Crystal structures of [bis(triisobutylphosphonium)trisulfane]-di[nonachlorooxodiniobiate(V )], [(((CH3)(2)CHCH2)(3)P)(2)S-3][Nb2OCl9](2) and [octachloro(triisobutylphosphinesulfide)-oxodiniobium(V)], [Nb2OCl8{((CH3)(2)CHCH2)(3)PS}]

Autor(en): Stumpf, K
Blachnik, R
Roth, G
Stichwörter: Crystallography
Erscheinungsdatum: 1999
Herausgeber: R OLDENBOURG VERLAG
Journal: ZEITSCHRIFT FUR KRISTALLOGRAPHIE
Volumen: 214
Ausgabe: 4
Startseite: 251
Seitenende: 254
Zusammenfassung: 
Red crystals of [(((CH3)(2)CHCH2)(3)P)2S(3)] [Nb2OCl9](2) 1 and [Nb2OCl8 {((CH3)(2)CHCH2)(3)PS}] 2 were obtained from equimolar solutions of niobium pentachloride and triisobutylphosphinesulfide in dichloromethane. The oxygen in the compounds originates from a reaction of the educts with traces of water. The complexes were characterized by single crystal structure determination. 1, triclinic, S.G.: P (1) over bar (Nr. 2) a = 10.986(1) Angstrom, b = 11.069(1) Angstrom c = 26.473(2) Angstrom alpha = 95.16(1)degrees, beta = 92.97(1)degrees, gamma = 116.61(1)degrees V = 2851.2(4) Angstrom(3), Z = 2. 2, triclinic, S.G.: P (1) over bar (Nr. 2), a = 10.818(l) Angstrom, b = 16.705(2) Angstrom, c = 16.782(2) Angstrom, alpha = 65.69(1)degrees, beta = 82.23(1)degrees, gamma = 88.63(1)degrees, V = 2736.8(5) Angstrom(3), Z = 4. The asymmetric unit of 1 consists of [(((CH3)(2)CHCH2)(3)P)(2)S-3] cation with a PSSSP-chain and two [Nb2OCl9](-)-anions. The anions have nearly linear Nb-O-Nb bridges (bond angles 169.3(3)degrees and 172.1(3)degrees) and Nb-O bond lengths of 1.746(5) Angstrom for the short and 2.121(5) Angstrom for the long bonds. Two anions are linked by symmetric chlorine bridges with bond lengths of 2.76 Angstrom and 2.77 Angstrom to form a dimer. 2 is built of neutral [Nb2OCl8 {((CH3)(2)CHCH2)(3)PS}] complexes. The Nb-O-Nb angles and Nb-O bond distances correspond to those found in 1. The neutral complexes in 2 are linked by symmetric chlorine bridges, analog 1, to dimers.
ISSN: 00442968
DOI: 10.1524/zkri.1999.214.4.251

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