• Title/Summary/Keyword: 사방정계

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Crystal Structure of Three-Dimensional Nickel(II) Tetraaza Macrocyclic Complex Linked by Hydrogen-Bonds (수소 결합에 의한 이차원의 Nickel(II) Tetraaza 거대 고리 착물 결합구조)

  • Park, Ki-Young;Choo, Geum-Hong;Suh, Il-Hwan
    • Korean Journal of Crystallography
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    • v.13 no.1
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    • pp.12-16
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    • 2002
  • The complex [Ni(L)](BDC)·4H₂O (1) (L = 3,14-dimethyl-2,6,13,17-tetraazatricyclo[16,4,O/sup 1.18/,O/sup 7.12/] docosane; BDC = 1,3-benzenedicarboxylate) has been synthesized and characterized by X-ray crystallography. Compound 1 crystallizes in the orthorhombic space group Pcnb, with a = 8.764(2) , b = 17.687(2) , c = 19.475(1) , V = 3018.7(8) ³, Z = 4, R₁, (wR₂) for 2148 observed reflections of [1>2σ(I) was 0.0822 (0.2236). Compound 1 is interconnected to give a three-dimensional network through weak hydrogen-bonding interactions.

Preparation and Structure of $Re(NC_6F_5)(PPh_3)_2Cl_3 $ ($Re(NC_6F_5)(PPh_3)_2Cl_3 $화합물의 합성 및 구조)

  • 박병규;김영웅
    • Korean Journal of Crystallography
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    • v.7 no.2
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    • pp.113-119
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    • 1996
  • Reaction of Re(O)(PPh3)2Cl3,I, with 2,3,4,5,6-pentafluoroaniline (C6F5NH2), produced Re(NC6F5)(PPh3)2Cl3, II. The product has been characterized by 1H-NMR, elemental analysis, and X-ray diffraction. II crystallizes in the orthorhombic system, space group Pna21 with cell parameters a=18.763Å, b=14.737(2)Å, c=16.707(3)Å, Z=4. Least-square refinement of the structure led to an R(wR2)factor of 0.0455(0.1148) for 3319 unique reflections of I > 2σ(I) and for 174 variables.

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Electrical Properties of YMnO3 Thin Film by Sol-gel Process (졸-겔 공정에 의한 YMnO3 박막의 전기적 특성)

  • Kim, Eung-Soo;Kim, Beng-Gu;Kim, Yoo-Taek
    • Journal of the Korean Ceramic Society
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    • v.39 no.5
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    • pp.511-516
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    • 2002
  • Hexagonal $YMnO_3$ thin films were prepared from $Y(NO_3)_3{\cdot}5H_2O$ and $Mn(CH_3CO_2)_2{\cdot}4H_2O$ as starting materials on the Si(100) substrates by the sol-gel method. The crystal structure and the electrical properties of the $YMnO_3$ thin films were investigated as a function of heat treatment temperature, the amount of water(Rw) of hydrolysis and the addition of catalysis. The crystallization of the $YMnO_3$ thin film began at 700${\circ}C$ and completed at 800${\circ}C$ for 1 h. The c-axis (0001) preferred orientation of hexagonal $YMnO_3$ was detected for the $YMnO_3$ thin films with Rw=6 and that was decreased for the $YMnO_3$ thin films with Rw=1 and Rw=12. The crystallinity and preferred orientation of the $YMnO_3$ thin films were depended on the addition of acid and/or alkali catalysis, which, in turn, the preferred orientation of c-axis was decreased and the orthorhombic phase of $YMnO_3$ was detected to the specimens with the addition of catalysis. The $YMnO_3$ thin film with Rw=6 showed good leakage current density of $1.2{\times}10-8 A/cm^2$ at the applied voltage of 0.2V and the leakage current density was not changed drastically with applied voltage.

