Xenon(IV) - carbon bonding has been realized for the first time in the product formed from the reaction of XeF(4) with C(6)F(5)BF(2) in CH(2)Cl(2) at -55 degrees C [Eq. (1)]. [C(6)F(5)XeF(2)][BF(4)] is a strong oxidative fluorinating agent. This xenon(IV) compound fluorinates (C(6)F(5))(3)P to (C(6)F(5))(3)PF(2), C(6)F(5)I to C(6)F(5)IF(2), and I(2) to IF(5). In all cases, [C(6)F(5)Xe][BF(4)] was obtained as a by-product.
XeF2·2CrF4 was prepared by
solvolysis of XeF2·CrF4 in anhydrous
hydrogen fluoride (aHF) and subsequent
decantation of the majority of dissolved XeF2 in aHF.
Remaining XeF2 and a large excess of CrF4
form XeF2·2CrF4 after aHF is removed. Ruby-red single crystals
were obtained either by heating the sample in a thermal
gradient or by recrystallization in supercritical SF6.
The compound crystallizes in the triclinic space group
P1̄
with a = 855.1(3) pm, b = 922.1(3)
pm, c = 1043.8(3) pm, α = 76.02(2)°, β
= 81.36(2)°, γ = 88.08(3)°, and
Z = 4 at 293 K. The basic structural unit is formed
by four independent Cr atoms, each octahedrally
coordinated
by six F atoms. Two fluorine ligands are provided by two different
XeF2 molecules. The distorted octahedra
are
connected via common F atoms to form a three-dimensional network.
XeF5
+CrF5
-
was prepared from XeF6 and
CrF4 at room temperature or by the reaction of
XeF6 and CrF5 at 333 K. Red single
crystals were grown from
the solution of
XeF5
+CrF5
- in
aHF. The compound crystallizes in the orthorhombic space group
Pbca with a =
1828.1(13) pm, b = 842.9(7) pm, c =
1852.1(12) pm, and Z =16 at 268 K. The main
structural feature is
formed by an infinite chain of distorted CrF6 octahedra
joined via cis vertexes, while XeF5
+ cations
compensate
the negative charge of each octahedron.
Erstmals wurden schwarze, metallisch glänzende Einkristalle von AgF2 durch Erhitzen des mikrokristallinen AgF2 dargestellt (Monel‐Autoklaven, T ≈ 400°C, HF/F2‐Gemisch, 4 d). Die röntgenographische Untersuchung (a = 556,8(1); = 583,1(1); c = 510,1(1) pm; Z = 4; Parameter siehe Text) bestätigt die aus Neutronenbeugungsuntersuchung ermittelte Raumgruppe Pbca – D 2h15 (Nr. 61) und ergibt Lageparameter, die mit den damals ermittelten Werten praktisch übereinstimmen. Der Madelunganteil der Gitterenergie, MAPLE, sowie Effektive Koordinationszahlen, ECoN, werden über Mittlere Fiktive Ionenradien, MEFIR, berechnet und diskutiert.
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