#------------------------------------------------------------------------------
#$Date: 2016-03-21 17:18:11 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178777 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/31/4103155.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_4103155
loop_
_publ_author_name
'Matthew D. Moran'
'David S. Brock'
'Hélène P. A. Mercier'
'Gary J. Schrobilgen'
_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            'F N O3 Xe'
_chemical_formula_weight         212.31
_chemical_name_common            'F Xe O N O2'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 90.325(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.6663(4)
_cell_length_b                   8.7995(7)
_cell_length_c                   9.4153(8)
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      73
_cell_measurement_theta_min      0
_cell_volume                     386.60(6)
_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      243(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.943
_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  0.0565
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9069
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         36.33
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    8.804
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.648
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.842
_refine_diff_density_min         -2.652
_refine_diff_density_rms         0.376
_refine_ls_extinction_coef       0.0172(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   1.755
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         1780
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.755
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0133P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0807
_reflns_number_gt                1495
_reflns_number_total             1780
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja105618w_si_002_1.cif
_cod_data_source_block           FXeONO2
_cod_database_code               4103155
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Xe1 Xe 0.15697(9) 0.04186(3) 0.27774(4) 0.01024(10) Uani 1 1 d
F1 F -0.1644(10) -0.0664(4) 0.3726(4) 0.0179(7) Uani 1 1 d
N1 N 0.4824(10) 0.1829(5) 0.0422(5) 0.0105(9) Uani 1 1 d
O3 O 0.6680(10) 0.2600(5) -0.0078(4) 0.0190(9) Uani 1 1 d
O2 O 0.2814(8) 0.1239(5) -0.0210(5) 0.0158(9) Uani 1 1 d
O1 O 0.5062(9) 0.1603(4) 0.1852(4) 0.0116(8) Uani 1 1 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
Xe1 0.01284(14) 0.00965(13) 0.00821(15) 0.00080(14) -0.00154(14) -0.00085(13)
F1 0.0222(18) 0.0172(15) 0.0144(17) 0.0053(12) -0.0001(18) -0.0049(15)
N1 0.013(2) 0.0085(18) 0.010(2) -0.0005(16) -0.0043(18) 0.0025(16)
O3 0.025(2) 0.0158(18) 0.016(2) 0.0027(16) 0.002(2) -0.002(2)
O2 0.019(2) 0.0151(18) 0.014(2) -0.0027(17) -0.0071(16) -0.0013(16)
O1 0.0131(18) 0.0144(16) 0.0073(19) 0.0009(14) -0.0043(15) -0.0016(14)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
Xe Xe -0.4205 1.9578 '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
F1 Xe1 O1 177.55(15)
O3 N1 O2 127.1(5)
O3 N1 O1 114.5(4)
O2 N1 O1 118.4(5)
N1 O1 Xe1 114.7(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Xe1 F1 1.992(4)
Xe1 O1 2.126(4)
N1 O3 1.199(6)
N1 O2 1.224(6)
N1 O1 1.365(7)
