• Title/Summary/Keyword: crystallography

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Electron Crystallography of CaMoO4 Using High Voltage Electron Microscopy

  • Kim, Jin-Gyu;Choi, Joo-Hyoung;Jeong, Jong-Man;Kim, Young-Min;Suh, Il-Hwan;Kim, Jong-Pil;Kim, Youn-Joong
    • Bulletin of the Korean Chemical Society
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    • v.28 no.3
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    • pp.391-396
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    • 2007
  • The three-dimensional structure of an inorganic crystal, CaMoO4 (space group I 41/a, a = 5.198(69) A and c = 11.458(41) A), was determined by electron crystallography utilizing a high voltage electron microscope. An initial structure of CaMoO4 was determined with 3-D electron diffraction patterns. This structure was refined by crystallographic image processing of high resolution TEM images. X-ray crystallography of the same material was performed to evaluate the accuracy of the TEM structure determination. The cell parameters of CaMoO4 determined by electron crystallography coincide with the X-ray crystallography result to within 0.033-0.040 A, while the atomic coordinates were determined to within 0.072 A.

Recent Advances in Electron Crystallography

  • Chung, Jeong Min;Lee, Sangmin;Jung, Hyun Suk
    • Applied Microscopy
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    • v.47 no.3
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    • pp.160-164
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    • 2017
  • Electron crystallography has been used as the one of powerful tool for studying the structure of biological macromolecules at high resolution which is sufficient to provide details of intramolecular and intermolecular interactions at near-atomic level. Previously it commonly uses two-dimensional crystals that are periodic arrangement of biological molecules, however recent studies reported a novel technical approach to electron crystallography of three-dimensional crystals, called micro electron-diffraction (MicroED) which involves placing the irregular and small sized protein crystals in a transmission electron microscope to determine the atomic structure. In here, we review the advances in electron crystallography techniques with several recent studies. Furthermore, we discuss the future direction of this structural approach.

Structural Investigation of Bistrifluron Using X-Ray Crystallography, NMR Spectroscopy, and Molecular Modeling

  • Moon, Joon-Kwan;Kim, Jeong-Han;Rhee, Sang-Kee;Kim, Gang-Beom;Yun, Ho-Seop;Chung, Bong-Jin;Lee, Sang-San;Lim, Yoong-Ho
    • Bulletin of the Korean Chemical Society
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    • v.23 no.11
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    • pp.1545-1547
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    • 2002
  • A new insecticide, bistrifluron acts as an inhibitor of insect development and interferes with the cuticle formation of insects. Since it shows low acute oral and dermal toxicities, it can be one of potent insecticides. Based on X-ray crystallography, NMR spectroscopy and molecular modeling, the structural studies of bistrifluron have been carried out.

HVEM Application to Electron Crystallography: Structure Refinement of $SmZn_{0.67}Sb_2$

  • Kim, Jin-Gyu;Kim, Young-Min;Kim, Ji-Soo;Kim, Youn-Joong
    • Applied Microscopy
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    • v.36 no.spc1
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    • pp.1-7
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    • 2006
  • The three-dimensional structure of an inorganic crystal, $SmZn_{0.67}Sb_2$ (space group $P4/nmm,\;a=4.30(3){\AA}\;and\;c= 10.27(1){\AA}$), was refined by electron crystallography utilizing high voltage electron microscopy (HVEM). Effects of instrumental resolution, image quality, beam damage and specimen tilting on the structure refinement have been evaluated. The instrumental resolution and image quality were the most important factors on the final results in the structure refinement, while the beam damage and specimen tilting effects could be experimentally minimized or controlled. The average phase errors $({\Phi}_{res})$ for the [001], [100] and [110] HVEM images of $SmZn_{0.67}Sb_2$ were $10.1^{\circ},\;9.6^{\circ}\;and\;6.8^{\circ}$, respectively. The atomic coordinates of $SmZn_{0.67}Sb_2$ were consistent within $0.0013{\AA}{\sim}0.0088{\AA}$, compared to the X-ray crystallography data for the same sample.

Structural Determination of cis- and trans-5-Hydroxymethyl-5-methyl-2-thiono-r-2-ethoxy-1,3,2-dioxaphosphorinane by NMR and X-ray Crystallography: Model Compounds for the Reaction Mechanism Study of Organophosphorus Pesticides

  • Kim, Jeong Han;Toia, Robert F.;Craig, Donald C.
    • Journal of Applied Biological Chemistry
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    • v.43 no.1
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    • pp.37-43
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    • 2000
  • 1,3,2-Dioxaphosphorinanes are suitable compounds for studying the stereochemistry of substitution at phosphorus. Cis- and trans-5-hydroxymethl-5-methyl-2-thiono-2ethoxy-1,3,2-dioxaphosphorinane were prepared, and their structures and stereochemistry unambiguously assigned by NMR and X-ray crystallography with acetoxy and 3,5-dinitrobenzoyloxy derivatives, respectively. Trans isomer gave $^{31}P$ NMR signal at higher field than cis isomer, and the ring proton Spectrum of cis isomer showed characteristic pattern for identifying its geometry. In X-ray crystallography they adopted a chair conformation with the ethoxy groups in the axial positions, and the sulfide groups in the equatorial positions. A flattening of the ring around the phosphorus center was noted, the POC bond angles were about $120^{\circ}$, and the C-O bonds in the ring were significantly longer than the C-O bond for the ethoxy group or the C-O bond for hydroxyl group.

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A Conformational Comparison of 1,2-Bis(phenylthio)-o-carborane, $C_{14}H_{20}B_{10}S_2$, by X-Ray Diffraction Method and Molecular Orbital Calculation

  • Song, Kyu-Ho;Ko, Jae-Jung;Kang, Sang-Ook;Han, Won-Sik;Kwon, Soon-Nam;Suh, Il-Hwan
    • Korean Journal of Crystallography
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    • v.19 no.1
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    • pp.1-6
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    • 2008
  • The reaction of dilithio-o-carborane with dipenyl disulfide produces a phenyl thiolated o-carborane and it has been confirmed that there is conformational similarity between the structure of the compound elucidated by X-ray crystallography and that calculated by ab initio and density functional theory.

The Derivation of the Space Groups in Triclinic and Monoclinic Systems (Triclinic과 Monoclinic Systems에 속한 Space Groups의 유도)

  • 김인회;강상욱;김문집;서일환
    • Korean Journal of Crystallography
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    • v.13 no.2
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    • pp.73-81
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    • 2002
  • Triclinic system에는 2개의 point group들 1,(equation omitted), 그리고 monoclinic system에는 3개의 point groups, 2, m, 2/m 가 있는데/sup 1)/ point group들 1, 2, m은 polar point group이고 이 중의 1, 2는 enantiomorphous point group이며 point group들 (equation omitted)와 2/m은 centric point group으로 Laue group이라 일컬어진다./sup 2-4)/ 본 해설문에서는 point group들 1, (equation omitted)에서 나오는 2개의 space group들과 point group들 2, m, 2/m에서 유도되는 13개의 space group들의 좌표들을 유도하였다 . Monoclinic system에서는 unique axis b 만을 다루었고, 그리고 space group No. 14은 3가지로 해석하였으며 나머지는 standard space group만을 다루었다. 모든 space group diagram은 “International Tables for Crystallography, Volume A edited by Theo Hahn, Third revised edition published for The International Union of Crystallography by Kluwer Academic Publishers, 1992”에 기재되어 있다.