• Title/Summary/Keyword: Single crystal X-ray analysis

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A Chromo- and Fluoroionophoric Thiaoxaaza-Macrocycle Functionalized with Nitrobenzofurazan Exhibiting Mercury(II) Selectivity

  • Lee, Ji-Eun;Lee, Shim-Sung;Choi, Kyu-Seong
    • Bulletin of the Korean Chemical Society
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    • v.31 no.12
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    • pp.3707-3710
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    • 2010
  • A chromo/fluorogenic $NO_2S_2$-macrocycle L functionalized with nitrobenzofurazan unit as a dual-signaling probe was synthesized and structurally characterized by single crystal X-ray analysis. In a cation-induced color change experiment, L exhibited excellent $Hg^{2+}$ ion selectivity by showing the color change from orange-red to yellow. However, this hypochromic shift by $Hg^{2+}$ was observed for the weaker coordinating anion system such as ${NO_3}^-$ and ${ClO_4}^-$ ions. The observed anion effect is due to the strong coordination of anions inhibits the bond formation between $Hg^{2+}$ and the macrocyclic tert-N atom, which is sensitive to induce the color change. In the fluorometric experiment, L showed chelate-enhanced fluorescence change effect only with $Hg^{2+}$ ion, together with a change from yellow to green emission. The sensing ability for $Hg^{2+}$ with the proposed chemosensor L is due to the stable complexation with 1:1 stoichiometry (metal-to-ligand).

Reaction and Theoretical Study of the Coordination of an N2O-Donor Amino Alcoholic Ligand Toward Group 12 Metals Mixtures

  • Mardani, Zahra;Moeini, Keyvan;Kazemshoar-Duzduzani, Reza
    • Journal of the Korean Chemical Society
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    • v.63 no.3
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    • pp.160-165
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    • 2019
  • A series of reactions between an amino alcoholic ligand, cis-2-((2-((2-hydroxyethyl)amino)ethyl)amino)cyclohexan-1-ol (HEAC), with the mixtures of group 12 metals including, $HgCl_2/CdCl_2$, $HgCl_2/CdI_2$, $ZnCl_2/CdCl_2$ and $ZnCl_2/CdCl_2/HgCl_2$ was experimentally and theoretically studied to determine the most stable product of these reactions. Furthermore, the Cambridge Structural Database (CSD) studies were done to evaluate the theoretical results. The products were characterized by elemental analysis, FT-IR, Raman, $^1H$ NMR spectroscopy and single-crystal X-ray diffraction. Based on these investigations a binuclear structure of cadmium, [$Cd_2(HEAC)_2({\mu}-Cl)_2Cl_2$] (1), is the most stable product that was formed in all studied reactions between HEAC and metals mixtures. In this structure, the cadmium atom has a $CdN_2O({\mu}-Cl)_2Cl$ environment and distorted octahedral geometry.

Effect of C/Ti Atom Ratio on the Deformation Behavior of TiCχ Grown by FZ Method at High Temperature

  • Shin, Soon-Gi
    • Korean Journal of Materials Research
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    • v.23 no.7
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    • pp.373-378
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    • 2013
  • In order to clarify the effect of C/Ti atom ratios(${\chi}$) on the deformation behavior of $TiC_{\chi}$ at high temperature, single crystals having a wide range of ${\chi}$, from 0.56 to 0.96, were deformed by compression test in a temperature range of 1183~2273 K and in a strain rate range of $1.9{\times}10^{-4}{\sim}5.9{\times}10^{-3}s^{-1}$. Before testing, $TiC_{\chi}$ single crystals were grown by the FZ method in a He atmosphere of 0.3MPa. The concentrations of combined carbon were determined by chemical analysis and the lattice parameters by the X-ray powder diffraction technique. It was found that the high temperature deformation behavior observed is the ${\chi}$-less dependent type, including the work softening phenomenon, the critical resolved shear stress, the transition temperature where the deformation mechanism changes, the stress exponent of strain rate and activation energy for deformation. The shape of stress-strain curves of $TiC_{0.96}$, $TiC_{0.85}$ and $TiC_{0.56}$ is seen to be less dependent on ${\chi}$, the work hardening rate after the softening is slightly higher in $TiC_{0.96}$ than in $TiC_{0.85}$ and $TiC_{0.56}$. As ${\chi}$ decreases the work softening becomes less evident and the transition temperature where the work softening disappears, shifts to a lower temperature. The ${\tau}_c$ decreases monotonously with decreasing ${\chi}$ in a range of ${\chi}$ from 0.86 to 0.96. The transition temperature where the deformation mechanism changes shifts to a lower temperature as ${\chi}$ decreases. The activation energy for deformation in the low temperature region also decreased monotonously as ${\chi}$ decreased. The deformation in this temperature region is thought to be governed by the Peierls mechanism.

