Author:
Oh Se-Woung,Bernard Guy M,Wasylishen Roderick E,McDonald Robert,Ferguson Michael J
Abstract
Variable-temperature solid-state31P,15N, and2H NMR spectroscopy, X-ray diffraction, and differential scanning calorimetry studies of the 1:1 adduct of silver nitrate and triphenylphosphine (AgNO3·PPh3) reveal a solidsolid phase transition at 300 K. The principal components of the phosphorus and nitrogen chemical shift tensors for both phases are determined from NMR spectra of MAS and stationary samples. In addition, the indirect spin-spin coupling between phosphorus and the naturally occurring isotopes of silver (107Ag and109Ag) are resolved. Experimental2H NMR line shapes for silver nitrate perdeuterated triphenylphosphine are those characteristic of rigid phenyl groups at temperatures above and below the phase-transition temperature. Powder and single-crystal X-ray diffraction data for AgNO3·PPh3obtained at 193, 295, and 313 K are reported; data obtained at 193 and 295 K are almost identical, but are significantly different from those obtained at 313 K and from an earlier single-crystal X-ray diffraction investigation performed at 298 K. All X-ray studies found that AgNO3·PPh3crystallizes in the monoclinic form, space group P21/c.Key words: 1:1 silver nitrate triphenylphosphine adduct, solid-state NMR, X-ray diffraction, phase transition.
Publisher
Canadian Science Publishing
Subject
Organic Chemistry,General Chemistry,Catalysis
Cited by
8 articles.
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