A redetermination of the crystal structure of tetramethyldiphosphine disulphide

Lee, J. D.; Goodacre, G. W.

doi:10.1107/s0567740871002139

Cited by 31 publications

(13 citation statements)

References 6 publications

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“…This indicates that through-space interactions are weak in the conformers which are more likely to occur in the gas phase, i.e. anti-planar and gauche by analogy with nmr and X-ray crystallographic data [1,2,[25][26][27][28][29], supported by our computations.…”

Section: Resultssupporting

confidence: 70%

Study of Sulfur-Sulfur Nonbonded Interactions in Substituted Diphosphine Disulfides by Gas-Phase UV Photoelectron Spectroscopy

Alagna

Cauletti

Andreocci

et al. 1981

Zeitschrift Für Naturforschung A

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Herrn Professor Hermann Hartmann zum 65. Geburtstag gewidmet Ultraviolet photoelectron spectra (UPS) of tetrasubstituted diphosphine disulfides RR'P(S)-P(S)RR' exhibit peculiar 1:2:1 splitting patterns in the region 7.5-9.5 eV for which a throughbond coupling mechanism between the sulfur lone pairs lying in the PPS planes is proposed. Further bond orbitals are related to bands at higher I. E. in the UP spectra.

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Section: Resultssupporting

confidence: 70%

Study of Sulfur-Sulfur Nonbonded Interactions in Substituted Diphosphine Disulfides by Gas-Phase UV Photoelectron Spectroscopy

Alagna

Cauletti

Andreocci

et al. 1981

Zeitschrift Für Naturforschung A

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“…The P1–P2 bond length of 225.41(8) pm lies in the expected range of diphosphanes (226.3(4) pm) which are bonded to aromatic substituents and is significantly elongated in comparison to those in aliphatic diphosphane disulfides (approximately 221(1) pm) . 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: Resultsmentioning

confidence: 98%

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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“…It is however, significantly shorter than the P=S bonds in diphosphine disulphides, e.g. 1.95-1.97 A in (III): R = R' = Me (Lee & Goodacre, 1971a). The estimate for P=S corrected for electronegativity difference is 1.92 ~ (Pauling, 1960).…”

Section: Trans-13-diethy L-24-d Iphenyl-24-dithio Cy Clo Dipho Sphmentioning

confidence: 88%

The crystal and molecular structure of trans-1,3-diethyl-2,4-diphenyl-2,4-dithiocyclophosphazane

Bullen¹,

Rütherford²,

Tucker³

1973

Acta Crystallogr Sect B

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Crystals of Ph]2 are triclinic, a= 8"06, b=9"34, c= 13.13 A, ~=93"6, t= 104.2, y=99.2 °, space group P], 2 molecules in the unit cell. The atomic positions have been determined by least-squares refinement from X-ray diffractometer intensity data, the final R being 0.095 for 3101 reflexions. The two molecules in the unit cell lie on centres a.J of symmetry at (0,0,0) and (2, z-,½) and in consequence the phosphazane ring is planar. These molecules, although not mutually related by symmetry, differ in shape only by the position of the terminal carbon atom of the ethyl group. Mean bond lengths and angles are: P-N 1.688, P-S 1.928, P-C 1-807, N-C 1.47 ~, N-P-N 83.25 °, and P-N-P 96.75 °. The geometry of the molecule is discussed in terms of steric factors.

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A redetermination of the crystal structure of tetramethyldiphosphine disulphide

Cited by 31 publications

References 6 publications

Study of Sulfur-Sulfur Nonbonded Interactions in Substituted Diphosphine Disulfides by Gas-Phase UV Photoelectron Spectroscopy

Study of Sulfur-Sulfur Nonbonded Interactions in Substituted Diphosphine Disulfides by Gas-Phase UV Photoelectron Spectroscopy

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

The crystal and molecular structure of trans-1,3-diethyl-2,4-diphenyl-2,4-dithiocyclophosphazane

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A redetermination of the crystal structure of tetramethyldiphosphine disulphide

Cited by 31 publications

References 6 publications

Study of Sulfur-Sulfur Nonbonded Interactions in Substituted Diphosphine Disulfides by Gas-Phase UV Photoelectron Spectroscopy

Study of Sulfur-Sulfur Nonbonded Interactions in Substituted Diphosphine Disulfides by Gas-Phase UV Photoelectron Spectroscopy

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

The crystal and molecular structure of trans-1,3-diethyl-2,4-diphenyl-2,4-dithiocyclophosphazane

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