Study on Effect of Various Underlayer on Bilayer Agglomerlation (다양한 하지층이 이중층의 응집현상에 미치는 영향에 관한 연구)

  • Ha, J.H.;Ryu, D.H.;Im, H.W.;Jung, J.M.;Choi, H.J.;Hong, I.G.;Koh, J.H.;Koo, S.M.;Kamiko, M.;Ha, J.G.
    • Journal of the Korean Vacuum Society
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    • v.21 no.5
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    • pp.233-241
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    • 2012
  • We have deposited the bilayer consisted of the underlayer and the overlayer by using DC magnetron sputter on Single crystal MgO (001) substrate. This bilayer was fabricated at fixed annealing temperature and time. We have controlled agglomeration effect by changing of the bilayer thickness. Finally, we have made the self-organization and nano-structured film. In this processing, we have made nano-dot which consists of the underlayer and the overlayer, unlike the existing method called the agglomeration effect in the single layer. The underlayer has deposited using Ti, Cr and Co. And the overlayer has deposited with Ag. Through the analysis of Atomic force microscopy (AFM), the microstructure of underlayer is observed by AFM to confirm the formation of nano-dot. As the nano-dot through above processing, we have found that the nano-dot has the different shape. As a result, when we manufactured nano-dot through the agglomeration effect of bi-layer, the best matching material is Ti for underlayer. And also, we have found that MgO/Ti/Ag samples have been grown expitaxially toward the direction of MgO (001) by X-ray Diffraction analysis.

A Two-Dimensional Terrace-Like N-heterocyclic-Pb(II) Coordination Compound: Structure and Photoluminescence Property

  • Ma, Kui-Rong;Zhu, Yu-Lan;Zhang, Yu;Li, Rong-Qing;Cao, Li
    • Bulletin of the Korean Chemical Society
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    • v.32 no.3
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    • pp.894-898
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    • 2011
  • The first example of lead compound from $Pb(NO_3)_2$ and $H_3L$ N-heterocyclic ligand $(H_3L\;=\;(HO_2C)_2(C_3N_2)(C_3H_7)CH_2(C_6H_4)(C_6H_3)CO_2H)$, $[Pb_4(L')_4]{\cdot}5H_2O$ 1 (L' = OOC$(C_3H_7)(C_3N_2)CH_2(C_6H_4)(C_6H_3)COO)$, has been obtained under hydrothermal condition by decarboxylation, and characterized by elemental analysis, IR, TGDTA, and single-crystal X-ray diffraction. Compound 1 possesses a rare two-dimensional upper-lower offset terrace-like layer structure. In 1, crystallographic distinct Pb(II) ion adopts five-coordination geometry, and two lattice water molecules occupy the voids between 2-D layers. Results of solid state fluorescence measurement indicate that the emission band 458 nm may be assigned to $\pi^*-n$ and $\pi^*-\pi$ electronic transitions within the aromatic systems of the ligand L', however, the emission bands centred at 555 nm, 600 nm and 719 nm may be derived from phosphorescent emission ($\lambda_{excitation}$ = 390 nm).

