Fast growth of single-crystal covalent organic frameworks for laboratory x-ray diffraction
The imine-exchange strategy makes single-crystal growth of covalent organic frameworks (COFs) with large size (>15 microns) possible but is a time-consuming process (15 to 80 days) that has had limited success (six examples) and restricts structural characterization to synchrotron-radiation sourc...
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| Published in | Science (American Association for the Advancement of Science) Vol. 383; no. 6686; pp. 1014 - 1019 |
|---|---|
| Main Authors | , , , , , , , |
| Format | Journal Article |
| Language | English |
| Published |
United States
The American Association for the Advancement of Science
01.03.2024
|
| Subjects | |
| Online Access | Get full text |
| ISSN | 0036-8075 1095-9203 1095-9203 |
| DOI | 10.1126/science.adk8680 |
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| Abstract | The imine-exchange strategy makes single-crystal growth of covalent organic frameworks (COFs) with large size (>15 microns) possible but is a time-consuming process (15 to 80 days) that has had limited success (six examples) and restricts structural characterization to synchrotron-radiation sources for x-ray diffraction studies. We developed a CF
3
COOH/CF
3
CH
2
NH
2
protocol to harvest single-crystal COFs within 1 to 2 days with crystal sizes of up to 150 microns. The generality was exemplified by the feasible growth of 16 high-quality single-crystal COFs that were structurally determined by laboratory single-crystal x-ray diffraction with resolutions of up to 0.79 angstroms. The structures obtained included uncommon interpenetration of networks, and the details of the structural evolution of conformational isomers and host-guest interaction could be determined at the atomic level.
The production of large crystals of porous covalent organic frameworks (COFs) usually requires slow growth over weeks to avoid precursor assembly that results in defects. Han
et al
. found that large imine-linked single-crystal COFs (15 to 100 micrometers) can be grown in 1 or 2 days using trifluoroacetic acid as a catalyst and trifluoroethylamine as an intermediate reactant that is displaced by the reactant amine. This approach grew a wide variety of large COF crystals with x-ray diffraction resolutions up to 0.8 angstroms. —Phil Szuromi
A modulator-catalyst protocol enabled growth of large-sized single-crystal covalent organic frameworks within 1 to 2 days. |
|---|---|
| AbstractList | Editor’s summaryThe production of large crystals of porous covalent organic frameworks (COFs) usually requires slow growth over weeks to avoid precursor assembly that results in defects. Han et al. found that large imine-linked single-crystal COFs (15 to 100 micrometers) can be grown in 1 or 2 days using trifluoroacetic acid as a catalyst and trifluoroethylamine as an intermediate reactant that is displaced by the reactant amine. This approach grew a wide variety of large COF crystals with x-ray diffraction resolutions up to 0.8 angstroms. —Phil Szuromi The imine-exchange strategy makes single-crystal growth of covalent organic frameworks (COFs) with large size (>15 microns) possible but is a time-consuming process (15 to 80 days) that has had limited success (six examples) and restricts structural characterization to synchrotron-radiation sources for x-ray diffraction studies. We developed a CF3COOH/CF3CH2NH2 protocol to harvest single-crystal COFs within 1 to 2 days with crystal sizes of up to 150 microns. The generality was exemplified by the feasible growth of 16 high-quality single-crystal COFs that were structurally determined by laboratory single-crystal x-ray diffraction with resolutions of up to 0.79 angstroms. The structures obtained included uncommon interpenetration of networks, and the details of the structural evolution of conformational isomers and host-guest interaction could be determined at the atomic level.The imine-exchange strategy makes single-crystal growth of covalent organic frameworks (COFs) with large size (>15 microns) possible but is a time-consuming process (15 to 80 days) that has had limited success (six examples) and restricts structural characterization to synchrotron-radiation sources for x-ray diffraction studies. We developed a CF3COOH/CF3CH2NH2 protocol to harvest single-crystal COFs within 1 to 2 days with crystal sizes of up to 150 microns. The generality was exemplified by the feasible growth of 16 high-quality single-crystal COFs that were structurally determined by laboratory single-crystal x-ray diffraction with resolutions of up to 0.79 angstroms. The structures obtained included uncommon interpenetration of networks, and the details of the structural evolution of conformational isomers and host-guest interaction could be determined at the atomic level. The imine-exchange strategy makes single-crystal growth of covalent organic frameworks (COFs) with large size (>15 microns) possible but is a time-consuming process (15 to 80 days) that has had limited success (six examples) and restricts structural characterization to synchrotron-radiation sources for x-ray diffraction studies. We developed a CF 3 COOH/CF 3 CH 2 NH 2 protocol to harvest single-crystal COFs within 1 to 2 days with crystal sizes of up