The Latest Advances in Crystallography:

Micro crystalline Electron Diffraction (MicroED) can extract structural information from crystals that are orders of magnitude smaller than the size required for X-ray diffraction. This technique is designed to overcome single crystal growth challenges or the inability to grow crystals of suitable diffraction size.

X-ray (PXRD, XRD, SCXRD) and micro crystal electron diffraction (MicroED) are nondestructive techniques that provide detailed information about the crystallographic structure, chemical composition, and physical properties of materials. XRD relies on the dual wave/particle nature of X-rays to obtain information about the structure of crystalline and non-crystalline materials. A primary use of the technique is the identification and characterization of compounds based on their diffraction pattern. MicroED was developed as a hybrid method that exploits the advantages of both electron microscopy and crystallography. The crystals required for MicroED can often be one-billionth the size of those needed for X-ray diffraction.

Skip the months-long crystal-growing grind!

Why wait for perfect single crystals when powders can reveal atomic detail? Microcrystalline Electron Diffraction (MicroED) solves structures from crystals smaller than a grain of pollen—often overnight. Faster insights mean faster decisions for salt selection, polymorph screening, and IP protection.

Micro crystal Electron Diffraction Analysis (MicroED)-

Routinely solve high-resolution crystal structures without the need to grow large single crystals..

Application AND Technique Description

Micro crystalline Electron Diffraction (MicroED) can extract structural information from crystals that are orders of magnitude smaller than the size required for X-ray diffraction. This technique is designed to overcome single crystal growth challenges or the inability to grow crystals of suitable diffraction size. MicroED has the ability to diffract and extract high-resolution structural information from samples that resist forming large crystals while using significantly less material. Micro ED can utilize crystallite sizes in the range of 10-1000nm (for comparison Single Crystal XRD requires 1-100um). With minimal sample preparation and reduced radiation damage, Triclinic's MicroED approach is not only efficient but also gentle on your samples.

As recently as 2021, MicroED was a relatively expensive technique, required extensive sample prep, and often posed significant data processing challenges. ELDICO and Triclinic have addressed these issues with a completely redesigned instrument which is optimized to reduce electron beam damage to the molecule. The ED-1 overcomes the limitations of older Cryo-TEM systems that have been used for MicroED. The ED-1 goniometer is unique, and the instrument uses a fixed beam, continuous rotation scanning mode instead of using electron beam TEM magnets - reducing beam damage and improving diffraction results. An automated software suite allows our on site crystallographers to efficiently and cost effectively process data to generate structural configurations (determine unit cells) up to absolute configurations.

This technique can be used on a wide range of materials including complex organic compounds, catalysts, metals, ceramics, polymers, composites, thin films, nanomaterials, nanostructures, and the microstructure of semiconductor materials.

Our services include:

Assessment/Feasibility (Short electron diffraction measurement to evaluate the crystal quality and beam stability of the sample)
Electron diffraction measurement for Structure determination (Unit Cell)
Dynamical Processing and Refinement - Absolute configuration determination
Full Dynamical Refinement (Absolute configuration determination with accurate hydrogen/atom positions)

Lab Instrumentation

Model

Notes:

ELDICO

ED-1

Ideal for: Structure determination and absolute configuration.
95% probabilityof obtaining a unit cell.

• Routinely solve high-resolution crystal structures without the need to grow large single crystals.
• Accurate structure determination from <1mg of solid material and in liquids - where crystals are 10-1000nm in size.
• Accurately determine pure phase or mixtures, verify supplier starting materials.
• Micro ED can identify low level impurities/crystallinity in as received materials
• Guide Amorphous Solid Dispersio development
• Aid Process chemistry in phase ID.

Whitepaper

Q4 2024

Microcrystal Electron Diffraction Study of Multicomponent Salt and Cocrystal Forms of 3-Nitrobenzoic Acid and Pyrimethanil

Stephan X.M. Boerrigter and G. Patrick Stahly, Triclinic Labs, Lafayette IN, USA, Matthias Zeller, Purdue University, West Lafayette, IN, USA, Christian Jandl, Eldico Scientific AG, Allschwil, Switzerland.

Abstract

Three single-phase crystals containing 3-nitrobenzoic acid (NBA) and pyrimethanil (PYR) in a 1:1 stoichiometry were found, and their structures were determined. This system (NBA•PYR), whose components have a ΔpKa <1, can crystallize in one salt and two cocrystal forms. Structures were determined using both single-crystal X-ray diffraction (XRD) and microcrystal electron diffraction (microED). Both methods produced essentially equivalent crystallographic results that independently allow the solid form assignment of either salt or cocrystal. A remarkable result from the microED analysis was the complete crystal structure solution of a new polymorph of the cocrystal from a single impurity particle.

To download a copy of this Whitepaper - click here.