Resolve crystal structures when suitable single crystals can be grown, isolated, or supplied.
Resolve crystal structures when suitable single crystals can be grown, isolated, or supplied.
We use this technique for atomic-level crystal structure determination, absolute configuration, molecular packing, and crystallographic confirmation when suitable crystals are available.
SCXRD remains the structural gold standard when the sample allows it
SCXRD is a method for determining the arrangement of atoms within a crystal, including mean atomic positions, chemical bonds, disorder, and additional crystallographic information.
SCXRD is appropriate when a diffraction-quality single crystal is available or can be grown. We offer both services. It can support molecular structure, absolute configuration, stoichiometry, hydrogen-bonding interpretation, and patent or regulatory examples when the experimental record is well documented.
Figure 1.A loop/mounting tool for retrieving and mounting small molecule/inorganic crystals suitable for SCXRD.
Reference: https://www.mitegen.com/product/loops/
Figure 2: Typical diffraction patterns from SCXRD instruments. The mounting point is shown in the center of the image. A set of consecutive diffraction images obtained with an Image Plate Scanner or a CCD detector. After several images two concentric dark circles appear, corresponding to an infinite number of reciprocal points Reference:https://www.xtal.iqf.csic.es/Cristalografia/parte_06-en.html
When you can't achieve diffraction quality single crystals: Use SCXRD and Micro Electron Diffraction (MicroED) as complementary tools
The right strategy is not SCXRD versus MicroED; it is the method that fits the material. SCXRD is preferred when high-quality single crystals are available. MicroED is a strong alternative when the material exists only as microcrystalline powder, a low-level impurity, or a form that resists large-crystal growth.
In either case, final interpretation should include phase purity, sample history, and orthogonal evidence so that the structure is connected to the development question.
SCXRD versus MicroED workflow comparison
The 2026 Triclinic MicroED workflow white paper presents a stepwise comparison showing that the SCXRD timeline is dominated by crystallization and optimization, while MicroED can move directly from microcrystalline sample to structure solution. The point is not that MicroED replaces SCXRD, but that it removes the large-single-crystal bottleneck when the available material is a powder, trace impurity, or otherwise unsuitable for conventional SCXRD. Source: Comella, George, and Boerrigter, Triclinic Labs white paper, Q2 2026. See the abstract and link below to download the whitepaper.
How the evidence fits together using orthogonal techniques
Question
Useful evidence
Decision output
Molecular identity or formula
LC/MS HR/MS, MS/MS fragments, NMR, elemental or isotope information where relevant.
Candidate formula and structure assignment with alternatives and limitations.
Crystal structure or absolute configuration
SCXRD, MicroED, crystallographic refinement, and chemistry context.
Structure solution, unit-cell or form confirmation, stereochemical interpretation when supported.
Impurity or contaminant identity
Chromatography, HRMS, MicroED if crystalline, NMR if sufficient material, Raman/IR, microscopy.
Root-cause-ready identity conclusion and evidence package.
Phase/form assignment and control or follow-up recommendation.
Examples and Publications.
These source-backed examples include author, publication date, and an abstract-level explanation.
Integrating Microcrystal Electron Diffraction as a Mainstream Work Tool in Solid Form Development and Structure Elucidation
Author: Shawn C. Comella, Gary C. George III, and Steef X.M. Boerrigter
Publication date: Q2 2026
Abstract: This Triclinic Labs white paper explains how MicroED removes the large-single-crystal bottleneck by enabling molecular structure determination directly from sub-micron crystals. It frames MicroED as a mainstream structure-elucidation workflow when integrated with expert crystallography, PXRD, HRMS, Raman/IR, and other orthogonal methods.
Microcrystal Electron Diffraction Study of Multi-component Salt and Cocrystal Forms of 3-Nitro-benzoic Acid and Pyrimethanil
Author: Stephan X.M. Boerrigter, G. Patrick Stahly, Matthias Zeller, and Christian Jandl
Publication date: Q4 2024
Abstract: This Triclinic Labs white paper reports one salt and two cocrystal forms in a 3-nitrobenzoic acid/pyrimethanil system and compares SCXRD and MicroED structure results. The example is relevant to salt/cocrystal classification, proton-position questions, and the ability of MicroED to solve a new polymorph from a single impurity particle.
Abstract: This pharmaceutical-materials example demonstrates how mechanochemistry and MicroED can be combined when suitable single crystals are difficult to obtain. It supports using MicroED as a practical structure-elucidation tool for pharmaceutical salts and solid forms.
Frequently Asked Questions about Single-Crystal X-ray Diffraction
When is single-crystal X-ray diffraction the right structure method?
SCXRD is the right starting point when a diffraction-quality single crystal is available or can reasonably be grown, isolated, and mounted. It is especially useful when the decision requires an atomic-level crystal structure, absolute-configuration support, molecular packing information, or a crystallographic confirmation of a proposed structure.
What makes a crystal suitable for SCXRD?
A suitable crystal is generally a single, well-formed crystal with adequate size, low twinning or disorder, sufficient diffraction strength, and stability under the mounting and data-collection conditions. Very small, highly defective, poorly diffracting, or mixed crystalline material may require MicroED or another orthogonal approach.
What information should I provide before sending material for SCXRD?
Provide the compound identity or suspected identity, sample history, solvent and crystallization history, available amount, expected salts or solvates, prior XRPD or microscopy images, handling sensitivities, and the decision the structure must support.
Can Triclinic grow crystals suitable for SCXRD analysis?
Yes. Triclinic can evaluate crystallization options and attempt to grow or isolate crystals suitable for SCXRD analysis when the material, quantity, purity, solubility, stability, and timeline support that work. Crystal-growth efforts may include solvent screening, slow evaporation, cooling, vapor diffusion, slurry conversion, seeding, or other small-molecule crystallization approaches. Suitability is not guaranteed because some materials form powders, oils, twinned crystals, highly disordered crystals, unstable solvates, or crystals that diffract poorly, but early crystallization assessment helps determine whether SCXRD, MicroED, or another orthogonal structure method is the best path.
When should MicroED be considered instead of SCXRD?
MicroED should be considered when the material is microcrystalline, available only as powder or particles, present at very low level, or repeatedly fails to produce crystals large enough for conventional SCXRD. SCXRD and MicroED are complementary structure tools, and the best choice depends on the physical form of the available material.
What happens if suitable single crystals cannot be grown?▾
Crystal-growth conditions can be expanded, or MicroED may be considered when microcrystalline particles are available. XRPD, NMR, spectroscopy, thermal analysis, and computational methods may also provide complementary structural evidence.
Discuss single-crystal X-ray diffraction
Share crystal availability, sample history, target structure question, prior analytical data, timeline, and whether the work supports CMC, IP, or regulatory decisions.
