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Issue 9, 2016
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Largest perfluorometallate [Ti10F45]5− oligomer and polymeric ([Ti3F13]) and ([TiF5]) anions prepared as [XeF5]+ salts

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Abstract

Reactions between XeF2, TiF4 and UV-irradiated elemental F2 in anhydrous HF yielded XeF5TiF5 (XeF6·TiF4), [XeF5]5[Ti10F45] (XeF6·2TiF4), and [XeF5][Ti3F13] (XeF6·3TiF4) upon crystallization. [XeF5]5[Ti10F45] crystallizes in two crystal modifications at low (α-phase, 150 K) and ambient (β-phase, 296 K) temperatures. The crystal structure determination of [XeF5]5[Ti10F45] reveals the largest known discrete decameric [Ti10F45]5− anion built from ten TiF6 octahedra, sharing vertices, in the shape of a double-star. [XeF5]+ cations are completely ordered in the α-phase, while one of three crystallographically unique [XeF5]+ cations is two-fold disordered in the β-phase. The anionic part of [XeF5][Ti3F13] is built from tetrameric Ti4F20 and octameric Ti8F36 units sharing vertices and alternatively linked into ([Ti3F13]) columns. The charge balance is maintained by [XeF5]+ cations which form secondary Xe⋯F contacts with fluorine atoms of ([Ti3F13]) groups. The main structural feature of XeF5TiF5 is an infinite chain of distorted TiF6 octahedra joined by cis vertices.

Graphical abstract: Largest perfluorometallate [Ti10F45]5− oligomer and polymeric ([Ti3F13]−)∞ and ([TiF5]−)∞ anions prepared as [XeF5]+ salts

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Publication details

The article was received on 26 Mar 2016, accepted on 31 May 2016 and first published on 01 Jun 2016


Article type: Paper
DOI: 10.1039/C6NJ00955G
Citation: New J. Chem., 2016,40, 7320-7325
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    Largest perfluorometallate [Ti10F45]5− oligomer and polymeric ([Ti3F13]) and ([TiF5]) anions prepared as [XeF5]+ salts

    Z. Mazej and E. A. Goreshnik, New J. Chem., 2016, 40, 7320
    DOI: 10.1039/C6NJ00955G

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