#------------------------------------------------------------------------------ #$Date: 2016-03-21 17:18:11 +0200 (Mon, 21 Mar 2016) $ #$Revision: 178777 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/10/31/4103157.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_4103157 loop_ _publ_author_name 'Matthew D. Moran' 'David S. Brock' 'H\'el\`ene 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 'F2 N2 O4 Xe' _chemical_formula_weight 261.32 _chemical_name_common 'Xe F2 N2 O4' _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_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 79.170(7) _cell_angle_beta 88.454(5) _cell_angle_gamma 81.083(5) _cell_formula_units_Z 1 _cell_length_a 4.5822(3) _cell_length_b 5.0597(3) _cell_length_c 6.2761(5) _cell_measurement_temperature 243(2) _cell_measurement_theta_max 66 _cell_measurement_theta_min 0 _cell_volume 141.189(17) _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 0.986 _diffrn_measured_fraction_theta_max 0.822 _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 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0558 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 2267 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 32.99 _diffrn_reflns_theta_min 4.15 _exptl_absorpt_coefficient_mu 6.100 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.605 _exptl_absorpt_correction_type sphere _exptl_absorpt_process_details 'SADABS V2.10' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 3.073 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plates _exptl_crystal_F_000 118 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _refine_diff_density_max 1.382 _refine_diff_density_min -1.349 _refine_diff_density_rms 0.300 _refine_ls_extinction_coef 0.004(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 1.066 _refine_ls_matrix_type full _refine_ls_number_parameters 44 _refine_ls_number_reflns 870 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.066 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0385 _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^)+(0.0446P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0725 _refine_ls_wR_factor_ref 0.0742 _reflns_number_gt 847 _reflns_number_total 870 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ja105618w_si_002_3.cif _cod_data_source_block XeF2N2O4 _cod_database_code 4103157 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 Xe1 Xe 0.0000 0.0000 0.0000 0.0123(2) Uani 1 2 d S F1 F -0.2893(7) -0.2301(6) 0.1430(5) 0.0234(7) Uani 1 1 d . O1 O 0.7203(8) 0.2012(7) 0.4683(6) 0.0208(8) Uani 1 1 d . O2 O 0.2952(9) 0.3921(8) 0.3168(6) 0.0225(8) Uani 1 1 d . N1 N 0.5043(9) 0.3675(8) 0.4292(6) 0.0147(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 0.0112(3) 0.0163(3) 0.0091(2) 0.00238(13) 0.00045(13) -0.00663(15) F1 0.0207(15) 0.0298(16) 0.0189(15) 0.0051(11) 0.0034(12) -0.0138(12) O1 0.0222(19) 0.0145(16) 0.0241(19) -0.0026(13) 0.0035(15) 0.0001(14) O2 0.026(2) 0.0193(17) 0.0225(18) -0.0009(13) -0.0040(15) -0.0095(15) N1 0.018(2) 0.0124(18) 0.0133(18) 0.0003(13) -0.0010(15) -0.0043(15) 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 F1 Xe1 F1 180.00(15) 2 . O2 N1 O1 134.5(5) . . O2 N1 N1 113.0(4) . 2_666 O1 N1 N1 112.5(4) . 2_666 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Xe1 F1 1.985(3) 2 Xe1 F1 1.985(3) . O1 N1 1.194(6) . O2 N1 1.182(6) . N1 N1 1.738(8) 2_666