• 제목/요약/키워드: X-ray Crystallography

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Synthesis, X-Ray Crystal Structure and Coupling Reactions of 4,5-($1^{\prime},2^{\prime}$-diphenylethylenedithio)-1,3-dithiole-2-thione (dPhEDT-DTT)

  • 이하진;노동윤
    • Bulletin of the Korean Chemical Society
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    • 제19권3호
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    • pp.340-344
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    • 1998
  • A facile synthesis of 4,5-(1',2'-diphenylethylenedithio)-1,3-dithiole-2-thione (dPhEDT-DTT) is carried out via a Diels-Alder type [2+4] cycloaddition reaction of 1,3-dithiol-2,4,5-trithione oligomer and t-stilbene. Molecular structure of dPhEDT-DTT is determined by x-ray crystallography: space group P1, a=11.694(3) Å, b=12.117(3) Å, c=14.688(3) Å, α=113.12(2)°, β=102.23(2)°, γ=107.02(2)°, V= 1699.1(7) Å3, Z=2. It turns out that dPhEDT-DTT crystallizes as a racemic compound consisting of (R,R) and (S,S) enantiomers. Coupling reaction of dPhEDT-DTO undergone in neat P(OEt)3 yields TTF(SEt)4 instead of ET derivative. When PR3 (R=OEt, OPh, Ph) is used in benzene, toluene or xylene, however, dPhEDT-DTO is decomposed.

Nickel(II) trans-1,2-Diaminocyclohexane 착물의 합성 및 결정 구조 (Synthesis and Crystal Structure of Nickel(II) Complex of trans-1,2-Diaminocyclohexane)

  • 최기영;김용선;서일환;서만철
    • 한국결정학회지
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    • 제12권2호
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    • pp.88-91
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    • 2001
  • [NiL₃]Cl₂·3H₂O (1) (L=trans-1,2-diaminocyclohexane) 착물을 합성하고 구조를 규명하였다. 이 착물은 입방결정계, 공간군 P2₁3, a=13.830(1) Å, V=2645.9(2) ų, Z=4로 결정화 되었다. 이 착물의 구조는 최소자승법으로 정밀화하였으며, 최종 신뢰도 R₁(wR₂) 값은 1500회의 회절반점에 대하여 0.0766(0.2068)이었다.

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거대고리 Chlorotetraamine Zinc(II) 착물의 결정구조 (Crystal Structure of Macrocyclic Chlorotetraamine Zinc(II) Complex)

  • 최기영;박병빈;서일환;김진규;박영수
    • 한국결정학회지
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    • 제11권1호
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    • pp.42-45
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    • 2000
  • The complex [Zn(L)Cl](H₂O)(ClO₄) (1) (L=3,14-dimethyl-2,6,13,17-tetraazatricyclo[14,4,O/sup 1.18/,O/sup 7.12/]docosane) has been prepared and characterized by X-ray crystallography. 1 crystallizes in the monoclinic space group P2₁/c, with a=8.883(1), b=19.319(9), c=15.124(2)Å, β=101.65(1)°, V=2542.0(13) ų, Z=4, R₁(wR₂) for 4457 observed reflections of [I>2σ(I)] was 0.0640(0.1557). The coordination geometry around the zinc is a distorted square-pyramid with four nitrogen atoms of the macrocycle occupying the basal sites(Zn-N/sub av/=2.131(2)Å) and a chloride atom at the axial position with the Zn-Cl distance of 2.315(2)Å.

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Di-N-hydroxyethylated Tetraaza 거대고리 Copper(II) 착물 (Copper(II) Complex of a Di-N-hydroxyethylated Tetraaza Macrocycle)

  • 최기영;김용선;류해일;서일환;추금홍
    • 한국결정학회지
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    • 제11권3호
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    • pp.147-150
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    • 2000
  • The complex [CuL}Cl₂·3H₂O(1)(L=2,13-bis(2-hydroxyethyl)-5,16-dimethyl-2,6,13,17-tetraazatricyclo[14,4,0/sup 1.18/,0/sup 7.12/] docosane) has been synthesized and characterized by X-ray crystallography. 1. crystallized in the monoclinic, space group C2/c, with a=21.647(6)Å, b=8.549(1)Å, c=18.132(5)Å, β=118.58(2)°, V=2946.8(12)ų, Z=4, R₁(wR₂) for 2374observed reflections of [I>2σ(I)] was 0.052(0.187). The centrosymmetric complex 1 has an axially elongated octahedral geometry with four secondary and tertially amines of the macrocycle and tow oxygen atoms of the pendant hydroxyethyl groups.

