#\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2012-10-10 at 17:14:20 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\cifdoc.dat # CIF files read : shelxl ir _IR #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_global #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2012-10-10 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_update_record ? #------------------ SUBMISSION DETAILS --------------------------------------# # Name and address of author for correspondence _publ_contact_author_name 'Tram\^sek, Melita' _publ_contact_author_address ; Department of Inorganic Chemistry and Technology Jozef Stefan Institute Jamova 39 1000 Ljubljana SLOVENIA ; _publ_contact_author_email 'melita.tramsek@ijs.si' _publ_contact_author_fax '386(1)4773645' _publ_contact_author_phone '386(1)4773155' _publ_requested_journal 'Acta Crystallographica C' _publ_requested_coeditor_name ? _publ_contact_letter # Include date of submission ; Date of submission ? Please consider this CIF submission for publication as a Regular Structural Paper in Acta Crystallographica C. ; _publ_requested_category ? #------------------ PROCESSING SUMMARY (JOURNAL OFFICE ONLY) ----------------# _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ? _journal_techeditor_code ? _journal_techeditor_notes ? _journal_coden_ASTM ? _journal_name_full 'Acta Chimica Slovenica' _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #------------------ TITLE AND AUTHOR LIST------------------------------------# _publ_section_title ; Oxidation of ruthenium and iridium metal by XeF2 and crystal structure determination of [Xe~2~F~3~][RuF~6~]?XeF~2~ and [Xe~2~F~3~][MF~6~] (M = Ru, Ir) ; _publ_section_title_footnote . loop_ _publ_author_name _publ_author_address _publ_author_footnote _publ_author_email 'Tram\^sek, Melita' ; Department of Inorganic Chemistry and Technology Jozef Stefan Institute Jamova 39 1000 Ljubljana SLOVENIA ; . ; melita.tramsek@ijs.si ; 'Goreshnik, Evgeny' ; Department of Inorganic Chemistry and Technology Jozef Stefan Institute Jamova 39 1000 Ljubljana SLOVENIA ; . ; evgeny.goreshnik@ijs.si ; 'Tav\J. Appl. Cryst. 37, 335--338. Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993). J. Appl. Cryst. 26, 343--350. Blessing, R. H. (1995). Acta Cryst. A51, 33--38. Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837--838. Molecular Structure Corporation. (1997--1999). TEXSAN for Windows. Single Crystal Structure Analysis Software. Version 1.06. MSC, 9009 New Trails Drive, The Woodlands, TX 77381, USA. Pennington, W. T. (reviewer) (1999). J. Appl. Cryst. 32, 1028--1029. Rigaku Corporation. (1999). CrystalClear. Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122. ; _publ_section_figure_captions ; Figure 1. View of (I) (50% probability displacement ellipsoids) ; _publ_section_acknowledgements ; ? ; _publ_section_table_legends ; Table 1. Fractional atomic coordinates and equivalent isotropic displacement parameters (\%A^2^) Table 2. Selected geometric parameters (\%A ,\% ) ; #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_shelxl _audit_creation_date 2012-10-10T17:14:20-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'F6 Ir, F3 Xe2' _chemical_formula_sum 'F9 Ir Xe2' _chemical_formula_weight 625.8 _chemical_absolute_configuration ad #------------------ UNIT CELL INFORMATION -----------------------------------# _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'C c' _symmetry_space_group_name_Hall 'C -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 14.544(3) _cell_length_b 8.0808(7) _cell_length_c 11.014(2) _cell_angle_alpha 90 _cell_angle_beta 136.954(7) _cell_angle_gamma 90 _cell_volume 883.