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

Author

Listed:
  • 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)

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.

Suggested Citation

  • Yasuhide Inokuma & Shota Yoshioka & Junko Ariyoshi & Tatsuhiko Arai & Yuki Hitora & Kentaro Takada & Shigeki Matsunaga & Kari Rissanen & Makoto Fujita, 2013. "X-ray analysis on the nanogram to microgram scale using porous complexes," Nature, Nature, vol. 495(7442), pages 461-466, March.
    • Handle: RePEc:nat:nature:v:495:y:2013:i:7442:d:10.1038_nature11990
    DOI: 10.1038/nature11990
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    Cited by:

    1. Tomasz Poręba & Piero Macchi & Michelle Ernst, 2022. "Pitfalls in the location of guest molecules in metal-organic frameworks," Nature Communications, Nature, vol. 13(1), pages 1-3, December.
    2. Daiji Ogata & Shota Koide & Hiroyuki Kishi & Junpei Yuasa, 2024. "Direct observation of electron transfer in solids through X-ray crystallography," Nature Communications, Nature, vol. 15(1), pages 1-7, December.
    3. Yuki Wada & Pavel M. Usov & Bun Chan & Makoto Mukaida & Ken Ohmori & Yoshio Ando & Haruhiko Fuwa & Hiroyoshi Ohtsu & Masaki Kawano, 2024. "Atomic-resolution structure analysis inside an adaptable porous framework," Nature Communications, Nature, vol. 15(1), pages 1-8, December.

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