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198 Topics in Current Chemistry Editorial Board: A. de Meijere KN ...

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196 M.R. Caira<br />

INTENSITY<br />

283 K<br />

293 K<br />

303 K<br />

305 K<br />

307 K<br />

309 K<br />

311 K<br />

313 K<br />

323 K<br />

2 3 4 5 6 7 8<br />

2 q / DEGREES<br />

SOLVATE C<br />

SOLVATE A<br />

Fig. 13. In situ X-ray diffraction patterns of an antibiotic substance for crystallization range<br />

283–323 K. (Repr<strong>in</strong>ted with permission from [149])<br />

accelerate data-acquisition, enhancement of 13 C magnetisation is achieved by<br />

the CP (“cross polarization”) strategy and the comb<strong>in</strong>ed method is referred to as<br />

CPMAS NMR spectroscopy. With it, polymorphic conformational differences,<br />

crystal pack<strong>in</strong>g differences and the effects of hydrogen bond<strong>in</strong>g may be characterised.<br />

Vary<strong>in</strong>g the sample temperature allows dynamic studies of solid-solid<br />

phase transformations. Incorporation of solvents <strong>in</strong> pseudopolymorphs <strong>in</strong>troduces<br />

significant changes <strong>in</strong> local environmental magnetic effects through, e.g.,<br />

hydrogen bond<strong>in</strong>g, and such changes are therefore also open to study by the<br />

CPMAS technique.<br />

Figure 14 shows 15 N CPMAS spectra for four polymorphic modifications<br />

[150] of the imidazole <strong>de</strong>rivative (3), from which it is clear that 15 N chemical<br />

shifts are good <strong>in</strong>dices for their i<strong>de</strong>ntification. 13 C CPMAS has also recently been<br />

used to dist<strong>in</strong>guish three polymorphs of complex triacylglycerols [151]. Spectral

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