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

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Synthesis, Structures and Properties of Three Metal-organic Frameworks Based on 3-(4-((1H-imidazol-1-yl)methyl)phenyl)acrylic Acid

  • Liang, Peng;Ren, Tian-Tian;Tian, Wei-Man;Xu, Wen-Jia;Pan, Gang-Hong;Yin, Xian-Hong
    • Bulletin of the Korean Chemical Society
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    • v.35 no.1
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    • pp.182-188
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    • 2014
  • Three new transition metal complexes based on Ozagrel $[Cu(Ozagrel)]_n$ (1), $[Zn(Ozagrel)(Cl)]_n$ (2), ${[Mn_2-(Ozagrel)(1,4-ndc)_2]{\cdot}(H_2O)}_n$ (3), (Ozagrel = 3-(4-((1H-imidazol-1-yl)methyl)phenyl)acrylic acid; 1,4-ndc = 1,4-Naphthalenedicarboxylic acid) have been hydrothermally synthesized and characterized by elemental analyse, IR, TG, PXRD, electrochemical analysis and single crystal X-ray diffraction. X-ray structure analysis reveals that 1 and 3 are 3D coordination polymers, while complex 2 is a two-dimensional network polymer, the 2D layers are further packed into 3D supramolecular architectures that are connected through hydrogen bonds. The electrochemistry of 1-3 was studied by cyclic voltammetry in methanol and water using a glassy carbon working electrode. Also, thermal decomposition process and powder X-ray diffraction of complexes were investigated.

Chemical Vapor Deposition of β-LiGaO2 Films on Si(100) Using a Novel Single Precursor

  • Sung, Myung M.;Kim, Chang G.;Kim, Yun-Soo
    • Bulletin of the Korean Chemical Society
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    • v.25 no.4
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    • pp.480-484
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    • 2004
  • $LiGaO_2$ films have been grown on Si (100) substrates using a new single precursor $[Li(OCH_2CH_2OCH_3)_2-Ga(CH_3)_2]_2$ under high vacuum conditions $(5{\times}10^{-6}Torr)$. The $[Li(OCH_2CH_2OCH_3)_2Ga(CH_3)_2]_2$ was synthe-sized and characterized by using spectroscopic methods and single-crystal X-ray diffraction analysis. The chemical composition, crystalline structure, and morphology of the deposited films were investigated by X-ray photoelectron spectroscopy, X-ray diffraction, and scanning electron microscopy. The results show that polycrystalline $LiGaO_2$ films preferentially oriented in the [010] direction can be deposited on Si (100) at 500-550$^{\circ}C$ by metal organic chemical vapor deposition (MOCVD). The single precursor $[LiOCH_2CH_2OCH_3)_2-Ga(CH_3)_2]_2$ has been found suitable for chemical vapor deposition of $LiGaO_2$ thin films on Si substrates.

The Crystal Structure of a $\beta$-Allyl Type Phenylpropanoid 2-(4-allyl-2, 6-dimethoxyphenoxy)-1-(4-hydroxy-3-methoxyphenyl) propan-1-ol, from the Seeds of Myristica fragrans

  • Kim, Yang-Bae;Park, Il-Yeong;Kim, Jeong-Ae;Shin, Kuk-Hyun
    • Archives of Pharmacal Research
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    • v.14 no.2
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    • pp.137-142
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    • 1991
  • The structure of a $\beta$-allyl type phenylpropanoid was determined by single crystal X-ray diffraction analysis. The compound was recrystallized from a mixture of n-hexane and benzene in monoclinic crystal system with a = 24.782 (2), b = 10.537 (1), c = 7.871 (1) ${\AA}, \beta=95.74$ (1)$^\circ, $D_x$=1.216, $D_m$=1.22g/$cm^3$, space group $P2_1/a$, and Z=4. The structure was solved by direct method and refined by least-squares procedure to the final R value of 0.054 for 2824 observed reflections {$F{\geq}3\sigma(F)$}. The molecular geometry shows a most stable trans-form with respect to the bulky phenyls, and this conformation is settled by an intramolecular hydrogen bond. In the crystal, the molecules are arranged along with the screw axis, and stabilized by the $O{\cdot}H{\cdots}O$ type intermolecular hydrogen bonds. The other intermolecular contacts appear to be the normal van der Waals' interactions. The compound is a dimeric phenylpropanoid, and belongs to the neolignan analogues.

