Polymorphs, hydrates and solvates of a co-crystal of caffeine with anthranilic acid

Acta Crystallogr B Struct Sci Cryst Eng Mater. 2014 Feb;70(Pt 1):72-80. doi: 10.1107/S2052520613033167. Epub 2014 Jan 16.

Abstract

A polymorph screen on a new 1:1 co-crystal of caffeine, C8H10N4O2, with anthranilic acid, C7H7NO2, has revealed a rich diversity of crystal forms (two polymorphs, two hydrates and seven solvates, including two sets of isostructural solvates). These forms were prepared by liquid-assisted grinding and solution crystallization, and the crystal structures of nine of these forms have been solved using either single-crystal or powder X-ray data. The structures contain O-H...N and N-H...O hydrogen bonds through which caffeine and anthranilic acid molecules assemble to form zigzag-type chains. These chains can interact in an anti-parallel and offset manner to form cage- or channel-type skeletons within which solvent molecules can be located, giving rise to the diversity of forms observed for this co-crystal. In contrast, an equivalent series of liquid-assisted grinding and solution crystallization experiments with the closely related system of theobromine, C7H8N4O2, and anthranilic acid resulted in the formation of only one 1:1 co-crystal form.

Keywords: co-crystals; hydrates; polymorphism; solvates.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Bromobenzenes / chemistry
  • Caffeine / chemistry*
  • Calorimetry, Differential Scanning
  • Central Nervous System Stimulants
  • Chlorobenzenes / chemistry
  • Crystallization
  • Crystallography, X-Ray
  • Hydrogen Bonding
  • Magnetic Resonance Spectroscopy
  • Models, Molecular
  • Molecular Conformation
  • Powder Diffraction
  • Solvents / chemistry
  • Thermogravimetry
  • Toluene / chemistry
  • Xylenes / chemistry
  • ortho-Aminobenzoates / chemistry*

Substances

  • Bromobenzenes
  • Central Nervous System Stimulants
  • Chlorobenzenes
  • Solvents
  • Xylenes
  • ortho-Aminobenzoates
  • anthranilic acid
  • Toluene
  • Caffeine
  • bromobenzene
  • chlorobenzene