Stabilizing Porous Single Crystals for Crystal Structure Analysis

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Solution Overview

Problem

The crystalline sponge method for producing crystal structure analysis samples often results in loss of single crystallinity when a single crystal is exposed to an analysis target compound solution, leading to poor quality samples, especially when the crystal is not adequately stabilized before contact.

Innovation Solution

Stabilizing single crystals by pre-exposing them to a solvent chemically identical to the analysis target compound solution, ensuring they maintain single crystallinity, and using these stabilized crystals as crystalline sponges to introduce analysis target compounds into their pores and voids.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Adaptability or versatility

If a single crystal is used as a crystalline sponge to introduce analysis target compound molecules into pores and voids, then it is possible to prepare crystal structure analysis samples without preparing a single crystal of the analysis target compound itself, but the single crystal sometimes loses single crystallinity when staying in contact with the solution containing the analysis target compound

Engineering Contradiction:
Improveability to analyze various compounds (liquid/gas, rare compounds)VSAvoidsingle crystallinity maintenance
Core Design Contradiction:
Adaptability or versatilityVSReliability

Solution Approach 1:

The patent applies preliminary action by pre-freezing the single crystal in a solvent that matches the analysis target compound solution before introducing the compound. This preliminary freezing stabilizes the crystal structure and prevents loss of single crystallinity during subsequent contact with the analysis solution, thereby resolving the contradiction between versatility and reliability.

Inventive Principle:
Principle #10Preliminary action

2Quantity of substance

If the crystalline sponge method is used to prepare crystal structure analysis samples, then a trace amount of analysis target compound is sufficient, but the single crystal may lose single crystallinity leading to poor quality samples

Engineering Contradiction:
Improveamount of analysis target compound requiredVSAvoidsample quality
Core Design Contradiction:
Quantity of substanceVSManufacturing precision

Solution Approach 1:

The patent applies preliminary action by freezing the single crystal in advance in a matching solvent before introducing the analysis target compound. This preliminary step ensures the crystal maintains its structural integrity and single crystallinity throughout the process, thereby guaranteeing high sample quality even when using only trace amounts of the analysis compound.

Inventive Principle:
Principle #10Preliminary action

3Shape

If a single crystal with fine external appearance is used, then it appears suitable for analysis, but it sometimes loses single crystallinity while in contact with the analysis solution

Engineering Contradiction:
Improveexternal appearance qualityVSAvoidsingle crystallinity stability
Core Design Contradiction:
ShapeVSReliability

Solution Approach 1:

The patent applies preliminary action by freezing the single crystal in a solvent that chemically matches the analysis solution before introducing the analysis target compound. This preliminary freezing stabilizes the crystal lattice structure, ensuring that even crystals with fine external appearance maintain their single crystallinity and structural integrity during the analysis process.

Inventive Principle:
Principle #10Preliminary action

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

This method reliably produces high-quality crystal structure analysis samples by maintaining single crystallinity and ensuring the structural integrity of the single crystal, even when exposed to the analysis target compound solution, allowing for accurate molecular structure determination.

Implementation Method 1

bringing the single crystal into contact with a solution of a compound whose molecular structure is to be determined to introduce molecules of the analysis target compound into pores and/or the voids of the single crystal

Methodology Applied
Scientific EffectAdsorption: Adsorption

Data Source

PatentUS10487420B2Single crystal of porous compound, method for assessing quality of single crystal, method for preparing solution including compound to be analyzed, method for producing crystal structure analysis sample, and method for determining molecular structure of compound to be analyzed
Publication Date: 2019.11.26 THE UNIV OF TOKYO
  • US10487420B2 patent drawing
  • US10487420B2 patent drawing
  • US10487420B2 patent drawing

AI summary

The present invention provides a single crystal of a porous compound, the single crystal being used to produce a crystal structure analysis sample for a compound to be analyzed by contacting the single crystal of the porous compound having a three-dimensional framework and three-dimensionally regularly-arranged pores and/or hollows formed by being divided by the three-dimensional framework with a solution that includes the compound to be analyzed, and arranging molecules of the compound to be analyzed in a regular array in the pores and/or hollows. The single crystal of the porous compound are characterized in that: one side of the single crystal is 10 to 2000 μm; and the single crystal maintains monocrystalline properties even after the single crystal is placed in contact with a solvent that is chemically the same as the solvent of the solution that includes the compound to be analyzed.