• Title/Summary/Keyword: single crystal X-ray crystallography

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Twist Boat Conformation of Thiane S-Oxide Both in Solid State and in Solution

  • Jeon, Dong-Ju;Kim, Ikyon
    • Bulletin of the Korean Chemical Society
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    • v.29 no.7
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    • pp.1369-1373
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    • 2008
  • A stable twist boat conformation of thiane S-oxide 1a in solid state and in solution was unambiguously determined by single crystal X-ray crystallography and solution NMR analyses. On the contrary, the thiane Sdioxide 2 which was obtained from the oxidation of corresponding thiane S-oxide 1a was confirmed to adopt a regular chair conformation.

A New Asymmetric Photoisomerization of 2,3-Dihydropyrrolo[1,2-b]benzisothiazole 5,5-Dioxides (2,3-Dihydropyrrolo[1,2-b]benzisothiazole 5,5-Dioxide들의 비대칭성 광이성질화 반응)

  • Elghamry, Ibrahim;Dopp, Dietrich
    • Journal of the Korean Chemical Society
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    • v.54 no.6
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    • pp.727-730
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    • 2010
  • A tricyclic ring system bearing new stereogenic center namely 2,3-dihydro[1]benzothieno[3,2-b]pyrrole 4,4-dioxide was synthesized by asymmetric photoisomerization of 2,3-dihydropyrrolo[1,2-b]benzisothiazole 5,5-dioxide by irradiation with 245 nm emission of the low-pressure mercury lamp. The chemical structure and the purity of the photoproduct were delineated preliminarily by IR, NMR, and MS and finally confirmed by single crystal X-ray crystallography.

Crystal Growth and Characterization of Compound Semiconductor Materials (화합물 반도체 재료의 결정성장과 특성평가)

  • 민석기
    • Korean Journal of Crystallography
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    • v.1 no.2
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    • pp.115-125
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    • 1990
  • We have investigated bulk and hetero-epitaxial growth of GaAs single crystal. Various growth techniques such as HB, HZM, and VGF for high quality bulk GaAs were successfully developed by appling the specially designed DM(direct monitoring) furnace. Al GaAs/GaAs superlattice structure and In(x)Ga(1-x) As/GaAs epilayers were also grown by MOCVD and VPE, respectively. The characterization of GaAs single crystals and epilayers was made by X-ray diffraction, Hall effect, PL, chemical etching and angle lapping technique.

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Crystal structure analysis of orthohombic $Sr_{0.6}Ca_{0.4}CuO_2$ compound (사방정계 $Sr_{0.6}Ca_{0.4}CuO_2$ 화합물의 결정구조해석)

  • Park, H.M.;Goetz, D.;Hahn, Th.
    • Korean Journal of Crystallography
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    • v.7 no.1
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    • pp.20-29
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    • 1996
  • Sr0.6Ca0.4CuO2 single crystal has been synthesized by flux method and characterized by the single crystal X-ray diffraction. The compound has the orthorhombic system and the space group is Cmcm(63), lattice parameters are a=3.4645Å, b=16.1417Å, c=3.8727Å. In the (Sr1-xCax)CuO2 compound the limit of Ca from substitution for Sr was determined by the change of bond length. For this, X-ray diffraction, scanning electron microscopy (SEM), energy dispersive X-ray fluorescence (EDAX) and electron probe micro-analysis (EPMA) were used. From the change of Cu-O bond length as the Ca substitution, we concluded the limit of Ca incorporation Xca≒0.73.

