Tetraphenyldiphosphine disulphide (tetraphenyl-1,2-dithioxodi-λ5-phosphane), Ph2P(S)P(S)Ph2

Blake, Alexander J.; Howie, R. Α.; McQuillan, Geoffrey P.

doi:10.1107/s0567740881004780

Cited by 11 publications

(2 citation statements)

References 3 publications

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“…80 Hz. This observation is in agreement with the X-ray diffraction crystal structure reported by Blake et al 27 The data show the unit cell to be of space group P2,/c and to contain two different half-molecules. Each of the two resonances, therefore, represents one of the non-congurent phosphorus molecules within the unit cell.…”

Section: Discussionsupporting

confidence: 92%

Phosphorus-31 nuclear magnetic resonance studies of solid diphosphine disulphides. Crystallographic considerations

Harris¹,

Merwin²,

Hägele³

1987

J. Chem. Soc., Faraday Trans. 1

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High-resolution 31P n.m.r. spectra have been obtained for a number of solid diphosphine disulphides under conditions of high-power decoupling, crosspolarization and magic-angle rotation. The results yield crystallographic information about the size of the asymmetric unit and are consistent with data from X-ray diffraction work when known. In one case, evidence of morphological variation is obtained.

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Section: Discussionsupporting

confidence: 92%

Phosphorus-31 nuclear magnetic resonance studies of solid diphosphine disulphides. Crystallographic considerations

Harris¹,

Merwin²,

Hägele³

1987

J. Chem. Soc., Faraday Trans. 1

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“…The molecular structure is a substituted cyclohexane ring with a chair conformation having two neighboring methylene units being replaced by phenylthiophosphanyl moieties. The P1−P2 bond length of 225.41 (8) pm lies in the expected range of diphosphanes (226.3(4) pm) 14 which are bonded to aromatic substituents and is significantly elongated in comparison to those in aliphatic diphosphane disulfides (approximately 221(1) pm). 15 A special case within this substance class is tetramethyldiphosphane disulfide, because the determination of the crystal structure showed two molecules in the asymmetric unit with significantly different P−P bond lengths of 216.1(6) and 224.5(6) pm.…”

Section: Photolysis Ofmentioning

confidence: 99%

Reactivity Studies of [(thf)₂Mg{μ-C(CH₃)₂C₂H₄C(CH₃)₂}]₂: Scrambling Reactions and Diverse Reactions with Dichlorophenylphosphane

2016

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I n T H F s o l u t i o n [ { ( t h f ) 2 M g { μ -C -(CH 3 ) 2 C 2 H 4 (CH 3 ) 2 C}} 2 ] (1) exchanges the alkanediide ligand with [{(thf) 2 Mg{μ-CH 2 ) 5 }} 2 ] in an equilibrium leading to the formation of [{(thf) 2 Mg} 2 {μ-C(CH 3 ) 2 C 2 H 4 C(CH 3 ) 2 }{μ-(CH 2 ) 5 }](2). Depending on the crystallization temperature, homoleptic 1 or heteroleptic 2 crystallizes from THF solutions, verifying a temperature-dependent Schlenk equilibrium. Irradiation of a solution of 1 in [D 8 ]THF with UV light yields magnesium hydride and alkene via a β-hydride elimination reaction. In a metathetical approach dichlorophenylphosphane reacts with 1 in THF to give the intermediate "PhP(Cl){C(CH 3 ) 2 C 2 H 4 (CH 3 ) 2 CMgCl" (3-MgCl), which forms three subsequent products. In order to ease handling and characterization of these compounds, hydrolysis and oxidation with sulfur has been performed. This product mixture was separated by column chromatography, yielding the chlorophosphane sulfide [Ph(S)P(Cl){C-(CH 3 ) 2 C 2 H 4 (CH 3 ) 2 CH)}] (3-S), the cyclic phosphane sulfide [Ph(S)P{C(CH 3 ) 2 C 2 H 4 (CH 3 ) 2 C)}] (4-S), and the cyclic 1,1diphosphane disulfide [{(Ph(S)P} 2 {μ-C(CH 3 ) 2 C 2 H 4 (CH 3 ) 2 C}] (6-S 2 ). Furthermore, traces of the acyclic 1,1-diphosphane disulfides [{PhP(S)(C(CH 3 ) 2 C 2 H 4 CH(CH 3 ) 2 )}{PhP(S)(C(CH 3 ) 2 C 2 H 4 C(CH 3 )(CH 2 )}] (8-S 2 ) and meso-[{Ph(S)P(C-(CH 3 ) 2 C 2 H 4 (CH 3 ) 2 CH)} 2 ] (7-S 2 ) have also been isolated. Compounds 6−8 represent the phosphorus-containing products of indirect Grignard reductions.

