1H AND 13C NMR Assignments of Artheethers

The ¹H and ¹³C nmr assignments for all hydrogen and carbon atoms were made for β and α arteethers (5 and 6) based on chemical shift theory and 2D-nmr techniques (COSY and HETCOR).     

Proton and Carbon - 13 NMR Assignments for Fluorinated and Nonfluorinated Aromatic Ketimines

The ¹H and ¹³C NMR spectra of three aromatic ketimines with varying degrees of fluoro substitution have been extensively studied using one and two dimensional techniques. COSY experiments were conducted to identify the protons on each of the aromatic groups, HETCORR experiments were then utilized to identify the corresponding carbon atoms, and then the order of the carbon atoms was established by long-range HETCORR (HRTCORRLR) results. These studies have allowed rigorous assignments to be made for most of the carbon and hydrogen atoms present in these compounds. Fluorine splittings were very helpful in the analyses. In the course of this study, the NMR absorbances (¹H and ¹³C) of related aldimines have also been assigned. This constitutes the first report on the assignments of ¹H and ¹³C absorbances for ketimines. The observed spectral properties suggest that the structure of aromatic ketimines is one in which the aromatic rings are in three different planes. Two of the aromatic rings, the N-substituted ring and the C-substituted ring in the cis configuration, are twisted substantially out of the plane with respect to the -C=N- bond. The remaining C-substituted aromatic ring, trans to the N-substituted ring, lies in the deshielding zone of the imine bond.     

NMR Studies of Hindered Rotation. The Diels-Alder Adduct of N-n-Butylmaleimide With Phencyclone: Restricted Motion of Bridgehead Phenyls

The Diels-Alder adduct of phencyclone and N-n-butylmaleimide has been prepared, and NMR studies have been carried out in CDCl₃ solution at ambient temperatures by one-and two-dimensional ¹H NMR (300 MHz) and ¹³C NMR (75 MHz) techniques. The resulting spectra appear to be consistent with slow rotation about the hindered C(sp²)-C(sp³) bonds to the bridgehead unsubstituted phenyls, i.e., slow exchange limit (SEL) spectra. Full rigorous ¹H spectral assignments have been made via high-resolution COSY experiments. The number of signals in the ¹³C NMR aryl region were also consistent with hindered phenyl rotations; preliminary ¹³C assignments are given. Striking evidence for magnetic anisotropic effects due to the phenanthrene moiety, bridging ketone carbonyl, and bridgehead phenyls are discussed, supporting endo stereochemical assignment of the adduct.     

13C NMR Assignments of the Antimalarials,Chloroquine, 4-Methylprimaquine, 5-Methoxy-4-methylprimaquine and 5-Methoxyprimaquine

The ¹³C nmr assignments for the antimalarial drugs chloroquine, 4-methyl primaquine, 5-methoxy-4-methylprimaquine and 5-methoxyprimaquine were established. These assignments were based on comparison with those of primaquine, proton-coupled data, and selective long-range proton decoupling.     

Captopril and Its Disulfide Metabolite: 13C NMR Assignments and Preferred Conformations

The ¹³C nmr assignments for captopril (1) and its disulfide mammalian metabolite (2) were made. Evidence was presented for the preferred conformations of these compounds to be in the trans forms.     

13C-NMR Assignments for Methyls and Quaternary Carbons of the Limonoid Obacunone

The high field ¹H and ¹³C resonances of obacunone were established by a series of I D and 2D NMR experiments. The ¹³C-NMR signals of the five tertiary methyl groups and all quatenary carbons were unambiguously assigned. The results confirm the stereochemical assignments at all stereogenic centres.     

First observation of F

We measured the excitation function for ¹³O + p elastic scattering to obtain data on the unknown ¹⁴F nucleus. The ground state and several low-lying excited states in ¹⁴F were observed and spin/parity assignments were made. ¹⁴F appears to be much less unstable than was predicted. We compare theoretical predictions for the ¹⁴F level scheme with the experimental results.     

Assignment of 13C Resonances in the Phencyclone-Norbornadiene Adduct Via 2D NMR. 13C Evidence for Hindered Rotation of Unsubstituted Bridgehead Phenyl Rings

¹³C NMR chemical shift assignments were obtained for the Diels-Alder adduct of phencyclone with norbornadiene in CD₂Cl₂ and in CDCl₃ solution. The ¹³C spectrum at 50.3 MHz, as well as the ¹H spectrum at 200.1 MHz, show evidence for hindered rotation of the two unsubstituted bridgehead phenyl rings of the adduct at ambient temperatures. In CD₂Cl₂ solution, all 19 of the unique ¹³C nuclei of this molecule give rise to individual ¹³C resonances. The ¹H assignments which were made earlier, together with one-bond and long-range 2D heteronuclear correlation experiments, allowed the assignment of all ¹³C chemical shifts in the molecule.     

