#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:41:47 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178790 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/44/4104434.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_4104434
loop_
_publ_author_name
'Gregory L. Smith'
'Hélène P. A. Mercier'
'Gary J. Schrobilgen'
_publ_section_title
;
 Solid-State and Solution Rearrangements of F3S\\tbNXeF+ Leading to the
 F4S=NXe+ Cation; Syntheses, HF Solvolyses, and Structural
 Characterizations of [F4S=NXe][AsF6] and [F4S=NH2][AsF6]
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7272
_journal_page_last               7286
_journal_paper_doi               10.1021/ja901187n
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'As F10 H2 N S'
_chemical_formula_weight         313.01
_chemical_name_common            'F4 S N H2, As F6'
_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                89.484(9)
_cell_angle_beta                 87.479(7)
_cell_angle_gamma                74.955(7)
_cell_formula_units_Z            2
_cell_length_a                   5.4447(6)
_cell_length_b                   6.6457(7)
_cell_length_c                   10.3063(11)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64
_cell_measurement_theta_min      0
_cell_volume                     359.79(7)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '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  0.0660
_diffrn_reflns_av_sigmaI/netI    0.1167
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5841
_diffrn_reflns_theta_full        32.00
_diffrn_reflns_theta_max         32.00
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    5.163
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.889
_exptl_crystal_description       blade
_exptl_crystal_F_000             296
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.835
_refine_diff_density_min         -1.961
_refine_diff_density_rms         0.309
_refine_ls_extinction_coef       0.167(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.418
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         2341
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.417
_refine_ls_R_factor_all          0.1335
_refine_ls_R_factor_gt           0.0855
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0600P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1623
_refine_ls_wR_factor_ref         0.1725
_reflns_number_gt                1588
_reflns_number_total             2341
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja901187n_si_001_2.cif
_cod_data_source_block           F4SNH2+AsF6-
_cod_database_code               4104434
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
As1 As 0.0000 0.0000 0.5000 0.0131(3) Uani 1 2 d S
F5 F -0.1294(10) -0.1351(7) 0.6134(5) 0.0239(11) Uani 1 1 d .
F6 F 0.2966(8) -0.0888(7) 0.5637(5) 0.0237(11) Uani 1 1 d .
F7 F -0.0649(9) 0.2110(7) 0.6014(4) 0.0214(11) Uani 1 1 d .
As2 As 0.0000 0.0000 1.0000 0.0116(3) Uani 1 2 d S
F8 F 0.2176(9) -0.1252(7) 0.8842(5) 0.0207(10) Uani 1 1 d .
F9 F 0.0677(9) -0.2206(7) 1.0937(4) 0.0187(10) Uani 1 1 d .
F10 F 0.2375(9) 0.0832(7) 1.0718(5) 0.0207(10) Uani 1 1 d .
S1 S 0.3680(4) 0.4036(3) 0.74923(18) 0.0139(4) Uani 1 1 d .
F1 F 0.3312(10) 0.4186(7) 0.5995(4) 0.0242(11) Uani 1 1 d .
F2 F 0.0973(9) 0.5341(7) 0.7701(5) 0.0232(11) Uani 1 1 d .
F3 F 0.5420(8) 0.5496(7) 0.7326(5) 0.0227(11) Uani 1 1 d .
F4 F 0.3992(9) 0.4076(7) 0.8986(4) 0.0216(11) Uani 1 1 d .
