X-ray analysis on the nanogram to microgram scale using porous complexes
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- 27 March 2013
- journal article
- research article
- Published by Springer Science and Business Media LLC in Nature
- Vol. 495 (7442), 461-466
- https://doi.org/10.1038/nature11990
Abstract
X-ray single-crystal diffraction (SCD) analysis has the intrinsic limitation that the target molecules must be obtained as single crystals. Here we report a protocol for SCD analysis that does not require the crystallization of the sample. In our method, tiny crystals of porous complexes are soaked in a solution of the target, such that the complexes can absorb the target molecules. Crystallographic analysis clearly determines the absorbed guest structures along with the host frameworks. Because the SCD analysis is carried out on only one tiny crystal of the complex, the required sample mass is of the nanogram–microgram order. We demonstrate that as little as about 80 nanograms of a sample is enough for the SCD analysis. In combination with high-performance liquid chromatography, our protocol allows the direct characterization of multiple fractions, establishing a prototypical means of liquid chromatography SCD analysis. Furthermore, we unambiguously determined the structure of a scarce marine natural product using only 5 micrograms of the compound.Keywords
This publication has 38 references indexed in Scilit:
- Bimolecular Reaction via the Successive Introduction of Two Substrates into the Crystals of Networked Molecular CagesJournal of the American Chemical Society, 2011
- Crystalline molecular flasksNature Chemistry, 2011
- Metal−Organic Frameworks with Functional Pores for Recognition of Small MoleculesAccounts of Chemical Research, 2010
- X-ray crystallography of chemical compoundsLife Sciences, 2010
- Selective gas adsorption and separation in metal–organic frameworksChemical Society Reviews, 2009
- A short history of SHELXActa Crystallographica Section A Foundations of Crystallography, 2007
- Determination of polymethoxylated flavones in peels of selected Jamaican and Mexican citrus (Citrus spp.) cultivars by high‐performance liquid chromatographyBiomedical Chromatography, 2006
- Reticular synthesis and the design of new materialsNature, 2003
- Crystal structure of 1.ALPHA.,2.BETA.-dibromo-1,2-dihydro-.ALPHA.-santonin.Analytical Sciences, 1991
- The Stereochemistry of Santonin, β-Santonin and ArtemisinJournal of the American Chemical Society, 1955