NMR Studies of Drugs. Methaqualone. Approaches to Rigorous 1H and 13C Assignments with Applications of Achiral and Chiral Shift Reagents

The ¹H and ¹³C NMR spectra of methaqualone, 1, have been extensively studied using one and two-dimensional techniques. These 300 MHz ¹H and 75 MHz ¹³C studies have allowed rigorous assignments to be made for the methyl groups and the quinazolinone nucleus. The 60 MHz ¹H spectra for 1 in CDCl₃ have been examined with     

Kinetics of solid-state NMR cross-polarization from protons to carbon-13 in surgical sutures

Commercial Dexon surgical sutures, made of polyglycolide (PGA), were examined using ¹³C CP/MAS NMR. The study shows that detailed analysis of the cross-polarization (CP) process is useful in the peak assignments and in the assessment of molecular mobility in the polymer domains. Crystallinity of PGA in the sutures was estimated at ca. 55%.     

An Investigation of 13C-NMR Spectra of Some Intramolecular Hydrogen Bonded and Non-Bonded Azo Dyes

The ¹³C-NMR spectra of the azo dyes which were synthesized by reacting substituted benzenediazonium chloride with derivatives of some phenol have been measured. The spectral data of these compounds were described considering intramolecular hydrogen bond and not. The chemical shift assignments were made regarding substituent effects.     

Structure Elucidation of Two Acetylated Derivatives of Oligomycin A

Partial acetylation of oligomycin A (1) resulted in the formation of 5,9, 33-tri-O-acetyl (2) and 5,9,13,33-tetraacetyl (3) derivatives whose structures have been established through complete assignments of their H and ¹³C NMR spectra. These derivatives were devoid of inhibitory activity when tested on Aspergillus niger spores.     

Vibrational and Rotational Spectroscopy of 13CD3OD

We have used Fourier Transform spectral data on the C-O stretching mode of ¹³CD₃OD in order to perform a vibro-rotational analysis for this molecule. We have estimated a few molecular parameters of the ground and C-O stretching vibrational modes. Based on these parameters, and by using the Kwan-Dennison model, we propose assignments for a number of far-infrared laser transitions of ¹³CD₃OD.     

Characterization of energy levels in the nucleus170Lu

Configuration assignments are derived for the observed energy levels in the odd-odd deformed nucleus¹⁷⁰Lu₉₉ based on the calculations of the two-particle band head energies for a zero range residual interaction, the beta-feeding characteristics, and the observed features for similar bands in the neighbouring nuclei. In particular, specific assignments are given for theJ ^π =1⁺ levels at 198.4 keV, 349.0 keV and 785.5 keV. The ambiguities with respect to the assignments for theK ^π=3⁻ bands are discussed. A new isomer withJ ^π =7⁺ and half-life of several seconds is predicted around (225±25) keV and experiments are suggested to identify it.     

13CH3OH and13CD3OH optically pumped fir laser: New large offset emission and optoacoustic spectroscopy

27 new, large offset, FIR laser lines from¹³CH₃OH and one from¹³CD₃OH have been discovered by pumping with a high tunability waveguide CW CO₂ laser. Optoacoustic measurements of isotopic methyl alcohol have also been performed and the pump offsets of the new and of previously known lines have been measured and checked. Frequency tunability by Stark effect has been observed for 6 strong lines. Some assignments are discussed.     

Beta decay of 125Sb and level structures in 125Te

The decay of 2.76y ¹²⁵Sb to levels of ¹²⁵Te has been studied using an HPGe detector for gamma-ray and a mini orange electron spectrometer for conversion electron measurements. We identify 38 transitions in this decay, including 13 gamma rays and 4 conversion electron lines being reported for the first time. New results also include E1 multipolarity assignments to 3 newly observed transitions and M-shell conversion coefficient for the 109 keV M4 transition. A revised ¹²⁵Te level scheme is constructed using Ritz combination principle. While confirming the existence of 10 well established levels below 700 keV excitation, we introduce 3 other levels at 402.0, 538.6 and 652.9 keV. Interpretation of the observed levels in terms of various theoretical approaches is briefly discussed. The newly introduced 538.6 keV (1/2⁺) and 652.9 keV (3/2⁺) levels are seen as the two missing members of the (s _1/2 ⊗ 2⁺) and (d _3/2 ⊗ 2⁺) sextuplet in the quasiparticle-phonon coupling scheme.     

