Analysis of solid state C-13 NMR spectra of biologically active compounds

Citation
I. Wawer et S. Witkowski, Analysis of solid state C-13 NMR spectra of biologically active compounds, CURR ORG CH, 5(10), 2001, pp. 987-999
Citations number
74
Categorie Soggetti
Organic Chemistry/Polymer Science
Journal title
CURRENT ORGANIC CHEMISTRY
ISSN journal
13852728 → ACNP
Volume
5
Issue
10
Year of publication
2001
Pages
987 - 999
Database
ISI
SICI code
1385-2728(200110)5:10<987:AOSSCN>2.0.ZU;2-Y
Abstract
The characteristic features of C-13 solid state NMR applications are discus sed. The spectra are routinely measured with cross-polarisation (CP) pulse sequence and fast spinning under magic angle (MAS). Additional techniques ( dipolar dephase, variation of cross-polarisation contact time) influence th e signal intensities and enable selective observation of nonprotonated or p rotonated carbons. Solid state NMR is complementary to X-ray diffraction an d provides structural information about solids when the attempts to grow su itable single crystals have failed. However the combination of both methods is more successful in characterisation of solid state conformations and dy namic processes. Many medium sized molecules such as: saccharides, amino acids, peptides, st eroids, polyphenols (flavonoids), and tocopherol derivatives have been stud ied. Samples that are insoluble in commonly used solvents or easily decompo se in solution should be investigated by solid state NMR. Since the method can be applied to crystalline as well as to amorphous powders it is especia lly interesting tool in the studies of macromolecules. Numerous results con cerning peptides, proteins and polysaccharides are reported.