Study of Gasless Combustion Synthesis of the Ti$Si_x$ (x = 0.6, 0.8, 1.0, 2.0) Systems (Ti$Si_x$ (x = 0.6, 0.8, 1.0, 2.0) 계의 비기체 합성법에 관한 연구)

  • Chul Hyun Yo;Sung Joo Lee;Eun Seok Lee;Pyon Mu Sil;Eung Ju Oh
    • Journal of the Korean Chemical Society
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    • v.33 no.4
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    • pp.337-342
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    • 1989
  • Gasless combustion is a vigorous exothermic reaction ignited directly in solid mixture, similar to Thermit reaction. The gasless combustion synthesis has the advantages of rapid processing, energy saving, low processing cost, and high purity of products. The Ti$Si_x$(x = 0.6, 0.8, 1.0, 2.0) systems are prepared by the gasless combustion synthesis without external sintering process. The crystallographic structures of $Ti_5Si_3$, $Ti_5Si_4$ are hexagonal and tetragonal system, respectively. Those of TiSi, $TiSi_2$ are orthorhombic systems. The results of X-ray analysis agree with the JCPDS data. The combustion modes of all combustion reactions are steady state combustions, and the propagation velocities of the combustion waves of $Ti_5Si_3$, $Ti_5Si_4$ and TiSi are greater than 0.6 cm/sec and that of $TiSi_2$ is 0.28 cm/sec.

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Study of Nonstoichiometry and Physical Properties of the Mixed Valency $Sr_xEu_{1-x}FeO_{3-y}$ ($0.00{\leq}x{\leq}$1.00) System (혼합원자가 $Sr_xEu_{1-x}FeO_{3-y}$ ($0.00{\leq}x{\leq}$1.00)계의 비화학량론과 물성 연구)

  • Ji Young Min;Kwon Sun Roh;Chul Hyun Yo
    • Journal of the Korean Chemical Society
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    • v.38 no.12
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    • pp.873-879
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    • 1994
  • A series of samples of solid solutions in the $Sr_xEu_{1-x}FeO_{3-y}(0.00{\leq}x{\leq}1.00)$ system has been prepared at $1200^{\circ}C$ under an atmospheric air pressure. The structures of solid solutions are studied by X-ray diffraction, thermal, Mohr salt, and Mossbauer spectroscopic analyses. Their physical properties are also discussed with the electrical conductivities. X-ray diffraction data for the compositions of x = 0.00, 0.25, and 1.00 are assigned to the orthorhombic and the compositions of x = 0.50 and 0.75 to the cubic systems. The lattice volume reduced to cubic cell increases with the x value. The mole ratio of $Fe^{4+}$ iometric chemical formulas of the system are formulated from the x, $\tau$, and y values. The mixed valency state of Fe ions, the oxygen coordination, and covalent bond character are discussed with the Mossbauer spectroscopic data. The activation enegy of the electrical conductivities depends on the $\tau$ value in the temperature range of -$100^{\circ}C$ to $600\circC$ under the air pressure. The Mossbauer spectrum and electrical conductivity of the solid solutions are discussed with nonstoichiometric chemical compositions.

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Synthesis and Characterization of Tetradentate N2O2 Schiff Base Ligand and its Rare Earth Metal Complexes (사배위 N2O2 Schiff 염기 리간드와 그 희토류 금속착물의 합성 및 특성)

