Metal(II) Hexafluorophosphates(V) (M = Sr, Pb) Containing XeF<sub>2</sub>-Coordinated Metal Ions [M(XeF<sub>2</sub>)<sub>3</sub>](PF<sub>6</sub>)<sub>2</sub>, [Pb<sub>3</sub>(XeF<sub>2</sub>)<sub>11</sub>](PF<sub>6</sub>)<sub>6</sub>, and [Sr<sub>3</sub>(XeF<sub>2</sub>)<sub>10</sub>](PF<sub>6</sub>)<sub>6</sub>
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From the system MF2/PF5/XeF2/anhydrous hydrogen fluoride (aHF), four compounds [Sr(XeF2)3](PF6)2, [Pb(XeF2)3](PF6)2, [Sr3(XeF2)10](PF6)6, and [Pb3(XeF2)11](PF6)6 were isolated and characterized by Raman spectroscopy and X-ray single-crystal diffraction. The [M(XeF2)3](PF6)2 (M = Sr, Pb) compounds are isostructural with the previously reported [Sr(XeF2)3](AsF6)2. The structure of [Sr3(XeF2)10](PF6)6 (space group C2/c; a = 11.778(6) Å, b = 12.497(6) Å, c = 34.60(2) Å, β = 95.574(4)°, V = 5069(4) Å3, Z = 4) contains two crystallographically independent metal centers with a coordination number of 10 and rather unusual coordination spheres in the shape of tetracapped trigonal prisms. The bridging XeF2 molecules and one bridging PF6- anion, which connect the metal centers, form complicated 3D structures. The structure of [Pb3(XeF2)11](PF6)6 (space group C2/m; a = 13.01(3) Å, b = 11.437(4) Å, c = 18.487(7) Å, β = 104.374(9)°, V = 2665(6) Å3, Z = 2) consists of a 3D network of the general formula {[Pb3(XeF2)10](PF6)6}n and a noncoordinated XeF2 molecule fixed in the crystal structure only by weak electrostatic interactions. This structure also contains two crystallographically independent Pb atoms. One of them possesses a unique homoleptic environment built up by eight F atoms from eight XeF2 molecules in the shape of a cube, whereas the second Pb atom with a coordination number of 9 adopts the shape of a tricapped trigonal prism common for lead compounds. [Pb3(XeF2)11](PF6)6 and [Sr3(XeF2)10](PF6)6 are formed when an excess of XeF2 is used during the process of the crystallization of [M(XeF2)3](PF6)2 from their aHF solutions.