N1 N 0.4497(12) 0.1683(10) 0.7459(6) 0.0149(13) Uani 1 1 d D
H1A H 0.405(16) 0.127(9) 0.658(3) 0.018 Uiso 1 1 d D
H1B H 0.482(17) 0.067(7) 0.821(4) 0.018 Uiso 1 1 d 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
As1 0.0134(6) 0.0139(6) 0.0100(6) -0.0023(4) -0.0022(4) 0.0001(4)
F5 0.029(3) 0.024(3) 0.018(2) -0.0006(19) 0.006(2) -0.007(2)
F6 0.011(2) 0.025(3) 0.032(3) -0.011(2) -0.0082(19) 0.0032(19)
F7 0.022(3) 0.022(2) 0.018(2) -0.0084(18) -0.0041(19) -0.002(2)
As2 0.0106(6) 0.0136(6) 0.0096(5) 0.0022(4) -0.0018(4) -0.0009(4)
F8 0.015(2) 0.019(2) 0.024(3) 0.0008(18) 0.0048(19) 0.0023(19)
F9 0.020(2) 0.015(2) 0.020(2) 0.0042(17) -0.0057(19) -0.0014(19)
F10 0.020(2) 0.025(3) 0.020(2) 0.0020(18) -0.0087(18) -0.010(2)
S1 0.0111(9) 0.0162(9) 0.0137(9) 0.0001(6) -0.0014(6) -0.0023(7)
F1 0.035(3) 0.024(3) 0.013(2) 0.0054(18) -0.009(2) -0.005(2)
F2 0.013(2) 0.019(2) 0.035(3) 0.001(2) -0.006(2) 0.0014(19)
F3 0.007(2) 0.025(3) 0.038(3) 0.000(2) -0.002(2) -0.0064(19)
F4 0.026(3) 0.026(3) 0.010(2) -0.0037(18) -0.0048(18) 0.000(2)
N1 0.015(3) 0.013(3) 0.016(3) 0.001(2) -0.001(2) -0.001(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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
F5 As1 F5 180.000(1) . 2_556
F5 As1 F7 89.9(2) . 2_556
F5 As1 F7 90.1(2) 2_556 2_556
F5 As1 F7 90.1(2) . .
F5 As1 F7 89.9(2) 2_556 .
F7 As1 F7 180.000(1) 2_556 .
F5 As1 F6 88.9(3) . 2_556
F5 As1 F6 91.1(3) 2_556 2_556
F7 As1 F6 90.0(2) 2_556 2_556
F7 As1 F6 90.0(2) . 2_556
F5 As1 F6 91.1(3) . .
F5 As1 F6 88.9(3) 2_556 .
F7 As1 F6 90.0(2) 2_556 .
F7 As1 F6 90.0(2) . .
F6 As1 F6 180.000(1) 2_556 .
F8 As2 F8 180.000(2) . 2_557
F8 As2 F9 89.7(2) . .
F8 As2 F9 90.3(2) 2_557 .
F8 As2 F9 90.3(2) . 2_557
F8 As2 F9 89.7(2) 2_557 2_557
F9 As2 F9 180.000(1) . 2_557
F8 As2 F10 90.8(2) . 2_557
F8 As2 F10 89.2(2) 2_557 2_557
F9 As2 F10 90.1(2) . 2_557
F9 As2 F10 89.9(2) 2_557 2_557
F8 As2 F10 89.2(2) . .
F8 As2 F10 90.8(2) 2_557 .
F9 As2 F10 89.9(2) . .
F9 As2 F10 90.1(2) 2_557 .
F10 As2 F10 180.000(1) 2_557 .
F2 S1 N1 125.2(3) . .
F2 S1 F3 108.5(3) . .
N1 S1 F3 126.3(3) . .
F2 S1 F4 88.9(3) . .
N1 S1 F4 91.9(3) . .
F3 S1 F4 88.9(3) . .
F2 S1 F1 88.7(3) . .
N1 S1 F1 92.6(3) . .
F3 S1 F1 88.3(3) . .
F4 S1 F1 175.5(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
As1 F5 1.705(5) .
As1 F5 1.705(5) 2_556
As1 F7 1.709(4) 2_556
As1 F7 1.709(4) .
As1 F6 1.726(4) 2_556
As1 F6 1.726(4) .
As2 F8 1.704(4) .
As2 F8 1.704(4) 2_557
As2 F9 1.716(5) .
As2 F9 1.716(5) 2_557
As2 F10 1.729(4) 2_557
As2 F10 1.729(4) .
S1 F2 1.511(5) .
S1 N1 1.511(6) .
S1 F3 1.526(5) .
S1 F4 1.558(5) .
S1 F1 1.564(5) .
