Solid-State and Solution Rearrangements of F3S\τbNXeF+ Leading to the F4S=NXe+ Cation; Syntheses, HF Solvolyses, and Structural Characterizations of [F4S=NXe][AsF6] and [F4S=NH2][AsF6]
Gregory L. Smith; Hélène P. A. Mercier; Gary J. Schrobilgen; Journal of the American Chemical Society 131 (2009) 7272–7286; doi:10.1021/ja901187n

data_4104434
_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'
_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       '\w 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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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