Search results for "Proton NMR"

Ab initio study of halogenated diphenyl ethers. NMR chemical shift prediction

2000

β-process of supercooled o-terphenyl: a comparison of dielectrical and NMR data guided by mode-coupling theory

1990

Abstract According to predictions of mode-coupling theory of the liquid-glass transition, a Cole-Cole dynamical susceptibility is applied to the β-relaxation of supercooled o -terphenyl as studied by 2 H NMR spin-lattice relaxation and by dielectrical relaxation. A temperature-dependent amplitude (1- f ) is assumed for the β-process which yields a description of the NMR data consistent with the dielectrical data. The plateau value f separating the α- and β-processes in the two-step correlation function reveals a similar temperature dependence as compared to the Debye-Waller factor.

Spectroscopic, radiochemical, and theoretical studies of the Ga3+-N-2-hydroxyethyl piperazine-N'-2-ethanesulfonic acid (HEPES buffer) system: evidenc…

2013

Recent reports have claimed a superior performance of HEPES buffer in comparison to alternative buffer systems for 67/68 Ga labeling in aqueous media. In this paper we report spectroscopic (1H and 71 Ga NMR), radiochemical, mass spectrometry and theoretical modeling studies on the Ga3+/HEPES system (HEPES = N-2-hydroxyethylpiperazine-N′-2-ethanesulfonic acid) performed with the aim of elucidating a potential contribution of HEPES in the 68/67 Ga radiolabeling process. Our results demonstrate that HEPES acts as a weakly but competitive chelator of Ga3+ and that this interaction depends on the relative Ga3+: HEPES concentration. A by-product formed in the labeling mixture has been identified …

Exceptionally long-lived light-emitting electrochemical cells: multiple intra-cation π-stacking interactions in [Ir(C^N)2(N^N)][PF6] emitters

2015

A series of cyclometalated iridium(iii) complexes [Ir(C^N)2(N^N)][PF6] (N^N = 2,2′-bipyridine (1), 6-phenyl-2,2′-bipyridine (2), 4,4′-di-tert-butyl-2,2′-bipyridine (3), 4,4′-di-tert-butyl-6-phenyl-2,2′-bipyridine (4); HC^N = 2-(3-phenyl)phenylpyridine (HPhppy) or 2-(3,5-diphenyl)phenylpyridine (HPh2ppy)) are reported. They have been synthesized using solvento precursors so as to avoid the use of chlorido-dimer intermediates, chloride ion contaminant being detrimental to the performance of [Ir(C^N)2(N^N)][PF6] emitters in light-electrochemical cell (LEC) devices. Single crystal structure determinations and variable temperature solution 1H NMR spectroscopic data confirm that the pendant pheny…

Convergence of nuclear magnetic shieldings and one‐bond 1J(11 B 1H) indirect spin–spin coupling constants in small boron molecules

2018

Self‐consistent field Hartree–Fock (SCF‐HF), density functional theory (B3LYP, KT1, KT2, and KT3), and coupled‐cluster calculations of the nuclear magnetic shielding constants of BH and BH3 molecules have been conducted to characterize the convergence of individual results obtained with correlation‐ and polarization‐consistent basis sets. The individual 11B and 1H NMR parameters were estimated in the complete basis set limit and compared with benchmark literature results. The SCF‐HF and density functional theory B3LYP predicted boron shieldings and shielding anisotropies of BH significantly differed from the results obtained by coupled‐cluster with single, double, and perturbative treatment…

1H and13C NMR spectroscopy of brominated diphenyl ethers. A multiple linear regression analysis

2000

The 1H and 13C NMR chemical shifts and 1H, 1H coupling constants of 27 brominated diphenyl ethers are reported. The increment models for the bromine substituent effects on the 1H and 13C NMR chemical shifts were constructed based on a multiple linear regression analysis. In addition to the single substituent effects, two particle increments and corrective terms for conformational effects are included in these models in order to obtain a reliable prediction of chemical shifts. Copyright © 2000 John Wiley & Sons, Ltd.

1H NMR and IR spectra of methyl dichloropropanoates and butanoates

1981

Abstract Methyl dichloropropanoates and butanoates were synthesized and their 1H NMR and IR spectra were studied. Comparisons were made with the spectral characteristics of corresponding monochlorocompounds. Special attention was given to the elucidation of the characteristic spectral features associated with particular chlorine substitution patterns. The 1H NMR of erythro and threo methyl 2,3-dichlorobutanoates were analyzed using a computer program MAOCON, a modified LAOCOON 3 program. In the spectrum of the threo form the order of the chemical shifts of protons on asymmetric carbons seems to be opposite to that reported in earlier literature. Also vicinal coupling constants J23 were foun…

Complete Spectral Analysis of the1H NMR 16-Spin System of β-Pinene

1997

The complete analysis of the 1H NMR spectrum of β-pinene, (1S)-(-)-6,6-dimethyl-2-methylenebicyclo[3.1.1]heptane, which is of the ABCDEFGHIJX3Y3 type, is reported and earlier results are corrected. The vicinal coupling constants, 3J(H,H), are compared with the theoretical values calculated by using the Altona and co-workers’ equations for the structure derived by molecular modelling. The results were applied to the conformational analysis of β-pinene. © 1997 John Wiley & Sons, Ltd.

Conformation of the galactose ring adopted in solution and in crystalline form as determined by experimental and DFT 1H NMR and single-crystal X-ray …

2003

The solution-state conformations of various galactose derivatives were determined by comparison of the experimental (1)H-(1)H vicinal coupling constants to those calculated using density functional theory (DFT) at the B3LYP/cc-pVTZ//B3LYP/6-31G(d,p) level of theory. The agreement between the experimental and calculated vicinal coupling constants for 1,2:3,4-di-O-isopropylidene-alpha-d-galactopyranose was good, thereby confirming an (O)S(2) skew conformation for it and its derivatives on the basis of their similar observed couplings. Single-crystal X-ray analysis of 1,2:3,4-di-O-isopropylidene-6-O-(3,4,6-tri-O-acetyl-2-deoxy-2-N-phthalimido-beta-d-glucopyranosyl)-alpha-d-galactopyranose and …

DSC, Dilatometric, Dielectric, and1H NMR Studies of Phase Transitions and Molecular Motions in [N(C2H5)4]3M2Cl9 (M = Sb, Bi) Crystals

1995

Results in the dependence of stoichiometry of obtained tetraethylammonium (TEA) chloroantiomonate and chlorobismuthate salts on the molar ratio of reactants used in the synthesis are presented. Seven tetraethylammonium salts are obtained: (TEA) 6 M 8 Cl 30 , TEAMCI 4 , (TEA) 3 M 2 Cl 9 (M = Sb, Bi) and (TEA) 2 SbCl 5 . Preliminary X-ray diffraction studies on (TEA) 3 M 2 Cl 9 (M = Sb, Bi) show that they are isomorphous, crystallizing at room temperature in monoclinic symmetry. The dilatometric, dielectric, and DSC studies show that (TEA) 3 Bi 2 Cl 9 undergoes two phase transitions at T c2 = 144 K and at T c1 = 322 K while (TEA) 3 Sb 2 Cl 9 undergoes three transitions at T c3 = 185, T c2 = 2…