The reaction between Ba(SbF(6))(2) and excess XeF(2) in anhydrous HF at room temperature yields the white solid Ba(SbF(6))(2).5XeF(2) after the excess XeF(2) and the solvent have been removed under vacuum. Ba(SbF(6))(2).5XeF(2) crystallizes in the monoclinic space group C2/m, with a = 13.599(6) A, b = 12.086(4) A, c = 9.732(5) A, beta = 134.305(6) degrees, V = 1144.7 (8) A(3), and Z = 2. The coordination sphere of each barium atom consists of 12 fluorine atoms. The structure consists of alternating layers of Ba(SbF(6))(2).XeF(2) and 4 XeF(2) molecules. The Ba atoms in the Ba(SbF(6))(2).XeF(2) layer are in a nearly rhombic-net array and are linked with trans F-bridging ligands of SbF(6)(-). A XeF(2) molecule is placed in the center of each rhombus of the Ba(2+) array so that its symmetry axis is perpendicular to the plane of the Ba(SbF(6))(2).XeF(2) layer. This layer is linked to its neighbors by a layer of centrosymmetric XeF(2) molecules. Raman spectra are in accord with all XeF(2) molecules being symmetrical.
Metal Centers. -Crystals of the title compounds are grown from M(SbF6)2 (M: Mg, Ca) dissolved in anhydrous HF. As revealed by single crystal XRD, [Mg(HF)2](SbF6)2 crystallizes in the space group Pnma with Z = 4. The structure contains alternating rows of Mg and Sb atoms forming a three-dimensional network. [Ca(HF) 2 ](SbF 6 ) 2 crystallizes in the space group P2 1 /n with Z = 4. The structure contains [Ca(SbF 6 ) + ] n layers connected by SbF 6 groups. HF molecules occupy the space between these layers and additionally contribute to the connection between the layers by hydrogen bonding. -(TURICNIK, A.; BENKIC, P.; ZEMVA*, B.; J.
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