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Syntheses of Dioxygenyl Salts by Photochemical Reactions in Liquid Anhydrous Hydrogen Fluoride: X-ray Crystal Structures of α- and β-OSnF, OSnF·0.9HF, OGeF·HF, and O[Hg(HF)](SbF).

By treating gaseous, liquid, or solid fluorides with UV-photolyzed O/F mixtures and by treating solid oxides with UV-photolyzed F (or O/F mixtures) in liquid anhydrous HF at ambient temperature, we investigated the possibility of the preparation of OMF (M = B, Fe, Co, Ag), OMF (M = Ti, Sn, Pb), (O)MF (M = Ti, Ge, Sn, Pb, Pd, Ni, Mn), OMF (M = Sn), OMF (M = As, Sb, Au, Pt), OMF (M = Pt), OMF (M = Se), (O)MF (M = Mo, W), and OMF (M = I). The approach has been successful in the case of previously known OBF, OMF (M = As, Sb, Au; Pt), OGeF, and (O)(TiF). Novel compounds OGeF·HF, α-OSnF (1-D), and the HF-solvated and nonsolvated forms of β-OSnF (2-D) were synthesized and their crystal structures determined using single-crystal X-ray diffraction. The crystal structures of all of these materials arise from the condensation of octahedral MF (M = Ge, Sn) units. The anion in the crystal structure of OGeF·HF is comprised of infinite ([GeF]) chains of GeF octahedra that share common vertices. The HF molecules and O cations are located between the chains. The crystal structure of α-OSnF (1-D) is constructed from [O] cations and polymeric ([SnF]) anions which appear as two parallel infinite chains comprised of SnF units, where each SnF unit of one chain is connected to a SnF unit of the second chain through a shared fluorine vertex. The single-crystal structure determination of [O][SnF]·0.9HF reveals that it is comprised of two-dimensional ([SnF]) grids with [O] cations and HF molecules located between them. The 2-D grids have a wavelike conformation. The ([SnF]) layer contains both six- and seven-coordinated Sn(IV) atoms that are interconnected by bridging fluorine atoms. A new, more complex [O] salt, O[Hg(HF)][SbF], was prepared. In its crystal structure, the Hg atoms bridge to SbF units to form a 3-D framework. The O cations are located inside the voids while the HF molecules are bound to Hg atoms through the F atom. Attempts to prepare several chlorine analogues of O fluorine salts (i.e., OTiCl and OMCl (M = Nb, Sb)) failed.

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Discrete GeF Anion Structurally Characterized with a Readily Synthesized Imidazolium Based Naked Fluoride Reagent.

The recently prepared novel naked fluoride reagent 1,3-bis(2,6-diisopropylphenyl)imidazolium fluoride ([(L)H][F]), treated with an excess of MF (M = Si, Ge), results in isolation of [(L)H][MF] products with the elusive trigonal bipyramidal MF anions. Specific steric characteristics of the [(L)H] cation readily support isolation of monomeric and discrete trigonal bipyramidal fluorido anions of silicon and germanium. Based on combination of experimental results and DFT calculations, we demonstrate that the role of bulky cation is not solely due to steric hindering but also due to electrostatic effects, which are important in the design of such uncommon species. The discrete GeF anion was characterized by X-ray single-crystal diffraction for the first time. We report the missing F NMR entries for the discrete GeF and GeF anions in acetonitrile. All the products were also characterized by Raman spectroscopy and elemental analysis and supported by quantum-mechanical calculations.

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