Multinuclear solid state NMR investigation of two polymorphic forms of Ciprofloxacin-saccharinate

GARRO LINCK, YAMILA; CHATTAH, ANA KARINA; GRAF, ROBERT; ROMAÑUK, CAROLINA B.; OLIVERA, MARÍA E.; MANZO, R.H.; MONTI, GUSTAVO A.; SPIESS, HANS W.

ROYAL SOC CHEMISTRY

Lugar: Cambridge; Año: 2011 vol. 13 p. 6590 - 6590

wo polymorphic forms of a novel pharmaceutical compound, ciprofloxacin-saccharinate (CIP-SAC), are analyzed using one dimensional (1D) and two dimensional (2D) 1H nuclear magnetic resonance (NMR) at fast magic angle spinning (MAS). Additionally 15N spectroscopy and 1H-13C correlation experiments were performed to complement our conclusions. The 1D 1H NMR spectra of CIP and complexes reveal valuable information about the ionic bonding between ciprofloxacin and saccharine. Additionally, these spectra allow us to perform a clear characterization of each solid form, giving the number of molecules per unit cell in one of the polymorphs. From 2D 1H-1H spectra obtained through double quantum correlations we can arrive at important conclusions about the hydrogen bonding, conformation, and intra and inter-molecular interactions present in these compounds. Comparing and contrasting the 1H-1H correlation data obtained for both polymorphic forms and taking into account the single crystal structu