Synthesis, Characterization and Property Studies on a Dinuclear Copper(II) Complex with Dipyridine Derivate and Acetylacetone

  • Zhao, Pu Su;Guo, Zhi Yan;Sui, Jing;Wang, Jing;Jian, Fang Fang
    • Bulletin of the Korean Chemical Society
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    • v.32 no.1
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    • pp.49-52
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    • 2011
  • A dinuclear copper(II) complex of [$Cu_2(aceace)_4$(dipyph)] [aceace = acetylacetone, dipyph = 1,4-di(4-pyridylethene-2-yl-)benzene] has been synthesized and characterized by elemental analysis, IR and X-ray single crystal diffraction. It crystallizes in the monoclinic system, space group P21/c, with lattice parameters a = 7.9584(16) $\AA$, b = 18.594(4) $\AA$, c = 15.063(4) $\AA$ $\beta=120.97(2)^o$ and $M_r$ = 807.85 ($C_{40}H_{44}Cu_2N_2O_8$), Z = 2. Each of the $Cu^{2+}$ ion adopts a square pyramid geometry and coordinates with four oxygen atoms from two aceace ligands and one nitrogen atom from dipyph bidentate ligand. Magnetic measurement shows that the Weiss constant and Curie constant for the title compound are -0.22 K and 0.1154 emu K/mol, respectively. Thermal stability data indicate that the title complex undergoes two steps decomposition and the residue is $Cu_2O_4$. In the potential range of -1.5 ~ 0.8 V, the title complex represents an irreversible electrochemical process.

Syntheses, Structures and Luminescent Properties of Two Novel M(II)-Phen-SIP Supramolecular Compounds (M = Co, Ni)

  • Zhu, Yu-Lan;Shao, Shuai;Ma, Kui-Rong;Tang, Xue-Ling;Cao, Li;Zhao, Hui-Chao
    • Bulletin of the Korean Chemical Society
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    • v.33 no.4
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    • pp.1259-1263
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    • 2012
  • Two metal compounds, $[Co(phen)_2(H_2O)_2]{\cdot}2H_2SIP{\cdot}2H_2O$ 1 and $[Ni(phen)_3]{\cdot}2H_2SIP{\cdot}3H_2O$ 2, have been obtained by incorporating 1,10-phenanthroline (phen) and 5-sulfoisophthalic acid monosodium salt ($NaH_2SIP$) ligands under hydrothermal conditions. Meanwhile, the two compounds were characterized by element analysis, IR, XRD, TG-DTA and single-crystal X-ray diffraction. Both 1 and 2 present 3D supramolecular structures via O-H${\cdots}$O hydrogen bond interactions. Luminescent properties for 1 and 2 were also studied. The compound 1 has two fluorescence emission peaks centered at 398 nm attributed to the intraligand emission from the SIP ligand and at 438 nm assigned to the combined interaction of intraligand ${\pi}^*-{\pi}$ transitions of the phen ligand and ligand-to-metal-charge-transfer (LMCT) transitions (${\lambda}_{ex}$ = 233 nm). The compound 2 shows one emission band centered at 423 nm with a shoulder peak at 434 nm which may be originated from the intraligand ${\pi}^*-{\pi}$ transitions of the phen ligand (${\lambda}_{ex}$ = 266 nm).

Crystallographic Analysis of Ar Encapsulate within Cs3-A Zeolite

  • Lim, Woo Taik;Kim, Bok Jo;Park, Jong Sam;Chang, Chang Hwan;Jung, Sung Wook;Heo, Nam Ho
    • Analytical Science and Technology
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    • v.15 no.6
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    • pp.540-549
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    • 2002
  • The arrangement of encapsulated Ar atoms in the molecular-dimensioned cavities of fully dehydrated zeolite A of unit-cell composition $Cs_3Na_8HSi_{12}Al_{12}O_{48}$ ($Cs_3$-A) has been studied crystallographically to probe the confinement effect of guest species in microporous environment. Atoms of Ar were encapsulated in the cavities of $Cs_3$-A by treatment with 410 atm of Ar at $400^{\circ}C$ for two days, followed by cooling at room temperature. The crystal structure of $Cs_3Na_8H$-A(4Ar) ($P_e$ = 410 atm, $a=12.245(2){\AA}$, $R_1=0.0543$, and $R_2=0.0552$) has been determined by single crystal X-ray diffraction technique in the cubic space group $Pm\bar{3}m$ at 21 (1) $^{\circ}C$ and 1 atm. Encapsulated Ar atoms are distributed in three crystallographic distinct positions: 1.5 Ar atoms per unit cell opposite 6-rings, 1.5 opposite four-rings in the large cavity, and finally 1.0 in the sodalite-unit. The possible structures of argon clusters, such as $Ar_2$, $Ar_3$, and $Ar_4$, are proposed.

