The worldwide heparin contamination crisis in 2008 led health authorities to take fundamental steps to better control heparin manufacture, including implementing appropriate analytical and bio-analytical methods to ensure production and release of high quality heparin sodium product. Consequently, there is an increased interest in the identification and structural elucidation of unusually modif...

Oxidized flavodoxin from Cyanobacterium anabaena PCC 7119 is used as a model system to investigate the fast internal dynamics of a flavin-bearing protein. Virtually complete backbone and side chain resonance NMR assignments of an oxidized flavodoxin point mutant (C55A) have been determined. Backbone and side chain dynamics in flavodoxin (C55A) were investigated using (15)N amide and deuterium m...

This paper describes an efficient and regioselective method for the synthesis of novel fluorinated spiro-heterocycles in excellent yield by cascade [5+1] double Michael addition reactions. The compounds 7,11-bis(4-fluorophenyl)-2,4-dimethyl- 2,4-diazaspiro[5.5] undecane-1,3,5,9-tetraone (3a) and 2,4-dimethyl-7,11-bis (4-(trifluoromethyl)phenyl)-2,4-diazaspiro[5.5]undecane-1,3,5,9-tetraone (3b) ...

A miniature (1.73 mm in diameter) NMR probe, which contains a magnet and a radiofrequency (RF) coil, is presented. This probe is integrated at the tip of a standard catheter and can be inserted into the human coronary arteries, creating local magnetic fields needed to obtain the NMR signal from the blood vessel walls, without the need for external magnet or RF coils. The basic theory governing ...

We elucidate local packing motifs and dynamical order parameters in a perylene tetracarboxydiimide derivative (C(8,7)-PDI), one of the most promising candidates for rationally designed, self-assembling, and self-healing molecular wires. Spectroscopic fingerprints obtained from solid-state NMR spectroscopy are interpreted by means of first-principles calculations and molecular dynamics simulatio...

Introduction: The cellular structure of living tissues is much finer than the achievable resolution of MRI images. Water molecules diffusing through the tissue explore its microstructure, but the observed signal, the sum of all spin contributions, is effectively averaged over macroscopic voxels, so that most of the subvoxel information is lost. The relevant question is which of the structural p...

Solid state 59Co nuclear magnetic resonance (NMR) spectra were recorded on diamagnetic complexes with general structure Co(Por)L2, where Por ) tetraphenylporphyrin, tetramethoxyphenylporphyrin, and octaethylporphyrin; and L ) imidazole, methylimidazole, pyridine, and isoquinoline. Measurements were carried out at different magnetic field strengths (4.7, 7.1, and 11.7 T) on both static and spinn...

The history and development of microwave spectroscopy and nuclear magnetic resonance (NMR) spectroscopy have much in common. In this Account, we discuss the less widely appreciated connections between the parameters measured using the two techniques. Selected examples from our laboratory and from the recent literature attest to the utility and importance of these connections. For example, how a...

MICE--multiple-peak identification, characterization, and estimation--is a procedure for estimating a lower bound of the number of frequency peaks and for estimating the frequency peak parameters. The leading application is protein structure determination using nuclear magnetic resonance (NMR) experiments. NMR frequency data are multiple-peak data, where each frequency peak corresponds to two c...

We demonstrate the use of two-dimensional ((13)C,(13)C) double-quantum spectroscopy to detect molecular dynamics by solid-state NMR. Data collected on tyrosine-ethylester (TEE) are in line with previously determined ((1)H,(13)C) order parameters. Application of these experiments to microcrystalline ubiquitin reveals the presence of dynamics on millisecond or faster time scales and differences i...