• Title/Summary/Keyword: X-ray crystal diffraction

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Growth and Characterization of Lithium Potassium Phthalate (LiKP) Single Crystals for Third Order Nonlinear Optical Applications

  • Sivakumar, B.;Raj, S. Gokul;Kumar, G. Ramesh;Mohan, R.
    • Bulletin of the Korean Chemical Society
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    • v.33 no.11
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    • pp.3755-3760
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    • 2012
  • Single crystals of lithium potassium phthalate (LiKP) were successfully grown from aqueous solution by solvent evaporation technique. The grown crystals were characterized by single crystal X-ray diffraction. The lithium potassium phthalate $C_{16}\;H_{12}\;K\;Li_3\;O_{11}$ belongs to triclinic system with the following unit-cell dimensions at 298(2) K;$a=7.405(5){\AA}$;$b=9.878(5){\AA}$;$c=13.396(5){\AA}$;${\alpha}=71.778(5)^{\circ}$;${\beta}=87.300(5)^{\circ}$;${\gamma}=85.405(5)^{\circ}$; having a space group P1. Mass spectrometric analysis provides the molecular weight of the compound and possible ways of fragmentations occurs in the compound. Thermal stability of the crystal was also studied by both simultaneous TGA/DTA analyses. The UV-Vis-NIR spectrum shows a good transparency in the whole of Visible and as well as in the near IR range. Third order nonlinear optical studies have also been studied by Z-scan technique. Nonlinear absorption and nonlinear refractive index were found out and the third order bulk susceptibility of compound was also estimated. The results have been discussed in detail.

One-Pot Synthesis, Crystal Structures and Thermal Properties of Two Three-Dimensional Cobalt(II) Complexes

  • Tao, Bo;Lei, Wen;Cheng, Feiran;Xia, Hua
    • Bulletin of the Korean Chemical Society
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    • v.33 no.6
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    • pp.1929-1933
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    • 2012
  • Two cobalt(II) compounds $[Co(2,2{^\prime}-bipy)(H_2O)_2(SO_4)]_n$ (1) and $[Co_2(2,2^{\prime}-bipy)_2(btec)(H_2O)_6]{\cdot}2H_2O$ (2) (2,2'-bipy = 2,2'-bipyridine, $H_4btec$ = 1,2,4,5-benzenetetracarboxylic acid), have been simultaneously synthesized by a one-pot slow solvent evaporation reaction. Their structures were determined by single-crystal X-ray diffraction and further characterized by X-ray powder diffraction (XRPD), IR, elemental and thermogravimetric analysis (TGA). The structural analysis reveals that compound 1 exhibits an infinite 1D chain structure with the octahedral Co(II) centers bridging by the tetrahedral ${\mu}_2-SO{_4}^{2-}$ ligands, while compound 2 possesses a dinuclear $Co_2(2,2^{\prime}-bipy)_2(btec)(H_2O)_6$ unit and the two adjacent octahedral Co(II) ions are linked by the bismonodentately coordinated btec ligand. Additionally, compound 2 exhibits blue fluorescent emission in the solid state at room temperature.

Measurement of Crystallite Size of Method and Evaluation of Crystal Defects (X선 회절법에 의한 할로겐화 은 유제입자의 크리스탈라이트 크기 측정과 결정결함 평가에 관한 연구)

  • Bae, Chang-Hwan;Lee, Ju-Hee;Han, Chang-Suk
    • Korean Journal of Materials Research
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    • v.19 no.6
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    • pp.330-336
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    • 2009
  • The size of crystallites in mono-dispersed cubic silver bromide grains was measured by applying a powder X-ray diffraction method and Scherrer's equation to grains that were suspended in swollen gelatin layers. In order to evaluate the existence of defects, the measured crystallite size was compared to those measured by using a scanning electron microscope. In the case of the grains prepared by the controlled double jet method, the size of crystallites was equal to the edge length of the grains that had edge lengths smaller than 400 nm. This result proved the usefulness of the above-stated method for measuring the size of crystallites and also evaluating the presence of any crystal defect in each grain. In the case of the grains, which were precipitated in the presence of a sensitizing dye and potassium iodide, the size of crystallites was smaller than the edge's length, indicating the discontinuities in the grains introduced during the precipitation process.