to 150 microns. The generality was exemplified by the feasible growth of 16 high-quality single-crystal COFs that were structurally determined by laboratory single-crystal x-ray diffraction with resolutions of up to 0.79 angstroms. The structures obtained included uncommon interpenetration of networks, and the details of the structural evolution of conformational isomers and host-guest interaction could be determined at the atomic level. The production of large crystals of porous covalent organic frameworks (COFs) usually requires slow growth over weeks to avoid precursor assembly that results in defects. Han et al . found that large imine-linked single-crystal COFs (15 to 100 micrometers) can be grown in 1 or 2 days using trifluoroacetic acid as a catalyst and trifluoroethylamine as an intermediate reactant that is displaced by the reactant amine. This approach grew a wide variety of large COF crystals with x-ray diffraction resolutions up to 0.8 angstroms. —Phil Szuromi A modulator-catalyst protocol enabled growth of large-sized single-crystal covalent organic frameworks within 1 to 2 days. The imine-exchange strategy makes single-crystal growth of covalent organic frameworks (COFs) with large size (>15 microns) possible but is a time-consuming process (15 to 80 days) that has had limited success (six examples) and restricts structural characterization to synchrotron-radiation sources for x-ray diffraction studies. We developed a CF COOH/CF CH NH protocol to harvest single-crystal COFs within 1 to 2 days with crystal sizes of up to 150 microns. The generality was exemplified by the feasible growth of 16 high-quality single-crystal COFs that were structurally determined by laboratory single-crystal x-ray diffraction with resolutions of up to 0.79 angstroms. The structures obtained included uncommon interpenetration of networks, and the details of the structural evolution of conformational isomers and host-guest interaction could be determined at the atomic level. |
| Author | Feng, Jie Wang, Wei Kang, Jia Du, Xin-Yu Han, Jing Ding, San-Yuan Liang, Lin Chen, Jie-Min |
| Author_xml | – sequence: 1 givenname: Jing orcidid: 0009-0001-3239-0299 surname: Han fullname: Han, Jing organization: State Key Laboratory of Applied Organic Chemistry, Lanzhou Magnetic Resonance Center, College of Chemistry and Chemical Engineering, Lanzhou University, Lanzhou, Gansu 730000, China – sequence: 2 givenname: Jie orcidid: 0000-0001-8047-3999 surname: Feng fullname: Feng, Jie organization: State Key Laboratory of Applied Organic Chemistry, Lanzhou Magnetic Resonance Center, College of Chemistry and Chemical Engineering, Lanzhou University, Lanzhou, Gansu 730000, China – sequence: 3 givenname: Jia orcidid: 0009-0002-4651-9732 surname: Kang fullname: Kang, Jia organization: State Key Laboratory of Applied Organic Chemistry, Lanzhou Magnetic Resonance Center, College of Chemistry and Chemical Engineering, Lanzhou University, Lanzhou, Gansu 730000, China – sequence: 4 givenname: Jie-Min surname: Chen fullname: Chen, Jie-Min organization: State Key Laboratory of Applied Organic Chemistry, Lanzhou Magnetic Resonance Center, College of Chemistry and Chemical Engineering, Lanzhou University, Lanzhou, Gansu 730000, China – sequence: 5 givenname: Xin-Yu orcidid: 0009-0007-3885-7199 surname: Du fullname: Du, Xin-Yu organization: State Key Laboratory of Applied Organic Chemistry, Lanzhou Magnetic Resonance Center, College of Chemistry and Chemical Engineering, Lanzhou University, Lanzhou, Gansu 730000, China – sequence: 6 givenname: San-Yuan surname: Ding fullname: Ding, San-Yuan organization: State Key Laboratory of Applied Organic Chemistry, Lanzhou Magnetic Resonance Center, College of Chemistry and Chemical Engineering, Lanzhou University, Lanzhou, Gansu 730000, China – sequence: 7 givenname: Lin orcidid: 0000-0002-4368-2297 surname: Liang fullname: Liang, Lin organization: State Key Laboratory of Applied Organic Chemistry, Lanzhou Magnetic Resonance Center, College of Chemistry and Chemical Engineering, Lanzhou University, Lanzhou, Gansu 730000, China., Institute of Nanoscience and Nanotechnology, School of Materials and Energy, Lanzhou University, Lanzhou, Gansu 730000, China – sequence: 8 givenname: Wei orcidid: 0000-0002-9263-7927 surname: Wang fullname: Wang, Wei organization: State Key Laboratory of Applied Organic Chemistry, Lanzhou Magnetic Resonance Center, College of Chemistry and Chemical Engineering, Lanzhou University, Lanzhou, Gansu 730000, China |
| BackLink | https://www.ncbi.nlm.nih.gov/pubmed/38422145$$D View this record in MEDLINE/PubMed |
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| Snippet | The imine-exchange strategy makes single-crystal growth of covalent organic frameworks (COFs) with large size (>15 microns) possible but is a time-consuming... Editor’s summaryThe production of large crystals of porous covalent organic frameworks (COFs) usually requires slow growth over weeks to avoid precursor... |
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| SubjectTerms | Catalysts Crystal defects Crystal growth Crystals Single crystals Trifluoroacetic acid X-ray diffraction |
| Title | Fast growth of single-crystal covalent organic frameworks for laboratory x-ray diffraction |
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