#\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2013-07-09 at 17:37:15 # 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 ru3_1 _Ru3_1 #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_global _publ_section_related_literature ? _publcif_datablock.id '{4c33ac4a-5a4d-4e19-9d85-6579004e640f}' # publcif _publ_body_element loop start loop_ _publ_body_element _publ_body_title _publ_body_contents section ; Introduction ; ; ; section ; Experimental ; ; ; subsection ; Synthesis and crystallization ; ; ; subsection ; Refinement ; ; Crystal data, data collection and structure refinement details are summarized in Table 1. ; section ; Results and discussion ; ; # Insert blank lines between paragraphs ? ; # publcif _publ_body_element loop end #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2013-07-09 _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 ; ? 2016-02-04 # Formatted by publCIF ; #------------------ 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 _publcif_datablock.id '{e2b99b57-d87e-4e92-9a6d-912f3fcec887}' _audit_creation_date 2013-07-09T17:37:15-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------ CHEMICAL INFORMATION ------------------------------------# _chemical_formula_moiety 'F6 Ru, F3 Xe2' _chemical_formula_sum 'F9 Ru Xe2' _chemical_formula_weight 534.67 _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 14.481(3) _cell_length_b 8.0837(8) _cell_length_c 10.952(2) _cell_angle_alpha 90 _cell_angle_beta 136.825(6) _cell_angle_gamma 90 _cell_volume 877.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200 _cell_measurement_reflns_used 890 _cell_measurement_theta_min 3.2522 _cell_measurement_theta_max 28.5637 #------------------ CRYSTAL INFORMATION -------------------------------------# _exptl_crystal_description Chunk _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 4.048 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 932 _exptl_absorpt_coefficient_mu 9.477 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.348 _exptl_absorpt_correction_T_max 0.642 _exptl_absorpt_process_details 'Blessing R.H., 1995' #------------------ DATA COLLECTION INFORMATION -----------------------------# _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_measurement_device ; Mercury CCD (2x2 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_reflns_number 1778 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 28.93 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_max 0.851 _diffrn_measured_fraction_theta_full 0.977 _reflns_number_total 1174 _reflns_number_gt 1064 _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^)+(0.0279P)^2^+9.4766P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.00169(13) _refine_ls_number_reflns 1174 _refine_ls_number_parameters 111 _refine_ls_number_restraints 2 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0849 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.38(8) _refine_diff_density_max 1.579 _refine_diff_density_min -1.236 _iucr_refine_instructions_details ; TITL Template texray.inf CELL 0.71069 14.4815 8.0837 10.9517 90.000 136.825 90.000 ZERR 4.00 0.0031 0.0008 0.0021 0.000 0.006 0.000 LATT -7 SYMM X, - Y, 1/2 + Z SFAC XE RU F UNIT 8 4 36 MERG 2 TWIN FMAP 2 PLAN 20 ACTA 50.00 L.S. 12 WGHT 0.027900 9.472199 EXTI 0.001689 BASF 0.38109 FVAR 0.83335 XE1 1 0.968395 0.334584 0.799276 11.00000 0.03610 0.03593 = 0.03438 -0.00633 0.02557 -0.00454 XE2 1 0.671148 0.654363 0.371635 11.00000 0.03341 0.03861 = 0.03364 -0.00208 0.02361 -0.00297 RU1 2 0.320646 0.622447 0.327839 11.00000 0.02926 0.03267 = 0.02932 -0.00279 0.02093 -0.00363 F1 3 0.819514 0.466912 0.561149 11.00000 0.07519 0.04355 = 0.05321 0.01354 0.04184 0.02645 F2 3 1.101909 0.205981 1.008494 11.00000 0.04186 0.06991 = 0.04965 0.01863 0.02598 0.00977 F3 3 0.538498 0.816948 0.199544 11.00000 