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200 _cell_measurement_reflns_used 264 _cell_measurement_theta_min 3.1256 _cell_measurement_theta_max 27.9323 #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description Chunk _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 4.704 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 22.745 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.243 _exptl_absorpt_correction_T_max 0.702 _exptl_absorpt_process_details 'Blessing R.H., 1995' #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_measurement_device ; Mercury CCD (2x2 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_reflns_number 1874 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 28.89 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_max 0.817 _diffrn_measured_fraction_theta_full 0.946 _reflns_number_total 1129 _reflns_number_gt 1074 _reflns_threshold_expression I>2\s(I) #------------------ COMPUTER PROGRAMS USED ----------------------------------# _computing_data_collection 'CrystalClear (Rigaku Corporation, 1999)' _computing_cell_refinement 'CrystalClear (Rigaku Corporation, 1999)' _computing_data_reduction 'CrystalClear (Rigaku Corporation, 1999)' _computing_structure_solution ; SIR92 (Altomare et al., 1993), TeXsan (Molecular Structure Corporation, 1997--1999). ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ; DIAMOND (Brandenburg, K. & Berndt, M., 1999) ; _computing_publication_material ; WinGX 1.70 (Farrugia, L. J., 1999), enCIFer v.1.3 (Allen et al., 2004) ; #------------------ REFINEMENT INFORMATION ----------------------------------# _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+15.0740P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00049(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.54(3) _refine_ls_number_reflns 1129 _refine_ls_number_parameters 111 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.1031 _refine_ls_wR_factor_gt 0.0963 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.699 _refine_diff_density_min -2.329 _iucr_refine_instructions_details ; TITL Template texray.inf CELL 0.71073 14.5445 8.0808 11.0138 90.000 136.954 90.000 ZERR 4.00 0.0033 0.0007 0.0024 0.000 0.007 0.000 LATT -7 SYMM X, - Y, 1/2 + Z SFAC XE IR F UNIT 8 4 36 MERG 2 TWIN FMAP 2 PLAN 20 ACTA 50.00 L.S. 12 WGHT 0.052800 20.920799 EXTI 0.000435 BASF 0.53515 FVAR 0.96670 XE1 1 0.968035 0.334384 0.799224 11.00000 0.03375 0.03111 = 0.03374 -0.00620 0.02442 -0.00452 XE2 1 0.671660 0.654052 0.371864 11.00000 0.03327 0.03726 = 0.03240 -0.00413 0.02377 -0.00366 IR1 2 0.320432 0.623957 0.327645 11.00000 0.02804 0.03020 = 0.02868 -0.00184 0.02082 -0.00273 F1 3 0.814946 0.465955 0.557483 11.00000 0.05959 0.03024 = 0.03947 0.00044 0.02691 0.00701 F2 3 1.102510 0.211838 1.008456 11.00000 0.06692 0.07003 = 0.06675 0.00576 0.05054 0.01498 F3 3 0.539923 0.822549 0.197240 11.00000 0.03329 0.03386 = 0.04449 0.00424 0.01838 0.01603 F4 3 0.312792 0.851960 0.292583 11.00000 0.06543 0.04085 = 0.06647 0.00425 0.04897 -0.00088 F5 3 0.239114 0.644612 0.399811 11.00000 0.03676 0.06197 = 0.04419 0.00115 0.03308 -0.00180 F6 3 0.329450 0.392310 0.358863 11.00000 0.06741 0.03222 = 0.09232 0.00590 0.06663 0.00251 F7 3 0.487725 0.649603 0.565420 11.00000 0.02197 0.06493 = 0.02860 -0.00659 0.01349 -0.00525 F8 3 0.153848 0.595065 0.090603 11.00000 0.05354 0.04387 = 0.04074 -0.02036 0.02804 -0.01827 F9 3 0.407474 0.598505 0.259114 11.00000 0.06979 0.06381 = 0.05926 0.00272 0.05560 0.00380 HKLF 4 REM Template texray.inf REM R1 = 0.0397 for 1074 Fo > 4sig(Fo) and 0.0430 for all 1129 data REM 111 parameters refined using 2 restraints END ; #------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _atom_site_disorder_assembly _atom_site_disorder_group Xe1 Xe 0.96804(12) 0.3344(3) 0.79922(16) 0.0331(4) Uani 1 1 d . . . Xe2 Xe 0.67166(12) 0.6541(3) 0.37186(17) 0.0345(5) Uani 1 1 d . . . Ir1 Ir 0.32043(12) 0.62396(8) 0.32764(17) 0.0289(3) Uani 1 1 d . . . F1 F 0.815(2) 0.4660(17) 0.557(2) 0.053(4) Uani 1 1 d . . . F2 F 1.103(2) 0.212(3) 1.008(3) 0.066(6) Uani 1 1 d . . . F3 F 0.5399(16) 0.823(2) 0.197(2) 0.048(4) Uani 1 1 d . . . F4 F 0.313(2) 0.8520(17) 0.293(3) 0.057(5) Uani 1 1 d . . . F5 F 0.2391(17) 0.645(3) 0.400(2) 0.044(4) Uani 1 1 d . . . F6 F 0.329(3) 0.3923(15) 0.359(4) 0.055(5) Uani 1 1 d . . . F7 F 0.4877(16) 0.650(2) 0.565(2) 0.044(4) Uani 1 1 d . . . F8 F 0.154(2) 0.595(2) 0.091(3) 0.053(5) Uani 1 1 d . . . F9 F 0.407(2) 0.599(3) 0.259(3) 0.055(6) 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 0.0338(10) 0.0311(8) 0.0337(8) -0.0062(7) 0.0244(8) -0.0045(8) Xe2 0.0333(10) 0.0373(10) 0.0324(8) -0.0041(8) 0.0238(8) -0.0037(9) Ir1 0.0280(3) 0.0302(4) 0.0287(4) -0.0018(6) 0.0208(3) -0.0027(6) F1 0.060(9) 0.030(9) 0.039(9) 0.000(7) 0.027(8) 0.007(9) F2 0.067(13) 0.070(14) 0.067(12) 0.006(10) 0.051(11) 0.015(10) F3 0.033(7) 0.034(8) 0.044(9) 0.004(7) 0.018(7) 0.016(6) F4 0.065(10) 0.041(7) 0.066(14) 0.004(7) 0.049(12) -0.001(9) F5 0.037(8) 0.062(11) 0.044(9) 0.001(7) 0.033(8) -0.002(7) F6 0.067(9) 0.032(6) 0.092(15) 0.006(10) 0.067(12) 0.003(10) F7 0.022(7) 0.065(12) 0.029(7) -0.007(7) 0.013(6) -0.005(7) F8 0.054(10) 0.044(10) 0.041(8) -0.020(7) 0.028(8) -0.018(8) F9 0.070(12) 0.064(13) 0.059(11) 0.003(8) 0.056(10) 0.004(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Xe1 F2 1.88(2) . ? Xe1 F1 2.124(18) . ? Xe2 F3 1.959(17) . ? Xe2 F1 2.146(17) . ? Ir1 F5 1.853(17) . ? Ir1 F4 1.869(14) . ? Ir1 F8 1.870(19) . ? Ir1 F7 1.873(15) . ? Ir1 F6 1.890(12) . ? Ir1 F9 1.90(2) . ? 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 _geom_angle_publ_flag F2 Xe1 F1 178.0(8) . . ? F3 Xe2 F1 178.4(7) . . ? F5 Ir1 F4 92.3(10) . . ? F5 Ir1 F8 91.6(9) . . ? F4 Ir1 F8 90.8(9) . . ? F5 Ir1 F7 88.5(7) . . ? F4 Ir1 F7 90.0(9) . . ? F8 Ir1 F7 179.2(8) . . ? F5 Ir1 F6 89.6(10) . . ? F4 Ir1 F6 178.1(10) . . ? F8 Ir1 F6 88.7(11) . . ? F7 Ir1 F6 90.5(10) . . ? F5 Ir1 F9 178.4(9) . . ? F4 Ir1 F9 88.9(10) . . ? F8 Ir1 F9 89.5(10) . . ? F7 Ir1 F9 90.3(9) . . ? F6 Ir1 F9 89.3(10) . . ? Xe1 F1 Xe2 161.3(8) . . ?