From the system MF
2/PF
5/XeF
2/anhydrous hydrogen fluoride (aHF), four compounds [Sr(XeF
2)
3](PF
6)
2, [Pb(XeF
2)
3](PF
6)
2, [Sr
3(XeF
2)
10](PF
6)
6, and [Pb
3(XeF
2)
11](PF
6)
6 were isolated and characterized by Raman spectroscopy andX-ray single-crystal diffraction. The [M(XeF
2)
3](PF
6)
2 (M = Sr, Pb) compounds are isostructural with the previouslyreported [Sr(XeF
2)
3](AsF
6)
2. The structure of [Sr
3(XeF
2)
10](PF
6)
6 (space group
C2
/c;
a = 11.778(6) Å,
b = 12.497(6) Å,
c = 34.6
0(2) Å,
![](/images/<font color=)
gifchars/beta2.
gif"
BORDER=
0 ALIGN="middle"> = 95.574(4)
![](/images/entities/deg.<font color=)
gif">,
V = 5
069(4) Å
3,
Z = 4) contains two crystallographically independentmetal centers with a coordination number of 1
0 and rather unusual coordination spheres in the shape of tetracappedtrigonal prisms. The bridging XeF
2 molecules and one bridging PF
6- anion, which connect the metal centers, formcomplicated 3D structures. The structure of [Pb
3(XeF
2)
11](PF
6)
6 (space group
C2
/m;
a = 13.
01(3) Å,
b = 11.437(4)Å,
c = 18.487(7) Å,
![](/images/<font color=)
gifchars/beta2.
gif" BORDER=
0 ALIGN="middle"> = 1
04.374(9)
![](/images/entities/deg.<font color=)
gif">,
V = 2665(6) Å
3,
Z = 2) consists of a 3D network of the general formula{[Pb
3(XeF
2)
10](PF
6)
6}
n and a noncoordinated XeF
2 molecule fixed in the crystal structure only by weak electrostaticinteractions. This structure also contains two crystallographically independent Pb atoms. One of them possessesa unique homoleptic environment built up by eight F atoms from eight XeF
2 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 prismcommon for lead compounds. [Pb
3(XeF
2)
11](PF
6)
6 and [Sr
3(XeF
2)
10](PF
6)
6 are formed when an excess of XeF
2 isused during the process of the crystallization of [M(XeF
2)
3](PF
6)
2 from their aHF solutions.