X-ray analysis on the nanogram to microgram scale using porous complexes

Yasuhide Inokuma, Shota Yoshioka, Junko Ariyoshi, Tatsuhiko Arai, Yuki Hitora, Kentaro Takada, Shigeki Matsunaga, Kari Rissanen and Makoto Fujita ()
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Yasuhide Inokuma: Graduate School of Engineering, The University of Tokyo, Hongo, Bunkyo-ku, Tokyo, 113-8656, Japan
Shota Yoshioka: Graduate School of Engineering, The University of Tokyo, Hongo, Bunkyo-ku, Tokyo, 113-8656, Japan
Junko Ariyoshi: Graduate School of Engineering, The University of Tokyo, Hongo, Bunkyo-ku, Tokyo, 113-8656, Japan
Tatsuhiko Arai: Graduate School of Engineering, The University of Tokyo, Hongo, Bunkyo-ku, Tokyo, 113-8656, Japan
Yuki Hitora: Laboratory of Aquatic Natural Products Chemistry, Graduate School of Agricultural and Life Science, The University of Tokyo, Yayoi, Bunkyo-ku, Tokyo, 113-8657, Japan
Kentaro Takada: Laboratory of Aquatic Natural Products Chemistry, Graduate School of Agricultural and Life Science, The University of Tokyo, Yayoi, Bunkyo-ku, Tokyo, 113-8657, Japan
Shigeki Matsunaga: Laboratory of Aquatic Natural Products Chemistry, Graduate School of Agricultural and Life Science, The University of Tokyo, Yayoi, Bunkyo-ku, Tokyo, 113-8657, Japan
Kari Rissanen: NanoScience Center, University of Jyväskylä, PO Box 35, 40014 Jyväskylä, Finland
Makoto Fujita: Graduate School of Engineering, The University of Tokyo, Hongo, Bunkyo-ku, Tokyo, 113-8656, Japan

Nature, 2013, vol. 495, issue 7442, 461-466

Abstract: 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.

Date: 2013
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DOI: 10.1038/nature11990

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