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Chapter 13 Noble-Gas Chemistry CHAPTER 13 NOBLE-GAS CHEMISTRY Wojciech Grochala ICM, University of Warsaw, Pawińskiego 5a, 02106 Warsaw Poland and Faculty of Chemistry, University of Warsaw, Pasteur 1, 02093 Warsaw Poland E-mail: [email protected] Leonid Khriachtchev and Markku Räsänen Department of Chemistry, P.O. Box 55, FIN-00014 University of Helsinki, Finland E-mails: [email protected]; [email protected] Noble-gas chemistry was started in 1962 with the discovery of xenon hexafluoroplatinate followed with a number of compounds binding xenon or krypton. We highlight the classical and more exotic noble-gas compounds and discuss the nature of their bonding starting with strongly bound systems and progressing to weak interactions. Noble-gas hydrides with the common formula HNgY were found in 1995, which led later to the identification of the first argon compound HArF. The formation mechanism of noble-gas hydrides at low temperatures is described in detail followed with a model of bonding. The interactions of the noble- gas hydrides with their surroundings and with complexing molecules are discussed. The chapter ends with known and potential applications of noble gases and with challenges encountered. 1. Introduction The chemistry of noble gases began with a room temperature synthesis of the first xenon compound in the solid state, xenon hexafluoroplatinate 1 (XePtF6 ) by Neil Bartlett. The true and indeed very complex nature of the “XePtF6” compound was confirmed by experiments conducted nearly chapter 13.indd 419 1/27/2011 8:57:08 PM 420 W. Grochala, L. Khriachtchev, and M. Räsänen 40 years after the initial preparation.2 The history of the breaking of the inertness of the noble gases is certainly complex and fascinating, full of many misleading reports, surprises, and ingenuity.3 The chemical bonds between noble gas and other atoms are usually quite fragile due to various redox (electron-transfer) reactions. In consequence of that, the exploration of noble-gas chemistry constitutes a very good probe of the capabilities offered by low-temperature experimental techniques and also serves as an important incentive for their development. Low- temperature solid hosts have shown to be excellent to synthesize and identify novel species. For noble-gas containing species, soon after the breakthrough of Neil Bartlett, matrix isolation methods were applied to 4,5 produce noble-gas halides like KrF2, XeCl2, and XeClF. Matrix photolysis and thermal annealing of different small hydrides resulted in a puzzle by producing extremely strong unidentified absorptions in the mid-IR region. One characteristic example was the photolysis of HCl in Kr and Xe matrices.6 The first suggestion on the structure of these species came from the diatomics-in-ionic-systems (DIIS) simulation of 7 the HCl–Xen system made by Last and George. They have found that a charge-transfer structure of HXeCl appears to be stable. Such a structure was then verified by quantum chemical calculations, and a number of noble-gas hydrides of the common structure HNgY, where Ng = Ar, Kr, or Xe and Y is an electronegative atom or fragment, were predicted and experimentally characterized. The latest member of this family of molecules is doubly “xenonated” water, HXeOXeH.8 By the year 2009, the number of these molecules amounts 23 (see Table 1), including the first neutral chemical compound of argon, HArF.9 In this chapter on noble-gas chemistry, we present our understanding of the properties of noble-gas compounds made at ambient or cryogenic temperatures and describe some interesting predictions and challenges. As a shining example, we discuss in detail the noble-gas hydrides, their synthesis, properties, and complexation with other molecules in low- temperature matrices. Physics & Chemistry low temp Tact/11/PAN/001 Physics & Chemistry low temp Tact/11/PAN/001 chapter 13.indd 420 1/27/2011 8:57:08 PM Noble-Gas Chemistry 421 Table 1. Experimentally identified noble-gas hydride molecules by the year 2009. HXeH HXeI HXeBr HKrCl HXeCl HArF HKrF HKrCN HXeCN HXeNC HXeOH HXeO HXeOXeH HXeSH HXeNCO HKrCCH HXeCCH HKrCCCN HXeCCCN HXeCCXeH HXeCC HKrCCCCH HXeCCCCH 2. Noble-Gas Chemistry from Cryogenic to Ambient Temperatures 2.1. The ambient temperature regime: “Classical” noble-gas compounds and the nature of chemical bonding The seminal 1962 discoveries that noble gases are indeed reactive enough to form chemical bonds have resulted in an avalanche of novel compounds during the next 50 years. It is estimated that the number of noble-gas compounds reaches today about five hundred. The barely noticeable seed immediately sprouted and the myth of inertness collapsed. The chemical bonding in the multitude of novel species is hardly different from those observed in the first synthesized compounds. Indeed, it is mostly the fluoro- and oxo-connections of the heavier noble gases (Kr and Xe), which predominate this beautiful chemistry.10,11 Xenon shows reactivity similar to iodine and it forms compounds at oxidation states from (II), via (IV) and (VI), to (VIII); these are isoelectronic and most often isostructural with connections of I(I), I(III), Physics & Chemistry low temp Tact/11/PAN/001 Physics & Chemistry low temp Tact/11/PAN/001 chapter 13.indd 421 1/27/2011 8:57:09 PM 422 W. Grochala, L. Khriachtchev, and M. Räsänen Fig. 1. Classical picture of chemical bonding in XeF2 molecule. The Lewis (dot) diagram (left) and the molecular orbital picture of three-center four-electron bonding neglecting the s/p mixing (right). Similar diagrams may be drawn for tetragonal-planar XeF4 and for octahedral XeF6. I(V), and I(VII), respectively. The binary fluorides of xenon (XeF2, XeF4, and XeF6) are probably the best characterized of all the compounds of this element by both experiment and theory.12 Meticulous studies of Xe(VI)O3 and Xe(VIII)O4 have been limited by the explosive nature of these compounds, but the oxo-salts of xenon (perxenathes) such as Ba2Xe(VIII)O6 are thermally quite stable. XeF2 is one of the most stable chemical compounds of the noble gases; it forms soft molecular crystals (space group I4/mmm) and sublimes easily (even at room temperature) without decomposition. The Xe–F bond length is 1.974 Å in the gas phase and increases only slightly to 2.00 Å in the solid state. The most frequently drawn picture of the chemical bonding in XeF2 is that of 3-center 4-electron bonding (molecular orbital diagram in Fig. 1 accounts only for 5p orbitals of Xe and neglects 5s contribution). Both Xe–F bonds are equivalent in the linear symmetric XeF2 molecule. However, the occupied Xe–F bonding HOMO-1 orbital (su) and the unoccupied LUMO (also su) are prone to mixing with the occupied Xe–F nonbonding HOMO (sg) when a molecule is found in an asymmetric environment (otherwise mixing is symmetry-forbidden). Thus, the Xe–F bonds have substantially different lengths in the case of ionic [A–F–]…[XeF+] salts, where A represents a strong Lewis acid (SbF5, SO3, etc.). For example, the closest Xe–F separations are 1.84 and 2.35 Å for the [XeF][Sb2F11] salt. Physics & Chemistry low temp Tact/11/PAN/001 Physics & Chemistry low temp Tact/11/PAN/001 chapter 13.indd 422 1/27/2011 8:57:09 PM Noble-Gas Chemistry 423 Fig. 2. Illustration of the plasticity of the first coordination sphere of (left) Kr(II) for a few fluoro-connections, (middle) hypervalent Sb(III) and Sb(V) linked to iodine, and (right) Cu(II) in an oxide environment. The first- and second-order Jahn–Teller effects are responsible to various degrees for deformation of the first coordination sphere of the central cations. Reproduced with permission from Refs. 13–15. One interesting observation is that if one Xe–ligand bond strengthens, the other weakens and vice versa. All known chemical connections of noble gases exhibit the same characteristic feature as illustrated in Fig. 2 for selected fluoro-connections of krypton. The electron-rich Ng(II) cations exhibit substantial flexibility of the first coordination sphere in analogy with other “hypervalent” species as Sb(III), Sb(V), etc.14 Such behavior, sometimes referred to as distortion isomerism, is due to the second-order Jahn–Teller effect; it renders noble-gas species analogous to the odd–electron transition-metal cations such as Cu(II) (susceptible to the first-order Jahn–Teller effect, see Fig. 2).15 It is remarkable that the entire route from ideally symmetric to highly asymmetric hypervalent bonding may be encompassed by deliberate variation of one parameter only: the Lewis acidity.16 Thus, at least five distinct well-characterized phases exist in the phase diagram of the XeF2/XeF5AsF6 mixture, and each of them exhibits a more or less – … + pronounced dissociation of XeF2 into the ionic [A–F ] [XeF ] form, consistent with the acid/base ratio, for example: . 2XeF2 + XeF5 AsF6 → 2[XeF2] XeF5 AsF6, (1) 2[XeF2]×[XeF5 AsF6] + XeF5 AsF6 → 2{XeF2×[XeF5 AsF6]}, (2) {XeF2×[XeF5 AsF6]} + XeF5 AsF6 → [XeF2]×2[XeF5 AsF6]. (3) Physics & Chemistry low temp Tact/11/PAN/001 Physics & Chemistry low temp Tact/11/PAN/001 chapter 13.indd 423 1/27/2011 8:57:10 PM 424 W. Grochala, L. Khriachtchev, and M. Räsänen The more covalent bond between Xe and F in the XeF+ cation is of course appreciably stronger than the average hypervalent Xe–F bond for 16 symmetric XeF2. This observation gives a hint as to one possible strategy toward new stable noble-gas species. As we see later, attempts to avoid hypervalence of the noble-gas atom by designing a highly asymmetric ionic structure in fact bring us closer to the first chemical connections of helium (F–…HeO and related species). Finally, we note that an entire family of compounds is known that 17 contain XeF2 or XeF4 as molecular ligands for “naked” metal cations.
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