A new method for the preparation of krypton difluoride

Slivnik, J.; Šmalc, Andrej; Lutar, K.; Žemva, Boris; Frlec, B.

doi:10.1016/s0022-1139(00)82488-4

Cited by 36 publications

(7 citation statements)

References 5 publications

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“…At the critical temperature of 502 K and critical pressure of 4.70 MPa, the degree of dissociation is about 10%. Kinetically only about 6.5% of the final equilibrium value dissociates in the first 8 min at 566 K, as was determined by measurements of the thermal dissociation of XeF6 (7). On the basis of all these data, it could be concluded that the degree of dissociation of XeFe at 502 K in the first 5 min of heating should be smaller than 0.5 %.…”

Section: Resultsmentioning

confidence: 68%

Critical constants of xenon hexafluoride

Ogrin¹,

Jesih²,

Žemva³

1987

J. Chem. Eng. Data

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Section: Resultsmentioning

confidence: 68%

Critical constants of xenon hexafluoride

Ogrin¹,

Jesih²,

Žemva³

1987

J. Chem. Eng. Data

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“…Xenon (99.99%) and krypton (99.99%) were used as supplied by Messer Griesheim. Xenon difluoride was prepared by irradiating a gaseous mixture of xenon and fluorine at room temperature. , Krypton difluoride was prepared photochemically from krypton in liquid fluorine at 77 K. , Xenon hexafluoride was synthesized from xenon and fluorine in the presence of nickel difluoride at 393 K . Fluorine (99%, Solvay) was used as supplied.…”

Section: Methodsmentioning

confidence: 99%

XeF₂·2CrF₄and XeF₅⁺CrF₅^-: Syntheses, Crystal Structures, and Some Properties

1998

Self Cite

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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.

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“…The known compounds of krypton are limited to the +2 oxidation state and include KrF 2 , − salts of the KrF + , − and Kr 2 F 3 + 11-13,15,16,18 cations, the molecular adducts KrF 2 ·MOF 4 (M = Cr, Mo, W), , KrF 2 · n MoOF 4 ( n = 2, 3), KrF 2 ·VF 5 , and KrF 2 ·MnF 4 , the RCN−KrF + (R = H, CF 3 , C 2 F 5 , n -C 3 F 7 ) cations, , and Kr(OTeF 5 ) 2 . While the strong oxidant characters of KrF 2 , KrF + , and Kr 2 F 3 + provide clean, low-temperature synthetic routes to BrF 6 + , , ClF 6 + , OsO 2 F 4 , AuF 5 , and TcOF 5 , they have also served as a significant impediment to their detailed structural characterization by single- crystal X-ray diffraction.…”

Section: Introductionmentioning

confidence: 99%

X-ray Crystal Structures of α-KrF₂, [KrF][MF₆] (M = As, Sb, Bi), [Kr₂F₃][SbF₆]·KrF₂, [Kr₂F₃]₂[SbF₆]₂·KrF₂, and [Kr₂F₃][AsF₆]·[KrF][AsF₆]; Synthesis and Characterization of [Kr₂F₃][PF₆]·nKrF₂; and Theoretical Studies of KrF₂, KrF⁺, Kr₂F₃
Lehmann
¹
,
Dixon
²
,
Schrobilgen
³