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Crystal Structure Analysis of 3-(4-ethylphenyl)-3H-chromeno[4,3-c]isoxazole-3a(4H)-carbonitrile

  • Malathy, P.;Ganapathy, Jagadeesan;Srinivasan, J.;Manickam, Bakthadoss
    • Journal of Integrative Natural Science
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    • v.8 no.4
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    • pp.250-257
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    • 2015
  • The crystal structure of the potential active 3-(4-ethylphenyl)-3H-chromeno[4,3-c]isoxazole-3a(4H)-carbonitrile ($C_{19}H_{16}N_2O_2$) has been determined from single crystal X-ray diffraction data. In the title compound crystallizes in the monoclinic space group $P2_1/c$ with unit cell dimension a=6.6869 (8) ${\AA}$, b=15.8326 (19) ${\AA}$ and c= 15.237 (2) ${\AA}$ [${\alpha}=90^{\circ}$, ${\beta}=100.663^{\circ}$ and ${\gamma}=90^{\circ}$]. In the structure chromene, isoxazole and carboxylate are almost coplanar each other. All geometrical parameters revelled that chromene ring of pyran ring adopt sofa conformation. The crystal packing is stabilized by intermolecular C-H...N and C-H...O hydrogen bond interaction.

Crystal Structure Analysis of 6-Ethoxy-3-phenyl-5a,9a-dihydro-3H-chromen[4,3-c][1,2]oxazole-3a(4H)-carbonitrile

  • Malathy, P.;Sharmila, P.;Srinivasan, J.;Manickam, Bakthadoss;Aravindhan, S.
    • Journal of Integrative Natural Science
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    • v.9 no.2
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    • pp.94-102
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    • 2016
  • The crystal structure of the potential active 6-ethoxy-3-phenyl-5a,9a-dihydro-3H-chromen[4,3-c][1,2]oxazole-3a(4H)-carbonitrile ($C_{19}H_{15}N_2O_3$) has been determined from single crystal X-ray diffraction technique. The title compound crystallizes in the monoclinic space group C2/c with unit cell dimension a= 29.3026(9) ${\AA}$, b= 6.7695(2) ${\AA}$ and c= 19.7597(6) ${\AA}$ [${\alpha}= 90^{\circ}$, ${\beta}= 125.709(10)^{\circ}$ and ${\gamma}= 90^{\circ}$]. Single crystals suitable for X-ray diffraction were obtained by slow evaporation method, the isoxazole and six membered pyran rings adopts envelope conformation. The crystal packing of the molecules is stabilized by the weak $C-H{\ldots}N$ hydrogen bond interaction.

Crystal Structure Analysis of Methyl 8-bromo-3-phenyl-5a,9a-dihydro-3H-chromen [4,3-c][1,2] isoxazole-3a(4H)-carboxylate

  • Malathy, P.;Sharmila, P.;Srinivasan, J.;Manickam, Bakthadoss;Aravindhan, S.
    • Journal of Integrative Natural Science
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    • v.9 no.2
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    • pp.103-112
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    • 2016
  • The crystal structure of the potential active Methyl 8-bromo-3-phenyl-5a,9a-dihydro-3H-chromen [4,3-c][1,2] isoxazole-3a(4H)-carboxylate ($C_{18}H_{15}BrNO_4$) has been determined from single crystal X-ray diffraction technique. The title compound crystallizes in the triclinic space group Pī with unit cell dimension a=8.3129 (3) ${\AA}$, b=9.5847 (4) ${\AA}$ and c=11.1463(4) ${\AA}$ [${\alpha}=98.457(3)^{\circ}$, ${\beta}=102.806(2)^{\circ}$ and ${\gamma}=105.033(5)^{\circ}$]. Single crystals suitable for X-ray diffraction were obtained by slow evaporation method, the isoxazole and six membered pyran rings adopts envelope conformation. In the crystal, molecules are linked via pairs of inter molecular $C-H{\ldots}O$ hydrogen bonds to form dimmers.