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Synthesis and Structure of $[Ni(dppe)_2] (dppe=Ph_2PCH_2CH_2PPh_2)$ ($[Ni(dppe)_2]$의 합성 및 구조)

  • Kim, Wan -Sung;Lee, Ji-Hwa;Lee, Soon W.
    • 한국결정학회지
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    • 제11권2호
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    • pp.80-83
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    • 2000
  • Compound [Ni(P(OEt)3)4] (1) reacted with bis(diphenylphosphino)ethane (Ph2PCH2CH2Ph2, dppe) to give bis(bis(diphenylphosphine)ethane)nickel(0), [Ni(dppe)2] (2). Compound 2 was characterized by spectroscopy (1H-and 31P{1H}-NMR) and X-ray crystallography. Crystallographic data for 2: monoclinic space group P21/n, a=9.826(1)Å, b=21.167(2)Å, c=21.425(2)Å, β=91.957(9)°, Z=4, R(wR2)=0.0377(0.0882).

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$[Ni(C_2N_2H_8)_3]\cdotCrO_4$의 결정구조 (The Crystal Structure of Tris(ethylenediamine)nickel(II)Chromate, $[Ni(C_2N_2H_8)_3]\cdotCrO_4$)

  • 김세환;김승빈;남궁해
    • 한국결정학회지
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    • 제6권2호
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    • pp.75-79
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    • 1995
  • The crystal structure of Tris(ethylenediamine)nickel(II)Chromate has been determined by X-ray crystallography. Crystal data : a=9.027(2)Å, c=9.751(5)Å이며, Z=2, V=687.9(2)Å3, Dc=1.714gcm-3, μ=21.635-1. The intensity were collected with Mo-Kα radiation (λ=0.7107Å) on an automatic four-circle diffractometer with a graphite monochromator. The structure was solved by Patterson method and refined by full matrix least-square methods using unit weights. The final R and S values were R=0.029, Rw=032, Rall=0.049 andS=0.018 for 342 observed reflections. The chromate ions are located at position of point of point symmetry 32 and their oxygens are sixfold disodered in an unusual way. Extensive strong hydrogen bonds between complex cations and chromatic anions are found in axial and equatorial directions.

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기판온도에 따른 ZnO박막의 결정구조 및 전기적 특성 (The effect of substrate temperature on crystallography and electrical properties of ZnO thin films)

  • 금민종;성하윤;손인환;장경욱;김경환
    • 한국전기전자재료학회:학술대회논문집
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    • 한국전기전자재료학회 1999년도 추계학술대회 논문집
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    • pp.415-418
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    • 1999
  • In this paper we studied that the effect of substrate temperature on crystallography and electrical properties of ZnO thin films. Facing Targets Sputtering system can deposit thin films in plasma-free situation and change the deposition condition in wide range. And prepared thin film\`s c-axis orientation and grain size were analyzed by XRD(x-ray diffractometer). In the results, we suggest that FTS system is very suitable to preparing high quality ZnO thin film with good c-axis orientation.

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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.
    • 통합자연과학논문집
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    • 제9권2호
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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.
    • 통합자연과학논문집
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    • 제9권2호
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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.

Synthesis and Structural Analysis of 2-Amino-4-(4-hydroxy-3-methoxyphenyl)-7,9-dimethyl-5-oxo-4, 5, 6, 7-tetrahydropyrano [2, 3-d] pyrazolo [3, 4-b] pyridine-3-carbonitrile through X-ray Crystallography

  • Ganapathy, Jagadeesan;Jayarajan, R.;Vasuki, G.;Sanmargam, Aravindhan
    • 통합자연과학논문집
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    • 제8권1호
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    • pp.30-39
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    • 2015
  • The crystal structure of the potential active 2-amino-4-(4-hydroxy-3-methoxyphenyl)-7, 9-dimethyl-5-oxo-4, 5, 6, 7-tetrahydropyrano [2, 3-d] pyrazolo [3, 4-b] pyridine-3-carbonitrile ($C_{21}H_{22}N_5O_6S$) has been determined from single crystal X-ray diffraction data. In the title compound crystallizes in the monoclinic space group P-1 with unit cell dimension a=8.1201(9)${\AA}$, b=12.2684(4)${\AA}$ and c=12.387(2)${\AA}$ [${\alpha}=69.573^{\circ}$, ${\beta}=12.168^{\circ}$ and ${\gamma}=76.060^{\circ}$]. In the structure the pyrazole, pyridine and pyran are almost coplanar each other. The crystal packing is stabilized by intermolecular C-H...O and N-H... O hydrogen bond interaction.