The Crystal Structure of Acemetacin Monohrdrate $(C_{21}H_{18}NO_6Cl-H_2O)$, A Non-Steroidal Antiinflammatory Agent

  • Kim, Yang-Bae;Kim, Jeong-Ae;Park, Yeong-Il
    • Archives of Pharmacal Research
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    • v.16 no.2
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    • pp.134-139
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    • 1993
  • The molecular structure of acemetacin, 1-(4-chlorobenzoyl)-5-methoxy-2-methyl-1H-indole-3-acetic acid carboxymethyl ester, was determined by single cystal X-ray diffraction analysis. The compound was recrystallized from a mixture of acetone and water in triclinic, space group P1, with a=7.796(1), b=10.245(2), c=13.542(3)$\AA,\;\alpha=97.35(1),\;\beta=96.34(1),\;\gamma=107.06(1)^\circ$, and Z=2. The calculated density is 1.422; the observed value is $1.42\;g/cm^3$. The structure was solved by the direct method and refined by full matrix least-squares procedure to the final R value of 0,037 for 2960 independent reflections. There are water molecules, which are thought to be co-crystallized during the evaporation procedure, with the ratio of one water per compound molecule in the crystal. The conformation of the compound is found to be very similar to that of indomethacin. The molecules are stabilized by three O-H.....O type intermolecular hydrogen bonds between the oxygen of water molecule and those of the compound.

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The Growth and Characterization of GaN Films by Direct reaction of Ga and $NH_3$ (금속 갈륨과 암모니아의 직접반응에 의한 GaN 후막성장과 특성 연구)

  • Yang, Seung-Hyeon;Nam, Gi-Seok;Im, Gi-Yeong;Yang, Yeong-Seok
    • Korean Journal of Materials Research
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    • v.10 no.3
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    • pp.241-245
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    • 2000
  • Thick GaN films were grown on (0001) sapphire substrates using the direct reaction gallium and ammonia. The GaN films grew dominantly along [0002] direction, but included the growth of GaN(1010) planeq with V-shaped facetted surfaces at low temperature. With increasing growth temperature, however, the growth of GaN (1010) and (1011) planes was appeared from the films, which gives rise to the growth of hexagonal crystal with pyramid-shaped surface. The growth rate of GaN films increased with increasing growth temperature, but decreased at $1270^{\circ}C$ because the GaN films began to decompose into Ga and N at the temperature. It seemed that the crystal and optical qualities of the GaN films improve with increasing $NH_3$ flow rate. From X-ray diffraction (XRD) and photoluminescence (PL) measurements, it was observed that the yellow luminescence (YL) appeared to be significant as the peak intensity of (1010) plane of XRD spectra increased.

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Synthesis and Crystal Structures of Di-nuclear Zinc(II) Diphenate Complexes with 1,10-Phenanthroline and 2,2'-Bipyridine

  • Koo, Bon-Kweon
    • Bulletin of the Korean Chemical Society
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    • v.32 no.8
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    • pp.2617-2622
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    • 2011
  • Two new Zn(II) complexes, $[Zn_2(dpa)_2(phen)_2(H_2O)_2]{\cdot}H_2O$ (1) (dpa = dephenate, phen = 1,10-phenanthroline) and [$Zn_2(dpa)_2(bpy)_2(H_2O)_2$] (2) (bpy = 2,2'-bipyridine) have been synthesized and characterized by elemental analysis, infrared spectroscopy, thermogravimetric analysis, and single crystal X-ray diffraction. The X-ray analysis reveals that the structures of 1 and 2 are dinuclear zinc(II) complexes bridged by dpa dianions, respectively. The zinc ions in 1 exhibit a distorted square pyramidal environments, while the zinc ions in 2 exhibit a trigonal bipyramid geometry. In each complex, the dpa ligand is coordinated to zinc ions as a bis-monodentate.

Crystal Forms of Ketorolac

  • Sohn, Young-Taek;Seo, Hyun-Ok
    • Archives of Pharmacal Research
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    • v.27 no.3
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    • pp.357-360
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    • 2004
  • Four crystal forms of ketorolac have been obtained by recrystallization in organic solvents under variable conditions. Different ketorolac polymorphs and pseudo polymorph were characterized by X-ray powder diffraction crystallography (XRD), Differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). In the dissolution studies in water at $37{\pm}0.5^{\circ}C$ four crystal forms showed different patterns. The solubility of Form I were the highest. The solubility decreased in rank order: Form I> Form II > Form III > Form IV. Form land Form III were shown to have a good physical stability at room temperature for 60 days. However, Form II is converted to Form III and Form IV is converted to Form I after 60 days storage. Therefore, these observations indicate that crystalline polymorphism for ketorolac is readily inter-convertible and the relationship may have to taken into consideration in the formulation of the drug.

