Single-crystal structure determination from microcrystalline powders (∼5 μm) by an orientation attachment mountable on an in-house X-ray diffractometer

Abstract

CrystEngComm COMMUNICATION Tsunehisa Kimura et al. Single-crystal structure determination from microcrystalline powders (~5 µm) by an orientation attachment mountable on an in-house X-ray diffractometer

X-ray diffraction from magnetically oriented microcrystal suspensions detected by a shutterless continuous rotation method

“…separated by ca 90 . The magnetic and crystallographic axes of l-alanine (orthorhombic, P2 1 2 1 2 1 , a = 6.031, b = 12.32, c = 5.78 Å ; Tsuboi et al, 2016) have the relationship a || 2 , b || 3 and c || 1 . Because the 3 axis aligns in the direction of the equator (|| rotation axis), the a and c axes appear in the meridional direction.…”

“…The three-dimensional magnetic orientation of microcrystals is achieved by rotating a suspension of microcrystals in a static magnetic field in a time-varying manner. The magnetically oriented microcrystal suspension (MOMS) is subjected to in situ X-ray measurements (Tsuboi et al, 2016) or the orientation of the microcrystals is fixed by consolidating the suspending medium to prepare a magnetically oriented microcrystal array (MOMA) that is subjected to conventional in-house (Kimura et al, 2009;Kimura et al, 2011Kimura et al, , 2014 or synchrotron (Tsukui et al, 2016) XRD measurements.…”

X-ray Single-Crystal Structural Analysis of a Magnetically Oriented Monoclinic Microcrystal Suspension of α-Glycine

“…The frequency-modulated rotation was maintained during the X-ray measurement. The details of the measurement have been reported elsewhere [7].…”

“…In this method, a microcrystal suspension is biaxially aligned using a magnetic field to obtain a "magnetically oriented microcrystal suspension" (MOMS) [5,6]. Then, the MOMS is subjected to in situ single-crystal X-ray analysis [7][8][9], or its suspending medium is consolidated to obtain a "magnetically oriented microcrystal array" (MOMA) to perform the single-crystal X-ray analysis ex situ [10,11]. The biaxial alignment was first reported by Stainer to align superconducting materials [12,13].…”

“…Those crystals belong to the orthorhombic [11,14] and monoclinic [10] systems. We also performed single-crystal structure determination of orthorhombic crystals using MOMS [7][8][9]. Magnetically aligned monoclinic microcrystals exhibit twin orientations [10], which makes the analysis of MOMA complicated (sucrose [10], cellobiose [15], and zinc citrate dihydrate [16]).…”