Growth and Characterization of $CuInS_2$ Single Crystal Thin Film by Hot Wall Epitaxy (Hot Wall Epitaxy(HWE) 방법에 의해 성장된 $CuInS_2$)

  • 최승평;홍광준
    • Korean Journal of Crystallography
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    • v.11 no.3
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    • pp.137-146
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    • 2000
  • The stoichiometric mix of evaporating materials for he CuInS₂ single crystal thin films was prepared. To obtain the single crystal thin films, CuINS₂ mixed crystal was deposited on etched semi-insulator GaAs(100) substrate by the hot wall epitaxy(HWE) system. The source and substrate temperature were 640℃ and 430℃, respectively and the thickness of the single crystal thin films was 2 ㎛. The crystalline structure of single crystal thin films was investigated by the photoluminescence and double crystal X-ray diffraction(DCXD). The carrier density and mobility deduced from Hall data are 9.64x10/sup 22//㎥ and 2.95x10/sup -2/ ㎡/V·s, respectively at 293 K. he optical energy gap was found to be 1.53 eV at room temperature. From the photocurrent spectrum obtained by illuminating perpendicular light on the c-axis of the thin film, we have found that the values of spin orbit coupling splitting ΔSo and the crystal field splitting ΔCr were 0.0211 eV and 0.0045 eV at 10K, respectively. From PL peaks measured at 10K, were can assign the 807.7 nm (1.5350 eV) peak to E/sub x/ peak of the free exciton emission, the 810.3 nm(1.5301 eV) peak to I₂ peak of donar-bound exciton emission and the 815.6 nm(1.5201 eV) peak to I₁ peak of acceptor-bound excition emission. In addition, the peak observed at 862.0 nm(1.4383 eV) was analyzed to be PL peak due to donor-acceptor pair(DAP).

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The Crystal Structure of Licarin-B $(C_{20}H_{20}O_4)$, A Component of the Seeds of Myristica fragrans

  • Kim, Yang-Bae;Park, Il-Yeong;Shin, Kuk-Hyun
    • Archives of Pharmacal Research
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    • v.14 no.1
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    • pp.1-6
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    • 1991
  • The crystal structure of licarin-B, a component of Myristicae Semen was determined by single crystal X-ray diffraction analysis. Crystal of the compound, which was recrystallized from the mixture of hexane and ether, is monoclinic with a=12.740(1), b=7.219(1), c=9.284(1) ${\AA}$, ${\beta}=94.75(1)^{\circ}$, $D_x=1.26$, $D_m=1.27\;g/cm^3$, space group P21, and Z=2. The structure was solved by direct method and refined by least-squares procedure to the final R value of 0.040 for 1532 independent reflections ${F{\ge}3{\sigma}(F)}$. The compound is a dimeric phenylpropanoid, and belongs to the neolignan analogues. The molecules are arranged along with the screw axis. The intermolecular contacts appear to be the normal van der Waals' forces.

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Crystal Growth of $YCa_4O(BO_3)_3$ and Preparation of Device for Second Harmonic Generation ($YCa_4O(BO_3)_3$ 비선형광학 단결정 성장 및 Second Harmonic Generation 소자 제조에 관한 연구)

  • ;A.Y. Ageyev
    • Korean Journal of Crystallography
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    • v.11 no.1
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    • pp.16-21
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    • 2000
  • (Yb/sub x/Y/sub 1-x/)Ca₄O(BO₃)₃ single crystals where x=0.3,8,15,20% were grown by Czochralski Method. The crystals grown under the optimum conditions were transparent and colorless with good crystal form. Using polarizing microscope, crystal defects such as parasite crystals and bubbles were detected depending on the composition of melts and pulling rates. The optimum growth parameters for high quality of single crystals were 15∼20 rpm of rotation rate and 2mm/h of pulling rate at the flow rate of 2 l/min of Nitrogen gas. The relationship between crystal axes and optical axes was investigated by optical crystallographic method, polarization technique and single crystal X-ray method. From the spectroscopic measurements, it was confirmed that there were strong absorption bands at 900 and 976.4 nm and strong emission band at 976.4 nm in Yb/sup 3+/ ion doped YCa₄O(BO₃)₃ crystal. For the application of second harmonic generation of 1.064 ㎛ laser, non-linear optical devices with θ=32.32° and Ψ=0°, λ/10 of flatness and the size of 6x8x5.73 mm were fabricated from the grown YCa₄O(BO₃)₃ crystal.

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