0.05418 0.05219 = 0.06495 0.01706 0.03814 0.01682 F4 3 0.314720 0.844990 0.294317 11.00000 0.05508 0.03827 = 0.07727 0.00707 0.05380 -0.00187 F5 3 0.238918 0.646153 0.398606 11.00000 0.04585 0.05341 = 0.04434 -0.00014 0.03499 0.00855 F6 3 0.331517 0.397024 0.359482 11.00000 0.05788 0.03286 = 0.08187 0.01051 0.05477 0.00800 F7 3 0.487290 0.643503 0.561256 11.00000 0.02944 0.07962 = 0.02720 -0.00008 0.01715 -0.00097 F8 3 0.156834 0.596019 0.092803 11.00000 0.04907 0.06525 = 0.03548 -0.00605 0.02948 -0.00082 F9 3 0.405280 0.593042 0.259433 11.00000 0.06137 0.07045 = 0.04700 0.00037 0.04492 -0.00379 HKLF 4 REM Template texray.inf REM R1 = 0.0371 for 1064 Fo > 4sig(Fo) and 0.0433 for all 1174 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 Xe Xe -0.4205 1.9578 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 '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' 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 0.96839(8) 0.33458(14) 0.79928(11) 0.0356(3) Uani 1 1 d . . . Xe2 Xe 0.67115(7) 0.65436(17) 0.37164(9) 0.0361(3) Uani 1 1 d . . . Ru1 Ru 0.3206(2) 0.62245(12) 0.3278(4) 0.0309(3) Uani 1 1 d . . . F1 F 0.8195(16) 0.4669(12) 0.5611(19) 0.062(3) Uani 1 1 d . . . F2 F 1.1019(16) 0.2060(19) 1.008(2) 0.061(4) Uani 1 1 d . . . F3 F 0.5385(18) 0.8169(16) 0.200(2) 0.063(4) Uani 1 1 d . . . F4 F 0.3147(14) 0.8450(10) 0.2943(18) 0.051(3) Uani 1 1 d . . . F5 F 0.2389(14) 0.6462(14) 0.3986(19) 0.046(3) Uani 1 1 d . . . F6 F 0.3315(18) 0.3970(9) 0.359(3) 0.054(4) Uani 1 1 d . . . F7 F 0.4873(13) 0.6435(18) 0.5613(17) 0.049(4) Uani 1 1 d . . . F8 F 0.1568(14) 0.5960(19) 0.0928(18) 0.051(3) Uani 1 1 d . . . F9 F 0.4053(14) 0.5930(16) 0.2594(19) 0.054(3) 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 0.0361(9) 0.0359(6) 0.0344(7) -0.0063(5) 0.0256(7) -0.0045(5) Xe2 0.0334(8) 0.0386(6) 0.0336(6) -0.0021(6) 0.0236(7) -0.0030(5) Ru1 0.0293(5) 0.0327(5) 0.0293(5) -0.0028(9) 0.0209(4) -0.0036(9) F1 0.075(7) 0.044(7) 0.053(8) 0.014(6) 0.042(6) 0.026(7) F2 0.042(7) 0.070(8) 0.050(8) 0.019(7) 0.026(7) 0.010(7) F3 0.054(9) 0.052(7) 0.065(10) 0.017(7) 0.038(8) 0.017(6) F4 0.055(6) 0.038(4) 0.077(11) 0.007(5) 0.054(8) -0.002(5) F5 0.046(7) 0.053(7) 0.044(7) 0.000(5) 0.035(6) 0.009(5) F6 0.058(7) 0.033(4) 0.082(11) 0.011(7) 0.055(9) 0.008(6) F7 0.029(6) 0.080(9) 0.027(6) 0.000(5) 0.017(6) -0.001(5) F8 0.049(8) 0.065(8) 0.035(7) -0.006(6) 0.029(6) -0.001(6) F9 0.061(8) 0.070(8) 0.047(7) 0.000(7) 0.045(7) -0.004(7) _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 1.899(15) . ? Xe1 F1 2.096(13) . ? Xe2 F3 1.921(15) . ? Xe2 F1 2.172(12) . ? Ru1 F4 1.826(8) . ? Ru1 F5 1.837(12) . ? Ru1 F6 1.840(8) . ? Ru1 F7 1.841(13) . ? Ru1 F8 1.842(14) . ? Ru1 F9 1.860(12) . ? 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 177.2(6) . . ? F3 Xe2 F1 178.7(6) . . ? F4 Ru1 F5 91.8(5) . . ? F4 Ru1 F6 177.1(14) . . ? F5 Ru1 F6 91.0(6) . . ? F4 Ru1 F7 90.6(6) . . ? F5 Ru1 F7 90.0(6) . . ? F6 Ru1 F7 89.1(8) . . ? F4 Ru1 F8 90.5(7) . . ? F5 Ru1 F8 91.8(6) . . ? F6 Ru1 F8 89.7(8) . . ? F7 Ru1 F8 177.8(6) . . ? F4 Ru1 F9 89.6(5) . . ? F5 Ru1 F9 178.5(6) . . ? F6 Ru1 F9 87.6(6) . . ? F7 Ru1 F9 89.4(6) . . ? F8 Ru1 F9 88.7(6) . . ? Xe1 F1 Xe2 161.5(5) . . ? loop_ _publcif_info_datablock.id _publcif_info_datablock.publ_exptl _publcif_info_datablock.publ_geom _publcif_info_datablock.structure '{4c33ac4a-5a4d-4e19-9d85-6579004e640f}' ? ? ? '{e2b99b57-d87e-4e92-9a6d-912f3fcec887}' y y y loop_ _publcif_info_exptl_table_extra_item sin_theta_over_lambda_max loop_ _publcif_info_exptl_table_header_item ? _publcif_info_exptl_table_max_cols 4 _publcif_info_exptl_table_use_headnotes n loop_ _publcif_info_tables.block_id _publcif_info_tables.reference_item "{4c33ac4a-5a4d-4e19-9d85-6579004e640f}" "_publcif_info_datablock.publ_exptl" loop_ _publcif_info_cif.paper_type CE