The Crystal and Molecular Structure of γ‐P4S6

Rödl, Thomas; Pfitzner, Arno

doi:10.1002/zaac.201100216

Cited by 9 publications

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“…Obwohl umfangreiche Untersuchungen im System Phosphor‐Schwefel bekannt sind, erhielt man nun erstmals Informationen zu Phosphorpolysulfiden 1_107. Ein weiteres Phosphorsulfid — γ‐P4S6 — wurde ebenfalls strukturell untersucht 1_108…”

Section: Gruppen 15 Bis 18unclassified

Anorganische Chemie 2011

2012

Nachr Chem

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Nachrichten aus der Chemie| 60 | März 2012 | www.gdch.de/nachrichten Abb. 32. Dieses Maschendrahtmuster ist nur eine von drei verschiedenen Topologien, die durch Wahl der Kristallisationsmethode von 2-iso-Propylimidazolatliganden mit Silber(I)-Kationen verwirklicht werden konnte. 60) Abb. 31. Zwölf bifunktionale Acetylacetonatliganden falten sich nach Deprotonierung und Koordination von acht Eisen(III)-Zentren zu einer komplizierten Knotenstruktur. 57)

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Section: Gruppen 15 Bis 18unclassified

Anorganische Chemie 2011

2012

Nachr Chem

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“…The high temperature synthesis of P 2 S 7 from P 4 S 3 and elemental sulfur by catalytic amounts of FeCl 3 shows up a new reaction pathway of phosphorus chalcogenides and metal halides. We recently observed the iron(III)-catalyzed formation of g-P 4 S 6 in CS 2 as a solvent, [16] the reaction of P 4 S 10 with TiCl 4 in solution results in the formation of [(TiCl 2 )(1,3-P 2 S 8 )] 2 . [12] In contrast, the cage molecules are preserved in adducts with TaCl 5 [17] or even as co-crystals with Ta 2 Cl 10 [18] when reactions are performed in solution.…”

Section: [11c]mentioning

confidence: 99%

Rational Syntheses and Structural Characterization of Sulfur‐Rich Phosphorus Polysulfides: α‐P₂S₇ and β‐P₂S₇

et al. 2011

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A wide range of binary compounds is known in the system phosphorus-sulfur. They consist of discrete cage-like molecules with the composition P 4 S n (n = 3-10) except for P 14 S. [1] The cages can formally be derived from the P 4 tetrahedron of white phosphorus either by insertion of sulfur atoms into P À P bonds or by exocyclic addition to phosphorus atoms. The maximum amount of sulfur per molecule is present in P 4 S 10 . [2] The congruently melting phosphorus sulfides P 4 S 3 , P 4 S 7 , and P 4 S 10 are synthesized by reaction of stoichiometric amounts of the elements in the melt. [3] Other phosphorus sulfides are not accessible by this route. For instance, a-P 4 S 5 is prepared by stirring a solution of P 4 S 3 , sulfur, and catalytic amounts of iodine in dry carbon disulfide at room temperature and diffuse daylight for three days. [4] Jason used triphenylarsenic sulfide and triphenylantimony sulfide as sulfur transfer reagents in the synthesis of g-P 4 S 6 , for example. [5] Another very useful sulfur transfer reagent is [(CH 3 ) 3 Sn] 2 S. [6] In contrast triphenylphosphine is suitable for the abstraction of sulfur atoms. [7] Note that the syntheses of phosphorus sulfides often result in mixtures of different compounds. In addition, various modifications of phosphorus sulfides of the same composition are known. Unfortunately the nomenclature is far from systematic. In fact, it is a quite confusing mix of Greek letter prefixes and Roman numeral suffixes that are used to distinguish between both different constitution isomers and different crystal structures of identical cage molecules. Herein we use Greek letter prefixes, not only to distinguish between two polymorphs but also to consider the chronological order of their discovery.As already mentioned P 4 S 10 is the most sulfur-rich phosphorus sulfide structurally characterized to date. However there is evidence for the existence of more sulfur-rich compounds P 4 S n with n > 10. [8] As early as 1910 Stock suspected that P 4 S 10 was not the most sulfur-rich phosphorus sulfide at all. [9] DØmarcq prepared PS x (x = 3-75) by heating P 4 S 10 with an excess of sulfur at 300 8C. [10] The corresponding solution 31 P NMR spectra indicated a number of novel species. He termed these compounds as "phosphorus polysulfides" or "phosphorus persulfides" implying the presence of S À S bonds. Though the system phosphorus-sulfur has been investigated for a long time, there are no structural data of phosphorus poly-(or per-) sulfides available.More than 150 years after the discovery of P 4 S 10 by Berzelius in 1843, we herein present the first crystal structure determinations of phosphorus polysulfides, namely a-P 2 S 7 and b-P 2 S 7 .The structures of a-P 2 S 7 and b-P 2 S 7 differ dramatically from those of common phosphorus sulfides. They do not consist of discrete cage-like molecules but of neutral polymeric strands featuring direct SÀS bonds. Both the polymers catena-P 2 S 7 in a-P 2 S 7 and in b-P 2 S 7 are quite similar: each phosphorus atom is tetrahedrally surr...

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“…So konnten wir kürzlich die Eisen(III)-katalysierte Bildung von g-P 4 S 6 in CS 2 als Lçsungsmittel beobachten, [16] während bei der Umsetzung von P 4 S 10 mit TiCl 4 in Lçsung [(TiCl 2 )(1,3-P 2 S 8 )] 2 entsteht. [12] Abbildung 3.…”

Section: Form Von Drei Verknüpften Schwefelatomen (-S-s-s-) Auf Die unclassified

Die rationale Synthese und strukturelle Charakterisierung schwefelreicher Phosphorpolysulfide – α‐P₂S₇ und β‐P₂S₇

et al. 2011

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The Crystal and Molecular Structure of γ‐P₄S₆

Abstract: Abstract. The crystal and molecular structure of γ-P 4 S 6 was determined from single-crystal X-ray diffraction. It crystallizes monoclinically in the space group P2 1 /m (No. 11) with a = 6.627(3) Å, b =

Cited by 9 publications

References 25 publications

Anorganische Chemie 2011

Anorganische Chemie 2011

Rational Syntheses and Structural Characterization of Sulfur‐Rich Phosphorus Polysulfides: α‐P₂S₇ and β‐P₂S₇

Die rationale Synthese und strukturelle Charakterisierung schwefelreicher Phosphorpolysulfide – α‐P₂S₇ und β‐P₂S₇

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The Crystal and Molecular Structure of γ‐P4S6

Abstract: Abstract. The crystal and molecular structure of γ-P 4 S 6 was determined from single-crystal X-ray diffraction. It crystallizes monoclinically in the space group P2 1 /m (No. 11) with a = 6.627(3) Å, b =

Cited by 9 publications

References 25 publications

Anorganische Chemie 2011

Anorganische Chemie 2011

Rational Syntheses and Structural Characterization of Sulfur‐Rich Phosphorus Polysulfides: α‐P2S7 and β‐P2S7

Die rationale Synthese und strukturelle Charakterisierung schwefelreicher Phosphorpolysulfide – α‐P2S7 und β‐P2S7

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The Crystal and Molecular Structure of γ‐P₄S₆

Rational Syntheses and Structural Characterization of Sulfur‐Rich Phosphorus Polysulfides: α‐P₂S₇ and β‐P₂S₇

Die rationale Synthese und strukturelle Charakterisierung schwefelreicher Phosphorpolysulfide – α‐P₂S₇ und β‐P₂S₇