4306441
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 H4 F N4 S3,  As F6'
_chemical_formula_sum            'C7 H4 As F7 N4 S3'
_chemical_formula_weight         448.24
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                83.467(1)
_cell_angle_beta                 84.680(1)
_cell_angle_gamma                66.607(1)
_cell_formula_units_Z            2
_cell_length_a                   6.5240(5)
_cell_length_b                   7.9184(7)
_cell_length_c                   14.3798(12)
_cell_measurement_reflns_used    3516
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.81
_cell_volume                     676.45(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(1)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker AXS SMART1000/P4'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0151
_diffrn_reflns_av_sigmaI/netI    0.0216
_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       -17
_diffrn_reflns_number            4743
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.43
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              K760
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.057
_exptl_absorpt_correction_T_max  0.734706
_exptl_absorpt_correction_T_min  0.427868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997b)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.173
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2952
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0511P)²+0.9060P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0898
_reflns_number_gt                2798
_reflns_number_total             2952
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic801253f_si_002_4.cif
_cod_data_source_block           2e
_cod_database_code               4306441
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 0.2887(4) 0.7416(4) 0.81210(18) 0.0202(5) Uani 1 1 d . . .
N1 N 0.0789(4) 0.8149(3) 0.78602(16) 0.0225(5) Uani 1 1 d . . .
S1 S -0.08569(11) 0.86643(10) 0.70794(5) 0.02331(16) Uani 1 1 d . . .
N2 N -0.0137(4) 0.8269(3) 0.60274(17) 0.0241(5) Uani 1 1 d . . .
S2 S 0.19318(12) 0.74115(10) 0.53278(5) 0.02603(17) Uani 1 1 d . . .
N3 N 0.4299(4) 0.6564(3) 0.57326(16) 0.0235(5) Uani 1 1 d . . .
S3 S 0.57353(11) 0.61350(10) 0.66052(5) 0.02413(16) Uani 1 1 d . . .
N4 N 0.4743(4) 0.6637(3) 0.76007(16) 0.0223(5) Uani 1 1 d . . .
C2 C 0.3136(5) 0.7469(4) 0.91283(19) 0.0228(5) Uani 1 1 d . . .
C3 C 0.4968(6) 0.7552(5) 0.9478(2) 0.0373(7) Uani 1 1 d . . .
C4 C 0.5142(7) 0.7628(6) 1.0420(2) 0.0462(9) Uani 1 1 d . . .
H4 H 0.6440 0.7700 1.0633 0.055 Uiso 1 1 calc R . .
C5 C 0.3455(6) 0.7602(5) 1.1043(2) 0.0336(7) Uani 1 1 d . . .
H5 H 0.3569 0.7646 1.1693 0.040 Uiso 1 1 calc R . .
C6 C 0.1581(7) 0.7512(7) 1.0726(3) 0.0563(12) Uani 1 1 d . . .
H6 H 0.0393 0.7496 1.1157 0.068 Uiso 1 1 calc R . .
C7 C 0.1421(6) 0.7443(7) 0.9782(2) 0.0515(11) Uani 1 1 d . . .
H7 H 0.0119 0.7377 0.9572 0.062 Uiso 1 1 calc R . .
F1 F 0.6737(5) 0.7483(6) 0.88888(18) 0.0986(13) Uani 1 1 d . . .
As As 0.75655(4) 0.76465(3) 0.329228(17) 0.01799(10) Uani 1 1 d . . .
F2 F 0.8467(3) 0.6407(3) 0.43372(13) 0.0360(4) Uani 1 1 d . . .
F3 F 0.6676(3) 0.8889(3) 0.22449(12) 0.0332(4) Uani 1 1 d . . .
F4 F 0.8269(4) 0.5616(3) 0.27766(15) 0.0426(5) Uani 1 1 d . . .
F5 F 0.4933(3) 0.7678(3) 0.35661(14) 0.0372(4) Uani 1 1 d . . .
F6 F 0.6869(4) 0.9676(3) 0.38007(15) 0.0425(5) Uani 1 1 d . . .
F7 F 1.0196(3) 0.7611(3) 0.30058(15) 0.0389(5) 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'
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'
H H 0.0000 0.0000 '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 128.4(2) . . ?
N4 C1 C2 116.9(2) . . ?
N1 C1 C2 114.7(2) . . ?
C1 N1 S1 149.0(2) . . ?
N1 S1 N2 124.02(13) . . ?
S1 N2 S2 143.87(16) . . ?
N3 S2 N2 117.71(13) . . ?
S2 N3 S3 147.84(17) . . ?
N4 S3 N3 123.84(13) . . ?
C1 N4 S3 145.3(2) . . ?
C3 C2 C7 116.3(3) . . ?
C3 C2 C1 124.0(3) . . ?
C7 C2 C1 119.7(3) . . ?
F1 C3 C2 119.2(3) . . ?
F1 C3 C4 117.9(3) . . ?
C2 C3 C4 122.8(3) . . ?
C5 C4 C3 119.9(3) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 119.5(3) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
C5 C6 C7 120.1(3) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C6 C7 C2 121.4(3) . . ?
C6 C7 H7 119.3 . . ?
C2 C7 H7 119.3 . . ?
F2 As F3 179.70(8) . . ?
F2 As F5 90.49(9) . . ?
F3 As F5 89.81(9) . . ?
F2 As F7 90.00(9) . . ?
F3 As F7 89.70(9) . . ?
F5 As F7 179.37(9) . . ?
F2 As F6 90.48(10) . . ?
F3 As F6 89.49(10) . . ?
F5 As F6 90.98(11) . . ?
F7 As F6 89.41(11) . . ?
F2 As F4 89.78(10) . . ?
F3 As F4 90.25(10) . . ?
F5 As F4 89.21(11) . . ?
F7 As F4 90.40(11) . . ?
F6 As F4 179.68(10) . . ?
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 1.323(4) . ?
C1 N1 1.329(3) . ?
C1 C2 1.480(4) . ?
N1 S1 1.533(2) . ?
S1 N2 1.570(2) . ?
N2 S2 1.572(3) . ?
S2 N3 1.559(3) . ?
N3 S3 1.561(2) . ?
S3 N4 1.543(2) . ?
C2 C3 1.366(4) . ?
C2 C7 1.398(4) . ?
C3 F1 1.354(4) . ?
C3 C4 1.380(5) . ?
C4 C5 1.359(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.374(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.379(5) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
As F2 1.7138(17) . ?
As F3 1.7159(17) . ?
As F5 1.7168(18) . ?
As F7 1.7171(18) . ?
As F6 1.7176(18) . ?
As F4 1.7226(18) . ?
