Optical Crystallographic Properties of Some Glucocorticoids

Ciência De Dados E Química Do Estado Sólido: Uma Plataforma Para Competitividade Da Indústria Farmoquímica E Farmacêutica Em Mercado Emergentes

“…Many works identifying solvates and polymorphs in steroid hormones date from the 1960s and 1970s. 13,14 In 1975, the monohydrate crystal structure of the 9a-Fluoro-16a-methyl-ll [I,17,21-trihydroxy-l,4-pregnadiene-3,20-dione-21-Acetate was determinate by Terzis and Theophanides. 15 According to this study, this molecule is a potent inducer of liver microsomal enzymes as well as a powerful glucocorticoid.…”

“…In relation to the statistical control of the diffraction data in order to increase confidence in measurements, Taupin [12] used the "BIAS" method and least squares method to optimize and improve accuracy of peak positions data, intensities and width from data complex numbers obtained by XRD. Afterwards, Huang [13] presented good results when using derivative methods, combining the first derivative of a cubic polynomial with the second derivative of quadratic/cubic polynomial, for precise determination of the diffraction peak position.…”

“…Taking only the 13 C CPMAS-NMR analysis into account, for both crystal structures, the number of NMR signals suggests only 1 molecule in asymmetric unit, in good agreement with the present crystallographic data. In addition, the comparison between 13 In fact, the molecular structure of dexamethasone acetate has 24 magnetically different carbons, whereas DEX-II 13 C CPMAS-NMR has only 22 signals. Taking into account the dexamethasone acetate 13 C{ 1 H} data, published by Hickey et al 41 (Table 3), the 41 does not allow an unambiguous assignment of both DEX-I and DEX-II 13 C CPMAS-NMR spectra.…”

“…In addition, DEX-II and DEX-I has 260 atoms (4 Â C 24 H 31 FO 6 .H 2 O) within its unit cell and the relaxation of the entire cell, considering the degrees of freedom of all heavy atoms, would be too computationally intensive. 13 C GIPAW shielding (s) of each polymorph was plotted versus its experimental chemical shift counterpart (Fig. 3) to achieve the It can be clearly seen from our ab initio calculations that the GIPAW approach exhibits an excellent experimental-theoretical correlation with r 2 >0.99 and a slope close to unit, j1.0282j for DEX-I and j1.0336j for DEX-II.…”

“…13 C CPMAS spectra for dexamethasone acetate (C 24 H 31 FO 6 ) polymorphs (DEX-I and DEX-II). The spinning side bands are indicated with asterisks.…”