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Acyl‐ und Alkylidenphosphane. XXV. Molekül‐ und Kristallstruktur des 1,2‐Di(tert‐butyl)‐3‐dimethylamino‐1‐thio‐4‐trimethylsilylsulfano‐1λ⁵,2λ³‐diphosphet‐3‐ens

Becker

Uhl

1984

Zeitschrift anorg allge chemie

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Die bei der Zersetzung von tert‐Butyl(N,N‐dimethylthiocarbamoyl)‐trimethylsilylphosphan mit nahezu quantitativer Ausbeute gebildete Titelverbindung 1 kristallisiert orthorhombisch in der Raumgruppe P212121 mit {a = 1067,3(1); b = 1077,1(1); c = 1924,6(5) pm; Z = 4} bei + 20°C. Nach den Ergebnissen einer Röntgenstrukturanalyse (RG = 0,038) ordnen sich die beiden tert‐Butylgruppen am vierfach (P1) und am dreifach koordinierten Phosphoratom (P2) trans zueinander an. Charakteristische Bindungslängen sind {endocycl.: P1–P2 221,9(1); P1–C4 177,7(3); P2–C3 185,1(4); C3–C4 136,0(5)} und {exocycl.: P1–S1 195,6(1); C3–N3 135,8(4); C4–S4 177,7(4); S4–Si4 216,1(2) pm}; die Ringinnenwinkel an den Atomen P1, P2, C3 und C4 betragen 79,0(1); 73,5(1); 105,0(3) und 102,2(3)°.

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Tetraphenyldiphosphine disulphide (tetraphenyl-1,2-dithioxodi-λ5-phosphane), Ph2P(S)P(S)Ph2

Cited by 11 publications

References 3 publications

Phosphorus-31 nuclear magnetic resonance studies of solid diphosphine disulphides. Crystallographic considerations

Phosphorus-31 nuclear magnetic resonance studies of solid diphosphine disulphides. Crystallographic considerations

Reactivity Studies of [(thf)₂Mg{μ-C(CH₃)₂C₂H₄C(CH₃)₂}]₂: Scrambling Reactions and Diverse Reactions with Dichlorophenylphosphane

Acyl‐ und Alkylidenphosphane. XXV. Molekül‐ und Kristallstruktur des 1,2‐Di(tert‐butyl)‐3‐dimethylamino‐1‐thio‐4‐trimethylsilylsulfano‐1λ⁵,2λ³‐diphosphet‐3‐ens

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Tetraphenyldiphosphine disulphide (tetraphenyl-1,2-dithioxodi-λ5-phosphane), Ph2P(S)P(S)Ph2

Cited by 11 publications

References 3 publications

Phosphorus-31 nuclear magnetic resonance studies of solid diphosphine disulphides. Crystallographic considerations

Phosphorus-31 nuclear magnetic resonance studies of solid diphosphine disulphides. Crystallographic considerations

Reactivity Studies of [(thf)2Mg{μ-C(CH3)2C2H4C(CH3)2}]2: Scrambling Reactions and Diverse Reactions with Dichlorophenylphosphane

Acyl‐ und Alkylidenphosphane. XXV. Molekül‐ und Kristallstruktur des 1,2‐Di(tert‐butyl)‐3‐dimethylamino‐1‐thio‐4‐trimethylsilylsulfano‐1λ5,2λ3‐diphosphet‐3‐ens

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Reactivity Studies of [(thf)₂Mg{μ-C(CH₃)₂C₂H₄C(CH₃)₂}]₂: Scrambling Reactions and Diverse Reactions with Dichlorophenylphosphane

Acyl‐ und Alkylidenphosphane. XXV. Molekül‐ und Kristallstruktur des 1,2‐Di(tert‐butyl)‐3‐dimethylamino‐1‐thio‐4‐trimethylsilylsulfano‐1λ⁵,2λ³‐diphosphet‐3‐ens