  • Shelke, Vinod A.;Jadhav, Sarika M.;Shankarwar, Sunil G.;Munde, chut S.;Chondhekar, Trimbak K.
    • Journal of the Korean Chemical Society
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    • v.55 no.3
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    • pp.436-443
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    • 2011
  • The solid complexes of La(III), Ce(III), Pr(III), Nd(III), Sm(III) and Gd(III) with 4-hydroxy-3-(1-{2-(2,4-dihydroxy-benzylidene)-amino phenylimino}-ethyl)-6-methyl-pyran-2-one ($H_2$L) derived from o-phenylenediamine, 3-acetyl-6-methyl-(2H)pyran,2,4(3H)-dione (dehydroacetic acid or DHA) and 2, 4-dihydroxy benzaldehyde have been synthesized and characterized by elemental analysis, conductometry, magnetic susceptibility, UV-visible, FT-IR, $^1H$-NMR, X-ray diffraction, thermal analysis study, and screened for antimicrobial activity. The FT-IR spectral data suggest that the ligand behaves as a dibasic tetradentate ligand with ONNO donor atoms sequence towards central metal ion. From the microanalytical data, the stoichiometry of the complexes has been found to be 1:1 (metal: ligand). The physico-chemical data suggests distorted octahedral geometry for La(III), Ce(III), Pr(III), Nd(III), Sm(III) and Gd(III) complexes. The X-ray diffraction data suggests monoclinic crystal system for La(III) and Ce(III) and orthorombic crystal system for Pr(III) and Nd(III) complexes. Thermal behavior (TG/DTA) of the complexes was studied and kinetic parameters were determined by Horowitz-Metzger and Coats-Redfern methods. The ligand and its metal complexes were screened for antibacterial activity against Staphylococcus aureus, Escherichia coli, Bacillus Sp. and fungicidal activity against Aspergillus Niger, Trichoderma and Fusarium oxysporum.

Synthesis and Characterization of Some Transition Metal Complexes of Unsymmetrical Tetradentate Schiff Base Ligand (비대칭 Tetradentate Schiff 염기 리간드의 전이금속 착물에 대한 합성 및 특성)

  • Munde, A. S.;Jagdale, A. N.;Jadhav, S. M.;Chondhekar, T. K.
    • Journal of the Korean Chemical Society
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    • v.53 no.4
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    • pp.407-414
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    • 2009
  • The solid complexes of Cu(II), Ni(II), Co(II), Mn(II) and Fe(III) with 4-hydroxy-3-(1-{2-(2-hydroxybenzylidene)- amino phenylimino}-ethyl)-6-methy-pyran-2-one (H2L) derived from o-phenylenediamine, 3-acetyl- 6-methyl-(2H) pyran, 2,4 (3H)-dione (dehydroacetic acid or DHA) and salicylic aldehyde have been synthesized and characterized by elemental analysis, conductometry, magnetic susceptibility, UV-visible, IR, $^1H$-NMR spectra, X-ray diffraction, thermal analysis, and screened for antimicrobial activity. The IR spectral data suggest that the ligand behaves as a dibasic tetradentate ligand with ONNO donor atoms sequence towards central metal ion. From the microanalytical data, the stoichiometry of the complexes has been found to be 1:1 (metal: ligand). The physico-chemical data suggests square planar geometry for Cu(II) and Ni(II) complexes and octahedral geometry for Co(II), Mn(II) and Fe(III) complexes. The x-ray differaction data suggests orthorhombic crystal system for Cu(II) complex, monoclinic crystal system for Ni(II), Co(II) and Fe(III) and tetragonal crystal system for Mn(II) complex. Thermal behaviour (TG/DTA) of the complexes was studied and kinetic parameters were determined by Coats-Redfern method. The ligand and their metal complexes were screened for antibacterial activity against Staphylococcus aureus and Escherichia coli and fungicidal activity against Aspergillus Niger and Trichoderma.

A Study of the Nonstoichiometry and Physical Properties of the Nd1-xBaxFeO3-y System ($Nd_{1-x}Ba_xFeO_{3-y}$계의 비화학량론과 물리적 성질에 관한 연구)