NMR Studies of Hindered Rotation. The Diels-Alder Adduct of Phencyclone with N-n-Propylmaleimide: Restricted Motion of Bridgehead Phenyls

The Diels-Alder adduct of phencyclone and N-n-propylmaleimide has been studied in CDCl₃ solution at ambient temperatures by one-and two-dimensional ¹H NMR (300 MHz) and ¹³C NMR (75 MHz) techniques. Clear evidence is presented from slow exchange limit (SEL) spectra for hindered rotation of the bridgehead phenyls in the adduct. Full ¹H spectral assignments have been made via selective homonuclear decoupling and high resolution COSY experiments. The number of signals in the aryl region of ¹³C NMR spectra also indicated slow rotation about the C(sp²)-C(sp³) bond to the unsubstantiated bridgehead phenyls. Striking evidence of magnetic anisotropic effects, seen from ¹H NMR, permits stereochemical assignment of the adduct as endo.     

IUPAC critical evaluation of the rotational-vibrational spectra of water vapor. Part II: Energy levels and transition wavenumbers for HDO, HDO, and HDO

This is the second of a series of articles reporting critically evaluated rotational-vibrational line positions, transition intensities, pressure dependences, and energy levels, with associated critically reviewed assignments and uncertainties, for all the main isotopologues of water. This article presents energy levels and line positions of the following singly deuterated isotopologues of water: HD¹⁶O, HD¹⁷O, and HD¹⁸O. The MARVEL (measured active rotational-vibrational energy levels) procedure is used to determine the levels, the lines, and their self-consistent uncertainties for the spectral regions 0-22 708, 0-1674, and 0-12 105 cm⁻¹ for HD¹⁶O, HD¹⁷O, and HD¹⁸O, respectively. For HD¹⁶O, 54 740 transitions were analyzed from 76 sources, the lines come from spectra recorded both at room temperature and from hot samples. These lines correspond to 36 690 distinct assignments and 8818 energy levels. For HD¹⁷O, only 485 transitions could be analyzed from three sources; the lines correspond to 162 MARVEL energy levels. For HD¹⁸O, 8729 transitions were analyzed from 11 sources and these lines correspond to 1864 energy levels. The energy levels are checked against ones determined from accurate variational nuclear motion computations employing exact kinetic energy operators. This comparison shows that the measured transitions account for about 86% of the anticipated absorbance of HD¹⁶O at 296 K and that the transitions predicted by the MARVEL energy levels account for essentially all the remaining absorbance. The extensive list of MARVEL lines and levels obtained are given in the Supplementary Material of this article, as well as in a distributed information system applied to water, W@DIS, where they can easily be retrieved. In addition, the transition and energy level information for H₂¹⁷O and H₂¹⁸O, given in the first paper of this series [Tennyson, et al. J Quant Spectr Rad Transfer 2009;110:573-96], has been updated.     

Infrared spectra of BeSO4.4H2O and its deuterated analogue at 110K in 1200–250 cm−1 region

IR absorption spectra of BeSO₄.4H₂O and its deuterated analogue are reported in the region 1200–250 cm⁻¹ at 110 K. The half-widths and relative integrated intensities of the bands are also reported. The study largely confirms the assignments for thev ₃ andv ₄ modes of SO ₄ ²⁻ ion and thev ₃ mode of Be(aq) ₄ ²⁺ , complex as made by Diemet al. The assignments of the other modes of SO ₄ ²⁻ and Be(aq) ₄ ²⁺ , and the librational modes of water are given a more solid footing as result of the present investigation.     

High spin spectroscopy of 139Pr

The high spin states in N=80 ¹³⁹Pr have been investigated by in-beam γ-spectroscopic techniques following the reaction ¹³⁰Te (¹⁴N, 5n) reaction at E=75 MeV, using a gamma detector array, consisting of seven 23% compton-suppressed high purity germanium detectors and a multiplicity ball of fourteen bismuth germanate elements. Based on γ-γ coincidence data, the level scheme of ¹³⁹Pr has been considerably extended up to 7.2 MeV excitation. Tentative spin-parity assignments are done for the newly proposed levels on the basis of the DCO ratios corresponding to strong gates and the available information from the earlier light ion experiments.