Effects of oxygen-17 and oxygen-18 on phosphorus-31 NMR: further investigation and applications

Determination of NMR interaction parameters from double rotation NMR

“…Owing to the high spectral resolution achieved via DOR, a splitting of the isotropic resonance due to 1 J OP can be clearly observed and readily determined to high accuracy ($1%). The observed 1 J OP (161 ± 2 Hz) agrees well with values measured in the 17 O MAS NMR spectrum (150 ± 20 Hz) [56] and in CDCl 3 solution (160.0 ± 2.4 Hz) [57].…”

“…Triphenylphosphine oxide (OPPh 3 ) (Ph = C 6 H 5 ) was labelled with [40%- 17 O]H 2 O following the reported method [56] and was recrystallized from acetone to produce the monoclinic polymorph [57]. DOR NMR spectra were acquired on a Chemagnetics Infinity spectrometer at an applied magnetic field of stabilized by computer control, with odd-order spinning sideband (ssb) suppression (henceforth simply denoted as 'ssb suppression') being achieved by synchronization of the excitation pulse to the outer rotor spinning frequency as described in Ref.…”

Oxygen-17 NMR spectroscopy: Basic principles and applications (part II)

“…A full line shape analysis of the experimental spectra will give T 1 (O), T 2 (X), and J OX . The theoretical treatment of Suzuki and Kubo [726] has been verified experimentally such as in the case of the 1 J( 31 PA 17 O) coupling constant [22,727,728]. Fig.…”

17O NMR investigation of phosphite hydrolysis mechanisms

“…5,6 The use of 17 O NMR spectroscopy to monitor reaction kinetics and mechanisms in biochemical phosphates and bioorganic systems has been extensively demonstrated. 9,10 The work presented here uses 17 O NMR to verify the phosphite hydrolysis mechanism proposed by Aksnes, 5 specifically for the reaction of trimethyl phosphite (TMP) with 17 O-labeled water. By monitoring the appearance of the 17 Olabeled reaction products, the mechanism is easily verified, and the kinetics directly measured and discussed.…”