  • Chang, Soon Ho;Yu, Gwang Hyeon;Kim, Seong Jin;Choe, Seung Cheol;Jang, Sun Ho
    • Journal of the Korean Chemical Society
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    • v.38 no.8
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    • pp.547-551
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    • 1994
  • A series of samples in the $Nd_{1-x}Ba_xFeO_{3-y}$ system has been prepared by heating the reactants to$1200^{\circ}C$ under an ambient atmosphere, and the solid solutions were identified by X-ray power diffraction analysis. The crystal systems of samples with x = 0.00 and 0.25 were found to be orthorhombic whose local symmetry is similiar to the distorted octahedral with orthoferrite type one, whereas those with x = 0.50 and 0.75 to be the cubic system. Since Fe ions in the solid solutions are a mixed valence state between $Fe^{3+}\;and\;Fe^{4+}$ ions, the nonstoichiometric chemical formulas could be determined from the mole ratio of $Fe^{4+}$ ion and oxygen vacacies. According to the Mossbauer spectroscopic analysis, the presence of 5-coordinated $FeO_5$ was evidenced only in the barium compounds along with $FeO_6,\;and\;FeO_4$, but not in the strontium and calcium compounds. The samples with x = 0.25 and 0.50 show a spectrum of superparamagnetism, which might be due to the formation of a domain of the ferromagnetic interaction between the $Fe^{3+}\;and\;Fe^{4+}$ ions. The electrical conductivities of all samples are within semiconducting range. Since the $Fe^{4+}$ ion acts as an electron acceptor level during the electron transfer between the Fe through intermediate $O^{2-}$ ions, the activation energy of the compounds decreases with the increment of $Fe^{4+}$ content.

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Nonstoichiometry and Magnetic Property of the $Nd_{-x}Sr_{x}CoO_{3-y}$ System ($Nd_{-x}Sr_{x}CoO_{3-y}$계의 비화학양론 및 자기적 특성)

  • Chul Hyun Yo;Kwon Sun Roh;Sung Joo Lee;Kyu Hong Kim;Eung Ju Oh
    • Journal of the Korean Chemical Society
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    • v.35 no.3
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    • pp.211-218
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    • 1991
  • A series of samples in the $Nd_{-x}Sr_{x}CoO_{3-y}$ system (x = 0.00, 0.25, 0.50, 0.75 and 1.00) have been produced by heating the reactants at 1200${\circ}$C under atmospheric pressure. The solid solutions were analysed by X-ray diffraction spectra, thermal analysis, and SEM micrographs. X-ray powder diffraction assigns the compositions of x = 0.00, 0.25, 0.50 and 0.75 to the cubic system and the composition of x = 1.00 to the orthorhombic system. The reduced lattice volume is increased with increasing x values in the system. The mole ratio of $Co^{4+}$ or ${\tau}$ values are determined by the Iodometric titration method and are maximum at the composition of x = 0.50. The magnetic measurement shows that a ferromagnetism is appeared in the compositions of x = 0.00, 0.25, 0.50 and 0.75 and then an antiferromagnetism in the composition of x = 1.00. The measurement of the electrical conductivity shows that the semiconductivity is appeared in the composition of x = 0.00, 0.25 and 1.00 and the metallic conductivity in the composition of x = 0.50 and 0.75. The magnetic and electrical properties of the samples are discussed with the nonstoichiometric chemical formulas.

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Synthesis and Structure of N-Methylphenazinium-Tetracynnopalladate(II) Hydrate (N-Methylphenazinium-Tetracyanopalladate(II) Hydrate의 합성 및 결정구조 연구)

  • NamGung, Hae;Lee, Hyun-Mi
    • Korean Journal of Crystallography
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    • v.17 no.1
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    • pp.6-9
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    • 2006
  • Crystal structure of Bis(N-Methylphenazinium)-Tetracyanopalladate(II) hydrate has been determined by X-ray crystallography. Crystal data: $(C_{13}H_{11}N_2){_2}[Pd(cn)_4]{\cdot}H_2O$, Monocline, Space group $P2_1/b$(No=14), a=9.783(4), b=10.788(4), c=13.666(4) ${\AA},\;{\beta}=104.59(5),\;Z=2,\;V=1392.9{\AA}{^3},\;Dc=1.476gcm^{-3},\;F(000)=632,\;{\mu}=7.05cm^{-1}$. 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=0.0257, Rw=0.0732, Rall=0.0283 and S=1.07 for 1930 observed reflections. Both cation and anion complexes are essentially planar and have dihedral angles of $10.16(4)^{\circ}$. The planar complex anions are sandwiched between slightly bent cations. The interplanar separations in one triad and between two triads are 3.419(3) and $3.402(4){\AA}$, respectively. The triads are stacked along b-axis.