CROSS-POLARIZATION MAGIC-ANGLE SPINNING NMR-STUDIES OF POLYMORPHISM - CORTISONE-ACETATE

被引:26
作者
HARRIS, RK
KENWRIGHT, AM
SAY, BJ
YEUNG, RR
FLETTON, RA
LANCASTER, RW
HARDGROVE, GL
机构
[1] GLAXO GRP RES LTD,GREENFORD UB6 0HE,MIDDX,ENGLAND
[2] ST OLAF COLL,DEPT CHEM,NORTHFIELD,MN 55057
来源
SPECTROCHIMICA ACTA PART A-MOLECULAR AND BIOMOLECULAR SPECTROSCOPY | 1990年 / 46卷 / 06期
关键词
D O I
10.1016/0584-8539(90)80010-V
中图分类号
O433 [光谱学];
学科分类号
0703 ; 070302 ;
摘要
13C CPMAS spectra have been recorded for nine samples of cortisone acetate (21-acetoxy-17α-hydroxy-4-pregnene-3,11,20-trione, C23H30O6) and the observed resonances are attributed to six crystalline forms. Two of these forms are novel. The spectra of all six are entirely distinct. The resonances are assigned to individual carbon atoms on the basis of previously-determined solution-state spectra together with dipolar dephasing experiments and observations of shielding anisotropies as reflected in spinning sideband manifolds. The results are interpreted in relation to known crystal structures. The value of solid-state NMR for analysis of polymorph mixtures is emphasized. © 1990.
引用
收藏
页码:927 / 935
页数:9
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