2001
Inorg. Chem.
77
19
115
0
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The crystal structures of alpha-KrF(2) and salts containing the KrF(+) and Kr(2)F(3)(+) cations have been investigated for the first time using low-temperature single-crystal X-ray diffraction. The low-temperature alpha-phase of KrF(2) crystallizes in the tetragonal space group I4/mmm with a = 4.1790(6) A, c = 6.489(1) A, Z = 2, V = 113.32(3) A(3), R(1) = 0.0231, and wR(2) = 0.0534 at -125 degrees C. The [KrF][MF(6)] (M = As, Sb, Bi) salts are isomorphous and isostructural and crystallize in the monoclinic space group P2(1)/c with Z = 4. The unit cell parameters are as follows: beta-[KrF][AsF(6)], a = 5.1753(2) A, b = 10.2019(7) A, c = 10.5763(8) A, beta = 95.298(2) degrees, V = 556.02(6) A(3), R(1) = 0.0265, and wR(2) = 0.0652 at -120 degrees C; [KrF][SbF(6)], a = 5.2922(6) A, b = 10.444(1) A, c = 10.796(1) A, beta = 94.693(4) degrees, V = 594.73(1) A(3), R(1) = 0.0266, wR(2) = 0.0526 at -113 degrees C; [KrF][BiF(6)], a = 5.336(1) A, b = 10.513(2) A, c = 11.046(2) A, beta = 94.79(3) degrees, V = 617.6(2) A(3), R(1) = 0.0344, and wR(2) = 0.0912 at -130 degrees C. The Kr(2)F(3)(+) cation was investigated in [Kr(2)F(3)][SbF(6)].KrF(2), [Kr(2)F(3)](2)[SbF(6)](2).KrF(2), and [Kr(2)F(3)][AsF(6)].[KrF][AsF(6)]. [Kr(2)F(3)](2)[SbF(6)](2).KrF(2) crystallizes in the monoclinic P2(1)/c space group with Z = 4 and a = 8.042(2) A, b = 30.815(6) A, c = 8.137(2) A, beta = 111.945(2) degrees, V = 1870.1(7) A(3), R(1) = 0.0376, and wR(2) = 0.0742 at -125 degrees C. [Kr(2)F(3)][SbF(6)].KrF(2) crystallizes in the triclinic P1 space group with Z = 2 and a = 8.032(3) A, b = 8.559(4) A, c = 8.948(4) A, alpha = 69.659(9) degrees, beta = 63.75(1) degrees, gamma = 82.60(1) degrees, V = 517.1(4) A(3), R(1) = 0.0402, and wR(2) = 0.1039 at -113 degrees C. [Kr(2)F(3)][AsF(6)].[KrF][AsF(6)] crystallizes in the monoclinic space group P2(1)/c with Z = 4 and a = 6.247(1) A, b = 24.705(4) A, c = 8.8616(6) A, beta = 90.304(6) degrees, V = 1367.6(3) A(3), R(1) = 0.0471 and wR(2) = 0.0958 at -120 degrees C. The terminal Kr-F bond lengths of KrF(+) and Kr(2)F(3)(+) are very similar, exhibiting no crystallographically significant variation in the structures investigated (range, 1.765(3)-1.774(6) A and 1.780(7)-1.805(5) A, respectively). The Kr-F bridge bond lengths are significantly longer, with values ranging from 2.089(6) to 2.140(3) A in the KrF(+) salts and from 2.027(5) to 2.065(4) A in the Kr(2)F(3)(+) salts. The Kr-F bond lengths of KrF(2) in [Kr(2)F(3)][SbF(6)].KrF(2) and [Kr(2)F(3)](2)[SbF(6)](2).KrF(2) range from 1.868(4) to 1.888(4) A and are similar to those observed in alpha-KrF(2) (1.894(5) A). The synthesis and Raman spectrum of the new salt, [Kr(2)F(3)][PF(6)].nKrF(2), are also reported. Electron structure calculations at the Hartree-Fock and local density-functional theory levels were used to calculate the gas-phase geometries, charges, Mayer bond orders, and Mayer valencies of KrF(+), KrF(2), Kr(2)F(3)(+), and the ion pairs, [KrF][MF(6)] (M = P, As, Sb, Bi), and to assign their experimental vibrational frequencies.

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A new method for the preparation of krypton difluoride

Cited by 36 publications

References 5 publications

Critical constants of xenon hexafluoride

Critical constants of xenon hexafluoride

XeF₂·2CrF₄and XeF₅⁺CrF₅^-: Syntheses, Crystal Structures, and Some Properties

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A new method for the preparation of krypton difluoride

Cited by 36 publications

References 5 publications

Critical constants of xenon hexafluoride

Critical constants of xenon hexafluoride

XeF2·2CrF4and XeF5+CrF5-: Syntheses, Crystal Structures, and Some Properties

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XeF₂·2CrF₄and XeF₅⁺CrF₅^-: Syntheses, Crystal Structures, and Some Properties