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Optimizing the Growth of Endothiapepsin Crystals for Serial Crystallography Experiments

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The interplay between nucleation and patterning during shear-induced crystallization from solution in a parallel

Cedric Devos¹, Anja Vananroye¹, Ruth Cardinaels^1,2

¹KU Leuven, Department of Chemical Engineering, Celestijnenlaan 200F, 3001 Leuven, Belgium. simon.kuhn@kuleuven.be.

|July 24, 2023

Summary

Shear-induced nucleation in supersaturated solutions leads to spontaneous crystal pattern formation. Modifying plate surfaces can control these crystallization patterns, crucial for drug purification.

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Area of Science:

Chemical Engineering
Materials Science
Crystallization Science

Background:

Cooling crystallization is vital for purifying small organic molecules, particularly in pharmaceuticals.
Understanding nucleation and crystal growth is key to controlling crystallization processes.

Purpose of the Study:

To investigate shear-induced nucleation in small organic molecule solutions.
To understand the formation of mesoscale circular crystalline patterns under shear.
To explore mechanisms controlling nucleation and pattern development.

Main Methods:

Utilizing a parallel plate geometry to study crystallization under controlled shear conditions.
Analyzing nucleation events and their spatial distribution on the plate surface.
Investigating the influence of shear rate, time, and surface properties on crystallization patterns.

Main Results:

Nucleation preferentially occurred in high shear rate zones, particularly at the plate edges.
Shorter nucleation times were observed with increased mean shear rate and duration.
Circular crystalline patterns emerged at the surface, linked to heterogeneous nucleation and a proposed stick-slip motion mechanism.

Conclusions:

A novel mechanism involving crystal stick-slip motion and secondary nucleation explains pattern formation.
Heterogeneous nucleation on plate surfaces plays a critical role in initiating crystallization patterns.
Surface modification offers a method to control crystallization pattern development and purification outcomes.