Growth of $NdAl_3(BO_3)_4$ Single Crystal for Miniature Solid State Laser (소형 고체 레이저용 $NdAl_3(BO_3)_4$ 단결정 육성)

  • 정선태;강진기;김정환;정수진
    • Journal of the Korean Ceramic Society
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    • v.30 no.8
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    • pp.643-650
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    • 1993
  • NdAl3(BO3)4 have been developed for miniature solid state laser material. Single crystals of NdAl3(BO3)4 were grown by TSSG technique using BaB4O7 flux. The effects of growth conditions such as cooling rate, seed orientation and rotation speed on crystal quality and the morphology were studied. At the cooling rate of 2.4$^{\circ}C$/day and the crystal rotation speed of 30~40rpm with the seed orientation in <201> or <100> directions, transparent and light violet colored crystals in size of 10$\times$15$\times$20㎣ with well developed {010}, {111}, {111}, {021}, {001}, {102}, {112}, {021} faces were obtained. By X-ray diffraction analysis, the space group was determined as C2/c, and the X-ray powder data was obtained.

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Preparation, Structure, and Photoemission Studies on the High Temperature Superconductor $YBa_2Cu_{3-x}Ni_xO_{7-{\delta}}$

  • Choy, Jin-Ho;Choe, Won-Young
    • Bulletin of the Korean Chemical Society
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    • v.11 no.5
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    • pp.379-383
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    • 1990
  • $YBa_2Cu_{3-x}Ni_xO_{7-{\delta}}$, with x = 0.05, 0.2, 0.4, 0.7 and 1.0 had been prepared by the thermal decomposition of corresponding nitrates. Among them, the sample with x = 0.05 shows above-liquid-$N_2$ temperature superconductivity with $T_c$ of 88.7K. According to the X-ray diffraction analysis, its crystal symmetry was estimated as orthorhombic with the lattice parameters of a = 3.866${\AA}$, b = 3.893${\AA}$, c = 11.715${\AA}$. The chemical composition of the sample was determined by electron probe microanalysis and the chemical composition around its grain boundaries was carefully studied by the X-ray line scanning technique. From the observed binding energy of Ni-$2p_{3/2}$ orbital electron (B.E. = 853 eV) measured by X-ray photoelectron spectroscopy, the valency state of nickel stabilized in $YBa_2Cu_{2.95}Ni_{0.05}O_{7-{\delta}}$ oxide lattice could be determined to be Ni(II).

Stage transformation characteristice of Li, K and Na-graphite intercalation compounds (Li, K과 Na-흑연 층간화합물의 stage 전이특성)

  • 오원춘;임창성;오근호;고영신
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.8 no.1
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    • pp.83-90
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    • 1998
  • Stage transformation characteristics of Li, K and Na-graphite deintercalation compounds (GDICs) were studied under consideration of a deintercalation mechanism of the intercalants between carbon layers. Li-graphite intercalation compounds (GICs) synthesized by a controlling temperatures and pressures have been spontaneously decomposed in the atmosphere. By X-ray differaction analysis the $d_{001}$-values of stage 1 and 2 were identified to be 3.71 and 7.06 $\AA$, respectively. After 6 weeks, the deintercalation reaction of the Li-GICs ceased and only residual compounds could be observed. K-GICs were synthesized by the modified two-bulb method resulting in structural stabilities and stage transitions. By X-ray diffraction analysis the very stable K-graphite residue compounds were observed after 10 weeks. Na-GICs with stage 1 and 2 were synthesized using the high temperature and pressure technique. The temperature dependence of a deintercalation reaction and a thermal stability of Na-GICs were discussed. The structure changes of the Na-GDICs depending on heating rates were identified by X-ray diffraction. According to the deintercalation process, the stage transformations could be attributed to irregular deintercalations of the GDICs with disordered stage.

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