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Constituents of Paulownia tomentosa Stem(III): The Crystal Structure of Methyl 5-Hydroxy-dinaphtho[1,2-2',3]furan-7,12-dione-6-carboxylate

  • Park, Il-Yeong;Kim, Bak-Kwang;Kim, Yang-Bae
    • Archives of Pharmacal Research
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    • v.15 no.1
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    • pp.52-57
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    • 1992
  • The molecular structure of a natural compound was determined by single crystal X-ray diffraction analysis. The compound was isolated by methanol extraction and repeated chromatography from the stem of Paulownia tomentosa. Yellow prismatic crystals of the compound, which were recrystallized from tetrahydrofuran, are triclinic, with a = 7.310 (6), b = 10.753(6), c = 11.586(5) ${\AA}.\;\alpha= 93.30(6),\;\beta=105.62(10),\;\gamma=109.49(7)^\circ,\;D_x=1.514,\;D_m=1.51 g/cm^3$, space group P1 and Z = 2. The structure was solved by direct method, and refined by least-squares procedure to the final R-value of 0.032 for 1271 independent reflections $(F\le3\sigma{(F))}$. The compound is one of new furanquinone analogue. The molecule has a nearly planar conformation with an intramolecular hydrogen bond. In the crystal, the planar molecules are arranged as a prallel sheet-like pattern, and these stackings are stabilized by the O-H...O type intermolecular hydrogen bonds. The other intermolecular contacts appear to be the normal van der Waals interactions.

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Spectral and Geometrical Study of Two Cadmium Complexes, mer-R,S-[Cd(aepn)2]X2 (X: I-, Cl-, aepn: N-(2-Aminoethyl)-1,3-propanediamine) Supported by Solution Experiments

  • Hakimi, Mohammad;Mardani, Zahra;Moeini, Keyvan
    • Journal of the Korean Chemical Society
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    • v.57 no.4
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    • pp.447-454
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    • 2013
  • In this research, two new complexes of N-(2-aminoethyl)-1,3-propanediamine (aepn), $[Cd(aepn)_2]I_2$ (1) and $[Cd(aepn)_2]Cl_2{\cdots}H_2O$ (2), were prepared and identified by elemental analysis, FT-IR, Raman spectroscopy and single-crystal X-ray diffraction. Geometry around the cadmium atom in two complexes by coordination of six nitrogen atoms of two aepn is distorted octahedral. If distortion in the mer-$[Cd(aepn)_2]^{2+}$ cation is disregarded, it has a $C_2$ axis and $C_2$ symmetry. The cyclic voltammetry experiments were carried out to study the complexation process. Two structural surveys on coordination modes and complexes of aepn are presented. A study was carried out using CSD data to estimate the averages of bond lengths for different types of the Cd-N bonds. It was found that the intermolecular $N-H{\cdots}I$, $C-H{\cdots}I$ hydrogen bonds in 1 and $N-H{\cdots}Cl$, $N-H{\cdots}O$, $C-H{\cdots}O$, $O-H{\cdots}Cl$ in 2 stabilized the crystal networks.

Structural Analysis and Single-Crystal EPR Study of Dimeric Cu(I) Complex with TTF Derivative

  • Kwon, Sun-Young;Seo, Young-Joo;Lee, Yang-Joo;Noh, Dong-Youn;Lee, Hong-In
    • Journal of the Korean Magnetic Resonance Society
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    • v.8 no.2
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    • pp.86-95
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    • 2004
  • A Cu(I) complex with an asymmetric TTF derivative (CET-EDTTTF) is prepared from the slow-diffusion method using CET-EDTTTF and Cu(I)Br solutions and characterized by X-ray crystallography and EPR spectroscopy. Structural analysis shows Cu(I) ions are tetrahedrally coordinated to two bridging bromides, one terminal bromide, and one S atom from CET-EDTTTF. Detailed geometrical and EPR analysis identified that the dimmer molecule contains [Cu$_2Br_4]^{2-}$ anion between two [CET-EDTTTF]$^+$ radical cations. Single-crystal EPR investigation of the complex reveals that the ganisotropy is unusually big, compared to those of the previously reported TTF+ cation radicals, implying that there is significant contribution of the Cu d-orbital to the HOMO of the complex.

