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Sildenafil citrate data bundle Open Access

A combination of solid-state NMR techniques, including 13C/1H correlation, 2H magic-angle spinning NMR and first principles calculation are employed to characterise the role of water in different hydration states of sildenafil citrate. The 13C spectrum is fully assigned for the first time and direct correlations made with respect to the crystal structure. 2H magic-angle spinning NMR is demonstrated to be a powerful tool for the study of dynamic and exchange processes in complex hydrate systems, allowing the behaviour at multiple solvate sites to be characterised without the need for expensive and selective labelling. Use of the 2H double-quantum frequency allows resolution of the different sites and, consequently, data fitting to determine rates of spin-diffusion between the different sites. The water is shown to be highly dynamic, undergoing C2 rotation, with chemical exchange between different water molecules and also with the host structure. The methods adopted are applicable to the investigation of an extensive range of hydration types found in pharmaceutical drug substances.

Descriptions

Resource type

Dataset

Contributors

Data collector: Hodgkinson, Paul ¹
Contact person: Hodgkinson, Paul ¹
Creator: Hodgkinson, Paul ¹

¹ Durham University, UK

Funder

Engineering and Physical Sciences Research Council

Research methods

Other description

Keyword

Solid-state NMR
pharmacetical API
hydrate

Subject

Nuclear magnetic resonance spectroscopy
Pharmaceutical chemistry

Location

Language

English

Cited in

doi:10.1039/c5ce02234g

Identifier

doi:10.15128/rf55z7713
ark:/32150/rf55z7713

Rights

Creative Commons Attribution 4.0 International (CC BY)

Publisher

Durham University

Date Created

7/1/2016

File Details

Depositor

P. Hodgkinson

Date Uploaded

6 October 2015, 13:10:06

Date Modified

26 July 2016, 14:07:36

Audit Status

passing

Characterization

File format: vnd.oasis.opendocument.text (OpenDocument Text)

Mime type: application/vnd.oasis.opendocument.text

File size: 17675438

Last modified: 2016:01:07 18:06:19+00:00

Filename: SildenafilCitrate_data.zip

Original checksum: 5009ff94f9ab56eb053f792a0f54285d