Reactions of halodifluorophosphines with silver salts

Flaskerud, Gerald; Pullen, Kent E.; Shreeve, Jean’ne M.

doi:10.1021/ic50074a005

Cited by 19 publications

(3 citation statements)

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“…An ampoule was opened with an ampoule key [19] attached to the vacuum line, an appropriate amount was taken out, and then the ampoule was flame sealed again. F 2 PCl [20] was prepared by the reaction of HCl with Et 2 NPF 2 , [21] F 2 PNCO [22] from F 2 PCl and AgOCN, and F 2 PN 3 [6] from F 2 PCl and NaN 3 in toluene and was purified by vacuum trap-to-trap condensation. For the preparation of 15 Nlabeled F 2 PN 3 , 1-15 N sodium azide (98 atom-% 15 N, EURISO-TOP GmbH) was used as received.…”

Section: Discussionmentioning

confidence: 99%

Structure and Conformational Properties of Azido(difluoro)phosphane, F₂PN₃

Zeng¹,

Beckers²,

Willner³

et al. 2010

Eur J Inorg Chem

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Azido(difluoro)phosphane, F2PN3, is a colorless gas, which freezes to a glassy solid at ca. –120 °C, and the boiling point obtained by extrapolating the vapor‐pressure curve is 8 °C. It has been characterized by IR (gas phase, Ar matrix), Raman (liquid, amorphous, and crystalline solid), and 19F, 31P, 14N, and 15N NMR spectroscopy. The conformational properties of F2PN3 have been studied by vibrational spectroscopy, gas electron diffraction (GED), and quantum chemical calculations. An almost equimolar mixture of two conformers was identified in the gas and neat liquid phases, as well as in Ar matrix, for which the N3 group adopts a syn and anti orientation with respect to the bisector of the FPF angle. The syn conformer was found to be slightly more stable than the anti conformer by 2.4 ± 0.6 kJ mol–1 (ΔH°) determined by gas–phase temperature‐dependent IR spectroscopy, but in the crystalline state at low‐temperature only the anti form is observed. The very different conformational properties of F2PN3 relative to that of the previously investigated F2PNCO are discussed, guided by a natural bond orbital (NBO) analysis of electron delocalizations and steric exchange repulsions.

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Section: Discussionmentioning

confidence: 99%

Structure and Conformational Properties of Azido(difluoro)phosphane, F₂PN₃

Zeng¹,

Beckers²,

Willner³

et al. 2010

Eur J Inorg Chem

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“…Difluoro(azido)phosphine F 2 PN 3 25 and difluoro(isocyanato)phosphine F 2 PNCO26 were prepared according to literature procedures and purified by repeated fractional condensation in vacuum. For the preparation of 15 N‐labeled F 2 PN 3 , 1‐ 15 N sodium azide (98 atom % 15 N, EURISO‐TOP GmbH) was used.…”

Section: Methodsmentioning

confidence: 99%

Cavitation of liquid flow in electrospray mass spectrometry especially for addition of internal calibrant in ‘accurate mass’ measurements

Lord

Lim

2010

Rapid Comm Mass Spectrometry

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'Accurate mass' measurements in electrospray mass spectrometry are becoming more prevalent with the increasing availability of mass spectrometers with sufficient resolution. A reference compound is ideally admitted separately but almost simultaneously with the analyte and this is achieved by use of a 'dual sprayer' or voltage switching between reference and sample sprayers. This paper describes a novel third method, relying on cavitation (segmentation) of the liquid stream containing the reference compound, allowing the sample to ionise independently from the sample, thus preventing interference. The technique may also find application in kinetic experiments, such as protein folding studies. A high-performance liquid chromatography (HPLC) injector was also used to provide a reference compound, producing Gaussian-shaped profiles of varying ion intensity, thus allowing easier selection of a desirable measurement point where the intensities of the reference and analyte were similar.

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“…Spectra of the gaseous phase were obtained using a 10-cm glass cell with KBr and high-density polyethylene windows for the mid-infrared and the far-infrared, respectively. Sample pressures were approximately 5 Torr for the mid-infrared and 100 Torr for the far-infrared spectra.…”

Section: Introductionmentioning

confidence: 99%

Raman and infrared spectra of cyanodifluorophosphine

Cox¹,

Zozulin²,

Odom³

et al. 1977

Inorg. Chem.

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Reactions of halodifluorophosphines with silver salts

Cited by 19 publications

References 0 publications

Structure and Conformational Properties of Azido(difluoro)phosphane, F₂PN₃

Structure and Conformational Properties of Azido(difluoro)phosphane, F₂PN₃

Cavitation of liquid flow in electrospray mass spectrometry especially for addition of internal calibrant in ‘accurate mass’ measurements

Raman and infrared spectra of cyanodifluorophosphine

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Reactions of halodifluorophosphines with silver salts

Cited by 19 publications

References 0 publications

Structure and Conformational Properties of Azido(difluoro)phosphane, F2PN3

Structure and Conformational Properties of Azido(difluoro)phosphane, F2PN3

Cavitation of liquid flow in electrospray mass spectrometry especially for addition of internal calibrant in ‘accurate mass’ measurements

Raman and infrared spectra of cyanodifluorophosphine

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Product

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Structure and Conformational Properties of Azido(difluoro)phosphane, F₂PN₃

Structure and Conformational Properties of Azido(difluoro)phosphane, F₂PN₃