Preparation of Ba2Mg(PO4)2:Eu Phosphors and Their Photoluminescence Properties Under UV Excitation (Ba2Mg(PO4)2:Eu 형광체의 합성과 자외선 여기하의 발광특성)

  • Tae, Se-Won;Jung, Ha-Kyun;Choi, Sung-Ho;Hur, Nam-Hwi
    • Korean Journal of Materials Research
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    • v.18 no.11
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    • pp.623-627
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    • 2008
  • For possible applications as luminescent materials for white-light emission using UV-LEDs, $Ba_2Mg(PO_4)_2:Eu^{2+}$ phosphors were prepared by a solid state reaction. The photoluminescence properties of the phosphor were investigated under ultraviolet ray (UV) excitation. The prepared phosphor powders were characterized to from a single phase of a monoclinic crystalline structure by a powder X-ray diffraction analysis. In the photoluminescence spectra, the $Ba_2Mg(PO_4)_2:Eu^{2+}$ phosphor showed an intense emission band centered at the 584 nm wavelength due to the f-d transition of the $Eu^{2+}$ activator. The optimum concentration of $Eu^{2+}$ activator in the $Ba_2Mg(PO_4)_2$ host, indicating the maximum emission intensity under the excitation of a 395 nm wavelength, was 5 at%. In addition, it was confirmed that the $Eu^{2+}$ ions are substituted at both $Ba^{2+}$ sites in the $Ba_2Mg(PO_4)_2$ crystal. On the other hand, the critical distance of energy transfer between $Eu^{2+}$ ions in the $Ba_2Mg(PO_4)_2$ host was evaluated to be approximately 19.3 A. With increasing temperature, the emission intensity of the $Ba_2Mg(PO_4)_2$:Eu phosphor was considerably decreased and the central wavelength of the emission peak was shifted toward a short wavelength.

Growth and Optical Properties of PbSnSe Epilayers Grown on BaF2(111) (PbSnSe 단결정 박막의 성장과 광학적 특성)

  • Lee, Il-Hoon
    • Journal of Korean Ophthalmic Optics Society
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    • v.9 no.1
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    • pp.35-41
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    • 2004
  • This study investigated the crystal growth, crystalline structure and the basic optical properties of $PbSnSe/BaF_2$ epilayers. The PbSnSe epilayer was grown on $BaF_2$(111) insulating substrates using a hot wall epitaxy (HWE) technique. It was found from the analysis of X-ray diffraction patterns that $PbSnSe/BaF_2$ epilayer was grown single crystal with a rock-salt structure oriented along [111] the growth direction. Using Rutherford back scattering, the atomic ratios of the PbSnSe was found to be proper stoichiometric. The best values for the full width at half maximum (FWHM) of the DCXRD was 162 arcsec for PbSnSe epilayer. The epilayer-thickness dependence of the FWHM of the DCXRD shows that the quality of the $PbSnSe/BaF_2$ is as expected. The dielectric function ${\varepsilon}(E)$ of a semiconductor is closely related to its electronic energy band structure and such relation can be drawn from features around the critical points(CPs) in the optical spectra. The real and imaginary parts(${\varepsilon}1$ and ${\varepsilon}2$) of the dielectric function ${\varepsilon}$ of PbSe were measured, and the observed spectra reveal distinct structures at energies of the E1, E2 and E3 CPs. These data are analyzed using a theoretical model known as the model dielectric function (MDF). The optical constants related to dielectric function such as the complex refractive index ($n^*=n+ik$), absorption coefficient (${\alpha}$) and normal-incidence reflectivity (R) are also presented for $PbSnSe/BaF_2$.

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