title: X-ray analysis on the nanogram to microgram scale using porous complexes.
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.
authors.affiliation: Department of Applied Chemistry, Graduate School of Engineering, The University of Tokyo, Hongo, Bunkyo-ku, Tokyo, 113-8656, Japan.
authors.forename: Yasuhide
authors.initials: Y
authors.lastname: Inokuma
authors.forename: Shota
authors.initials: S
authors.lastname: Yoshioka
authors.forename: Junko
authors.initials: J
authors.lastname: Ariyoshi
authors.forename: Tatsuhiko
authors.initials: T
authors.lastname: Arai
authors.forename: Yuki
authors.initials: Y
authors.lastname: Hitora
authors.forename: Kentaro
authors.initials: K
authors.lastname: Takada
authors.forename: Shigeki
authors.initials: S
authors.lastname: Matsunaga
authors.forename: Kari
authors.initials: K
authors.lastname: Rissanen
authors.forename: Makoto
authors.initials: M
authors.lastname: Fujita
mesh_terms: D000042:Absorption; D000480:Alkynes / Q000737:chemistry; D053000:Analytic Sample Preparation Methods / Q000379:methods*; D000818:Animals; D001688:Biological Products / Q000737:chemistry; D003460:Crystallization / Q000379:methods*; D018360:Crystallography, X-Ray / Q000379:methods*; D005233:Fatty Alcohols / Q000737:chemistry; D008832:Microchemistry / Q000379:methods*; D036103:Nanotechnology / Q000379:methods*; D011161:Porifera / Q000737:chemistry; D016062:Porosity
chemical_list: D000480:Alkynes; D001688:Biological Products; D005233:Fatty Alcohols
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