Ultrafast Electron Diffraction Tomography for Structure Determination of the New Zeolite ITQ-58

Abstract

In this work a new ultrafast data collection strategy for electron diffraction tomography is presented that allows reducing data acquisition time by one order of magnitude. This methodology minimizes the radiation damage of beam-sensitive materials, such as microporous materials. This method, combined with the precession of the electron beam, provides high quality data enabling the determination of very complex structures. Most importantly, the implementation of this new electron diffraction methodology is easily affordable in any modern electron microscope. As a proof of concept, we have solved a new highly complex zeolitic structure named ITQ-58, with a very low symmetry (triclinic) and a large unit cell volume (1874.6 Å3), containing 16 silicon and 32 oxygen atoms in its asymmetric unit, which would be very difficult to solve with the state of the art techniques.

Synthesis and Structure Determination of SCM‐15: A 3D Large Pore Zeolite with Interconnected Straight 12×12×10‐Ring Channels

“…To the extent of our knowledge, it is the first large pore zeolite consisting of interconnected 12×12×10‐ring channels. Its structure was initially determined using single‐crystal electron diffraction (SCED), and refined using synchrotron powder X‐ray diffraction (SPXD) data . The framework structure of SCM‐15 is related to that of FOS‐5 ( BEC ), ITQ‐7 ( ISV ), PKU‐16 ( POS ), ITQ‐26 ( IWS ), ITQ‐21, Beta polymorph B, and SU‐78B, since this class of framework structures can all be built from similar chains which are connected by shared 4‐ring or d 4 r units and the chains themselves are also built from similar or the same building units.…”

“…Its structure was initially determined using single-crystal electron diffraction (SCED), and refinedu sing synchrotron powder X-ray diffraction (SPXD) data. [17] The framework structure of SCM-15 is related to that of FOS-5 (BEC), ITQ-7 (ISV), PKU-16 (POS), ITQ-26 (IWS), ITQ-21, Beta polymorph B, and SU-78B, [18][19][20][21][22][23][24] since this class of framework structures can all be built from similar chainsw hich are connected by shared 4-ring or d4r units and the chains themselves are also built from similaro rt he same building units. Based on the structure relationship between these frameworks, six hypothetical zeoliteswere predicted.…”

Rapid Structure Determination of Microcrystalline Molecular Compounds Using Electron Diffraction

“…[11][12][13][14] Crystals must have as ide length of at least 5-10 mmw hen using strong synchrotron radiation. [16][17][18][19][20] Microcrystalline powders outnumber single-crystal compounds by afactor of 3to4(we refer to the term "microcrystalline" as "composed of small crystals", for example,s uitable for X-ray powder diffrac-tion). [2] In some cases,t he structure may be determined by X-ray powder diffraction.…”

Schnelle Strukturaufklärung mikrokristalliner molekularer Verbindungen durch Elektronenbeugung

“…[11][12][13][14] Eine Seitenlänge von mindestens 5-10 mmi st notwendig, wenn mit starker Synchrotronstrahlung gemessen wird. [16][17][18][19][20] Verbindungen, die als mikrokristallines Pulver vorliegen, übertreffen die Anzahl monokristalliner Stoffe um das 3-bis 4-fache. [2] In manchen Fällen kann hier die Struktur durch Rçntgenpulverbeugung bestimmt werden.…”