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_4104433
_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_moiety         'F4 S N Xe, As F6'
_chemical_formula_sum            'As F10 N S Xe'
_chemical_formula_weight         442.29
_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_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 119.5490(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.9305(12)
_cell_length_b                   5.0875(3)
_cell_length_c                   14.8171(8)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52
_cell_measurement_theta_min      0
_cell_volume                     1700.45(16)
_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  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13443
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.16
_exptl_absorpt_coefficient_mu    8.293
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.455
_exptl_crystal_description       needle
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.002
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       0.00028(5)
_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   1.081
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1669
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0224
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0196P)^2^+2.6022P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0509
_refine_ls_wR_factor_ref         0.0524
_reflns_number_gt                1494
_reflns_number_total             1669
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja901187n_si_001_1.cif
_cod_data_source_block           F4SNXe+AsF6-
_cod_database_code               4104433