Absorbing a little water: the structural, thermodynamic, and kinetic relationship between pyrogallol and its tetarto-hydrate

Doris E Braun, Rajni M. Bhardwaj, Jean-Baptiste Arlin, Alastair J. Florence, Volker Kahlenberg, Ulrich J. Griesser, Derek A. Tocher, Sarah L. Price

Research output: Contribution to journalArticle

24 Citations (Scopus)

Abstract

The anhydrate and the stoichiometric tetartohydrate of pyrogallol (0.25 mol water per mol pyrogallol) are both storage stable at ambient conditions, provided that they are phase pure, with the system being at equilibrium at a(w) (water activity) = 0.15 at 25 degrees C. Structures have been derived from single crystal and powder X-ray diffraction data for the anhydrate and hydrate, respectively. It is notable that the tetarto-hydrate forms a tetragonal structure with water in channels, a framework that although stabilized by water, is found as a higher energy structure on a computationally generated crystal energy landscape, which has the anhydrate crystal structure as the most stable form. Thus, a combination of slurry experiments, X-ray diffraction, spectroscopy, moisture (de)sorption, and thermo-analytical methods with the computationally generated crystal energy landscape and lattice energy calculations provides a consistent picture of the finely balanced hydration behavior of pyrogallol. In addition, two monotropically related dimethyl sulfoxide monosolvates were found in the accompanying solid form screen.
LanguageEnglish
Pages4071-4083
Number of pages13
JournalCrystal Growth and Design
Volume13
Issue number9
Early online date24 Jul 2013
DOIs
Publication statusPublished - 4 Sep 2013

Fingerprint

Pyrogallol
Hydrates
hydrates
Thermodynamics
thermodynamics
Kinetics
Water
kinetics
water
Crystals
lattice energy
Dimethyl sulfoxide
energy
Dimethyl Sulfoxide
diffraction
Crystal lattices
moisture
Hydration
X ray powder diffraction
sorption

Keywords

  • anhydrous pyrogallol
  • hydrated pyrogallol
  • moisture sorption analysis

Cite this

Braun, Doris E ; Bhardwaj, Rajni M. ; Arlin, Jean-Baptiste ; Florence, Alastair J. ; Kahlenberg, Volker ; Griesser, Ulrich J. ; Tocher, Derek A. ; Price, Sarah L. / Absorbing a little water : the structural, thermodynamic, and kinetic relationship between pyrogallol and its tetarto-hydrate. In: Crystal Growth and Design. 2013 ; Vol. 13, No. 9. pp. 4071-4083.
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Braun, DE, Bhardwaj, RM, Arlin, J-B, Florence, AJ, Kahlenberg, V, Griesser, UJ, Tocher, DA & Price, SL 2013, 'Absorbing a little water: the structural, thermodynamic, and kinetic relationship between pyrogallol and its tetarto-hydrate' Crystal Growth and Design, vol. 13, no. 9, pp. 4071-4083. https://doi.org/10.1021/cg4009015

Absorbing a little water : the structural, thermodynamic, and kinetic relationship between pyrogallol and its tetarto-hydrate. / Braun, Doris E; Bhardwaj, Rajni M.; Arlin, Jean-Baptiste; Florence, Alastair J.; Kahlenberg, Volker; Griesser, Ulrich J.; Tocher, Derek A.; Price, Sarah L.

In: Crystal Growth and Design, Vol. 13, No. 9, 04.09.2013, p. 4071-4083.

Research output: Contribution to journalArticle

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T1 - Absorbing a little water

T2 - Crystal Growth and Design

AU - Braun, Doris E

AU - Bhardwaj, Rajni M.

AU - Arlin, Jean-Baptiste

AU - Florence, Alastair J.

AU - Kahlenberg, Volker

AU - Griesser, Ulrich J.

AU - Tocher, Derek A.

AU - Price, Sarah L.

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Y1 - 2013/9/4

N2 - The anhydrate and the stoichiometric tetartohydrate of pyrogallol (0.25 mol water per mol pyrogallol) are both storage stable at ambient conditions, provided that they are phase pure, with the system being at equilibrium at a(w) (water activity) = 0.15 at 25 degrees C. Structures have been derived from single crystal and powder X-ray diffraction data for the anhydrate and hydrate, respectively. It is notable that the tetarto-hydrate forms a tetragonal structure with water in channels, a framework that although stabilized by water, is found as a higher energy structure on a computationally generated crystal energy landscape, which has the anhydrate crystal structure as the most stable form. Thus, a combination of slurry experiments, X-ray diffraction, spectroscopy, moisture (de)sorption, and thermo-analytical methods with the computationally generated crystal energy landscape and lattice energy calculations provides a consistent picture of the finely balanced hydration behavior of pyrogallol. In addition, two monotropically related dimethyl sulfoxide monosolvates were found in the accompanying solid form screen.

AB - The anhydrate and the stoichiometric tetartohydrate of pyrogallol (0.25 mol water per mol pyrogallol) are both storage stable at ambient conditions, provided that they are phase pure, with the system being at equilibrium at a(w) (water activity) = 0.15 at 25 degrees C. Structures have been derived from single crystal and powder X-ray diffraction data for the anhydrate and hydrate, respectively. It is notable that the tetarto-hydrate forms a tetragonal structure with water in channels, a framework that although stabilized by water, is found as a higher energy structure on a computationally generated crystal energy landscape, which has the anhydrate crystal structure as the most stable form. Thus, a combination of slurry experiments, X-ray diffraction, spectroscopy, moisture (de)sorption, and thermo-analytical methods with the computationally generated crystal energy landscape and lattice energy calculations provides a consistent picture of the finely balanced hydration behavior of pyrogallol. In addition, two monotropically related dimethyl sulfoxide monosolvates were found in the accompanying solid form screen.

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KW - hydrated pyrogallol

KW - moisture sorption analysis

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