The phase diagram of the system [Ph4P]Br/BiBr3. Synthesis, crystal structure, thermal behaviour, and vibrational spectra of [Ph4P](3)[Bi2Br9] center dot CH3COCH3 and two modifications of [Ph4P](4)[Bi6Br22]

Autor(en): Ahmed, IA
Blachnik, R
Kastner, G
Brockner, W
Stichwörter: bismuth(III)-bromide; Chemistry; Chemistry, Inorganic & Nuclear; crystal structure; phase diagram; thermal analysis; vibrational spectra
Erscheinungsdatum: 2001
Herausgeber: WILEY-V C H VERLAG GMBH
Journal: ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE
Volumen: 627
Ausgabe: 9
Startseite: 2261
Seitenende: 2268
Zusammenfassung: 
phase diagram of the system [Ph4P]Br/BiBr3 was investigated with the aid of DSC, TG and temperature dependent X-ray powder diffraction measurements. By varying the reaction conditions. stoichiometry and crystallisation conditions of the reaction between BiBr3 and [Ph4P]Br four polynuclear bromobismuthates are formed. We report here the crystal structure of the solvation product [Ph4P](3-) [Bi2Br9] . CH3COCH3, which crystallises with monoclinic symmetry in the S. G. P2(1)/n No. 14, a = 12.341(1), b = 32.005(3), c=19.929(3)Angstrom, beta =99.75(2)degrees, V=7758(7) Angstrom (3), Z = 4 and the crystal structures of two modifications of the compound [Ph4P](4)[Bi6Br22]. The alpha -form, crystallises with triclinic symmetry in the S.G. P (1) over bar No.2, a=13.507(4) Angstrom, b = 14,434(4) Angstrom, c = 17.709(5) Angstrom, alpha = 81.34(2)degrees, beta = 72.42(2)degrees, gamma = 72.53(2)degrees, V = 3132.7(1) Angstrom (3), Z = 2. The high-temperature fl-form, crystallises with triclinic symmetry in the S. G. P (1) over bar No. 2, a = 13.893(4) Angstrom, b = 14.267(3) Angstrom, c = 16.580(3), alpha = 100.13(2)degrees, beta =96.56(2)degrees, gamma =110.01(2)degrees, V=2985.5(1) Angstrom (3), Z = 2. Lattice parameters of [Ph4P](4)[Bi8Br28] are also given. The thermal behaviour of the compounds and in addition the vibrational spectra of [Ph4P](3)[Bi2Br9] . CH3COCH3 are presented and discussed.
ISSN: 00442313
DOI: 10.1002/1521-3749(200109)627:9<2261::AID-ZAAC2261>3.0.CO;2-T

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