Synthesis, crystal structure, vibrational spectra, and thermal behaviour of [Ph4P](2)[Bi-2(mu-Br)(2)Br-6 (CH3COCH3)(2)]

Autor(en): Ahmed, IA
Blachnik, R
Reuter, H 
Eickmeier, H
Schultze, D
Brockner, W
Stichwörter: ANTIMONY(III); bismuth; BISMUTH(III); Chemistry; Chemistry, Inorganic & Nuclear; crystal structure; PHOSPHINE COMPLEXES; thermal analysis; vibrational spectra
Erscheinungsdatum: 2001
Herausgeber: WILEY-V C H VERLAG GMBH
Journal: ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE
Volumen: 627
Ausgabe: 6
Startseite: 1365
Seitenende: 1370
Zusammenfassung: 
[Ph4P](2)[Bi2Br8(CH3COCH3)(2)] (1) was obtained by the reaction of [Ph4P]Br and BiBr3 in acetone. Single crystals were grown by allowing a layer of n-hexane to diffuse into the acetonic solution of 1. The crystal structure was determined by means of X-ray diffraction. 1 crystallises with monoclinic symmetry in the space group P2(1)/n, No. 14 with the lattice parameters: a = 13.358(2), b = 12.637(2), c = 18.565(3) Angstrom, beta = 102.62(1)degrees, V = 3058.1(8) Angstrom (3) and Z = 4. The structure is characterised by the anion [Bi2Br8(CH3COCH3)(2)](2-) which is embedded in a matrix of [Ph4P](+) cations. The anion can be described as two edge-sharing square pyramids with the apical bromide ions in anti-position. Acetone co-ordinates the bismuth atoms via oxygen atoms and increases the co-ordination number of central bismuth atoms to six which results in the formation of a distorted bi-octahedron. The distortion is due to the difference in terminal and bridging Bi-Br bond lengths. FT-IR and Raman spectroscopic data are presented. In addition, the thermal behaviour of the compound was studied with the aid of TG/DSC coupled with MS revealing that acetone leaves the crystal in two steps. The compound melts at 203 degreesC and transforms into a glass on cooling.
ISSN: 00442313
DOI: 10.1002/1521-3749(200106)627:6<1365::AID-ZAAC1365>3.0.CO;2-7

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