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Improving the Success Rate of Protein Crystallization by Random Microseed Matrix Screening

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Published on: August 31, 2013

Hetero-seeding and solid mixture to obtain new crystalline forms.

Dario Braga¹, Fabrizia Grepioni, Lucia Maini

¹Dipartimento di Chimica G. Ciamician, Università degli studi di Bologna, Via Selmi 2, 40126 Bologna, Italy. dario.braga@unibo.it

Chemistry (Weinheim an Der Bergstrasse, Germany)

|December 31, 2008

Summary

Hetero-seeding successfully induced a new para-methyl benzyl alcohol (p-MeBA) polymorph (p-MeBA I) isomorphous with para-chloro benzyl alcohol (p-ClBA). This crystal engineering approach overcomes limitations of conventional screening for novel crystalline forms.

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Area of Science:

Solid-state chemistry
Crystallography
Materials science

Background:

Para-methyl benzyl alcohol (p-MeBA) and para-chloro benzyl alcohol (p-ClBA) are quasi-isostructural with similar hydrogen-bonding patterns.
Despite structural similarities, their crystals are not isomorphous, and conventional screening methods failed to yield new polymorphs.

Purpose of the Study:

To investigate the potential for inducing new crystalline phases through hetero-seeding.
To explore the formation of isomorphous crystals between p-MeBA and p-ClBA.
To understand the role of functional groups in crystal structure formation.

Main Methods:

Hetero-seeding of p-MeBA solutions with p-ClBA crystals.
Conventional polymorph screening using various solvents and conditions.
Preparation of mixed crystals with varying p-MeBA/p-ClBA ratios.
Characterization using single-crystal and powder X-ray diffraction, differential scanning calorimetry, and solid-state NMR spectroscopy.

Main Results:

A new polymorph of p-MeBA (p-MeBA I) was successfully obtained via hetero-seeding with p-ClBA, exhibiting isomorphism with p-ClBA crystals.
Seeding p-ClBA with p-MeBA II did not result in a new phase isomorphous with p-MeBA II.
Mixed crystals were prepared, providing insights into the influence of functional groups on crystal packing.

Conclusions:

Hetero-seeding is an effective strategy for crystal engineering and obtaining specific polymorphs, particularly for compounds with similar structures.
The functional groups on benzyl alcohols play a crucial role in determining crystal structure and the potential for isomorphism.
This study demonstrates a targeted approach to polymorph discovery beyond conventional screening methods.