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Synthesis and Crystal Structures of Copper(II) Complexes with Schiff Base Ligands: [Cu2(acpy-mdtc)2(HBA)(ClO4)]·H2O and [Cu2(acpy-phtsc)2(HBA)]·ClO4

  • Koo, Bon Kweon
    • Bulletin of the Korean Chemical Society
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    • v.34 no.11
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    • pp.3233-3238
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    • 2013
  • Two new Cu(II) complexes, $[Cu_2(acpy-mdtc)_2(HBA)(ClO_4)]{\cdot}H_2O$ (1) (acpy-mdtc- = 2-acetylpyridine S-methyldithiocarbamate and $HBA^-$ = benzilic acid anion) and $[Cu_2(acpy-phtsc)_2(HBA)]{\cdot}ClO_4$ (2) (acpy-$phtsc^-$ = 2-acetylpyridine 4-phenyl-3-thiosemicarbazate) 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 copper(II) complexes bridged by two thiolate sulfur atoms of Schiff base ligand and bidentate bridging $HBA^-$ anion. For 1, each of the two copper atoms has different coordination environments. Cu1 adopts a five-coordinate square-pyramidal with a $N_2OS_2$ donor, while Cu2 exhibits a distorted octahedral geometry in a $N_2O_2S_2$ manner. For 2, two Cu(II) ions all have a five-coordinate square-pyramidal with a $N_2OS_2$ donor. In each complex, the Schiff base ligand is coordinated to copper ions as a tridentate thiol mode.

Crystal Growth and Spectroscopic Investigation of Yb,Er:$YCa_4O{(BO_3)}_3$ for 1.55$\mu m$ Laser

  • Jeong, Suk-Jong;Yu, Young-Moon
    • Proceedings of the Optical Society of Korea Conference
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    • 1999.08a
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    • pp.220-221
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    • 1999
  • Single crystals of Yttrium Calcium Oxyborate (YCOB) doped with different concentrations of Er3+ and Yb3+ ions were growth by Czochralski method. High qualities of crystals in morphology and transparency were obtained . Analysis on crystal structure and lattice parameters were performed by X-ray diffraction method. It was found that congruent melting composition is YCA4.2O1.2(BO3)3. Absorption and fluorescence properties of grown crystals were also reported.

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Vapor Phase Epitaxy of Magnesium Oxide on Si(001) Using a Single Precursor

  • Lee, Sun-Sook;Lee, Sung-Yong;Kim, Chang G.;Lee, Sang-Heon;Nah, Eun-Ju;Kim, Yunsoo
    • Proceedings of the Korean Vacuum Society Conference
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    • 2000.02a
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    • pp.122-122
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    • 2000
  • Magnesium oxide is thermodynamically very stable, has a low dielectric constant and a low refractive index, and has been widely used as substrate for growing various thin film materials, particulary oxides of the perovskite structure. There has been a considerable interest in integrating the physical properties of these oxides with semiconductor materials such as GaAs and Si. In this regard, it is considered very important to be able to grow MgO buffer layers epitaxially on the semiconductors. Various oxide films can then be grown on such buffer layers eliminating the need for using MgO single crystal substrates. Vapor phase epitaxy of magnesium oxide has been accomplished on Si(001) substrates in a high vacuum chamber using the single precursor methylmagnesium tert-butoxide in the temperature range 750-80$0^{\circ}C$. For the epitaxy of the MgO films, SiC buffer layers had to be grown on Si(001). The films were characterized by reflection high energy electron diffraction (RHEED) in situ in the growth chamber, and x-ray diffraction (XRD), x-ray pole figure analysis, scanning electron microscopy (SEM), and x-ray photoelectron spectroscopy (XPS) after the growth.

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Structural Characterization of Incommensurate Misfit Layer Compound $(LaS)_xVS_2(x\approx 1.18)$ (비정합 결정구조를 갖는 $(LaS)_xVS_2(x\approx 1.18)$의 결정구조적 특성연구)

  • 조남웅;유광수;정형진
    • Journal of the Korean Ceramic Society
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    • v.31 no.6
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    • pp.617-622
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    • 1994
  • Single crystals of misfit layered (LaS)xVS2(x 1.18) were grown using LaCl3(or I2) as a mineralizer (or transport agent) for the single crystal X-ray diffraction analysis. Procession photographs of (LaS)xVS2(x 1.18) were analyzed as the stacking structure of two kinds of LaS-and VS2-subcell. The result shows that two sublattices have common periodicities along the a*-and c*-axes, respectively, but not along the b*-axis. Sublattice dimensions of LaS and VS2 layers along b-axis were 5.67$\AA$ and 3.42$\AA$, respectively. Their ratio was 1.657 which is very close to 5/3.

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