Xe3OF3+, a Precursor to a Noble-Gas Nitrate; Syntheses and Structural Characterizations of FXeONO2, XeF2.HNO3, and XeF2.N2O4
Matthew D. Moran; David S. Brock; Hélène P. A. Mercier; Gary J. Schrobilgen; Journal of the American Chemical Society 132 (2010) 13823–13839; doi:10.1021/ja105618w

data_4103156
_publ_section_title
;
 Xe3OF3+, a Precursor to a Noble-Gas Nitrate; Syntheses and Structural
 Characterizations of FXeONO2, XeF2.HNO3, and XeF2.N2O4
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13823
_journal_page_last               13839
_journal_paper_doi               10.1021/ja105618w
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'F2 H N O3 Xe'
_chemical_formula_weight         232.32
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.3543(7)
_cell_length_b                   5.6539(2)
_cell_length_c                   4.7658(2)
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      85
_cell_measurement_theta_min      0
_cell_volume                     467.62(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL V6.10 2001 & Bruker-AXS'
_computing_publication_material  'SHELXTL V6.10 2001 & Bruker-AXS'
_computing_structure_refinement  'SHELXTL V6.10 2001 & Bruker-AXS'
_computing_structure_solution    'SHELXTL V6.10 2001 & Bruker-AXS'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0138
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            14132
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         42.56
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    7.323
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.675
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 v2.0-2 (Bruker, 2004)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.881
_refine_diff_density_min         -1.070
_refine_diff_density_rms         0.119
_refine_ls_extinction_coef       0.0239(7)
_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   1.302
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         1716
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.302
_refine_ls_R_factor_all          0.0160
_refine_ls_R_factor_gt           0.0140
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0135P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0311
_refine_ls_wR_factor_ref         0.0317
_reflns_number_gt                1610
_reflns_number_total             1716
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja105618w_si_002_2.cif
_cod_data_source_block           XeF2HNO3
_cod_database_code               4103156