• Title/Summary/Keyword: $^{13}$C$_{CH4}$

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Synthesis and Characterization of Tetranuclear Molybdenum(Ⅵ) Complexes with Butylamidoxime Derivatives (부틸아미드옥심 유도체의 몰리브덴(Ⅵ) 사핵 착물의 합성과 성질)

  • Roh, Soo-Gyun;Oh, Sang Oh
    • Journal of the Korean Chemical Society
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    • v.39 no.7
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    • pp.552-558
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    • 1995
  • The tetranuclear complexes, $X_2[M_{O4}O_12{R'C(NH_2)NO}_2](X= n-Bu_4N^+$, $R'=(CH_3)_2CH$, $CH_3CH_2CH_2$, $CH_3SCH_2$; $X=(CH_3)_2CHC(=NH_2)NH_2^+$, $R'=(CH_3)_2CH$; $X = CH_3CH_2CH_2C(=NH_2)NH_2^+$, $R'=CH_3_CH_2CH_2$; $X=CH_3SCH_2C(=NH_2)NH_2^+$, $R'=CH_3SCH_2)$ have been synthesized by the reactions of monomeric and polynuclear complexes with isobutyl-, butyl- and thiomethylacetamidoxime. The prepared complexes were identified by elemental analysis, infrared, $^1H$ NMR and $^{13}C$ NMR spectroscopy. The structure of complex ${(CH_3)_2CHC(NH_2)_2}_2[M_{O4}O_{12}{(CH_3)_2CHC(NH_2)NO}_2]$ was determined by X-ray single crystal diffraction. Crystal data are follows: Monoclinic, $P2_{1/c}$, $a=10.168(3){\AA}$, $b=11.768(1){\AA}$, $c=13.557(1){\AA}$, ${\beta}=102.08(1)^{\circ}$, $V=1586.2(5){\AA}^3$, Z=2, final R=0.026 for 2951($F_0>3s(F_0)$). This complex is composed of a planar cyclic $[Mo_4({\mu}-O)_4]$ and two ${\mu}_4$-amidoximate.

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Synthesis and Characterization of Group 13 Compounds of 2-Acetylpyridine Thiosemicarbazone. Single-Crystal Structure of $(iC_4H_9)-2Al(NC_5H_4C(CH_3)$NNC(S)NHPh)

  • 강영진;강상옥;고재정;손정인
    • Bulletin of the Korean Chemical Society
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    • v.20 no.1
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    • pp.65-68
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    • 1999
  • Novel mononuclear group 13 metal complexes with the formula (R2M){NC5H4C(CH3)NNC(S)NH(C6H5)} (M=Al, R=iC4H9 (1); M=Ga, R=iC4H9 (2); M=Al, R=CH2SiMe3 (3); M=Ga, R=CH2SiMe3 (4)) result when 2-acetyl pyridine 4-phenyl-thiosemicarbazone ligand is mixed with trialkyl aluminum or trialkylgallium. These compounds 1-4 are characterized by microanalysis, NMR (1H, 13C) spectroscopy, mass spectra, and singlecrystal X-ray diffraction. X-ray single-crystal diffraction analysis reveals that 1 is mononuclear metal compound with coordination number of 5 and N, N, S-coordination mode.

Microbial Production of N-Acetylglucosamine by Arthrobacter nicotianae (Arthrobacter nicotianae에 의한 N-acetylglucosamine의 생산)

  • Chang, Ji-Yoon;Kim, In-Cheol;Chang, Hae-Choon
    • Korean Journal of Food Science and Technology
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    • v.35 no.6
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    • pp.1188-1192
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    • 2003
  • Chitinase producing bacteria, Arthrobacter nicotianae CH4 and A. nicotianae CH13, were isolated from small crabs by an enrichment culture using chitin as the sole carbon source. Crude chitinases from the two isolated strains, A. nicotianae CH4 and A. nicotianae CH13, were stable in the pH range of $3.0{\sim}9.0$ and in the temperature range of $20{\sim}60^{\circ}C$. The reducing sugar $(GlcNAc)_1$, or $(GlcNAc)_4$, corresponding to over 98% of the enzyme reaction products, was obtained. The production of functional $(GlcNAc)_1$ and $(GlcNAc)_4$ from A. nicotianae CH13 and A. nicotianae CH4, respectively, from the chitinases was useful. The chitinase system of A. nicotianae CH13 was supposed to be endo- and exo-chitinase, and N-acetylglucosaminidase.

Synthesis and Characterization of New Group 13 Complexes of 2-Acetylpyridine-S-methyldithiocarbazate. Single-Crystal Structure of Me₂Ga[$NC_5H_4C$(CH₃)NNC(S)SMe] and Me₂In[$NC_5H_5C$(CH₃)NNC(S)SMe]

  • 백철기;강상욱;이채호;이영행;고재정
    • Bulletin of the Korean Chemical Society
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    • v.18 no.3
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    • pp.311-316
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    • 1997
  • The synthesis and characterization of the mononuclear group 13 heterocyclic carboxaldehyde methyldithiocarbazate complexes Me2M[NC5H4CRNNC(S)SCH3] (M=Al, R=H(1); M=Ga, R=H(2); M=Al, R=CH3(3); M-Ga, R=CH3(4); M=In, R=CH3(5)) are described. Compounds 1-5 were prepared by the reaction of MMe3 (M=Al, Ga, In) with 2-formy or 2-acetylpyridine-S-methyldithiocarbazate in toluene. These compounds 1-5 have been characterized by microanalysis, NMR (1H, 13C) spectroscopy, mass spectra, and single-crystal X-ray diffraction. X-ray single-crystal diffraction analyses reveal that 4-5 are mononuclear metal compounds with coordination number of 5 and N,N,S coordination mode.

Structural characteristics of [N(CH3)4]2CdCl4 determined by 1H MAS NMR, 13C CP/ MAS NMR, and 14N NMR

  • Lee, Seung Jin;Lim, Ae Ran
    • Journal of the Korean Magnetic Resonance Society
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    • v.19 no.1
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    • pp.18-22
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    • 2015
  • The structural geometry of $[N(CH_3)_4]_2CdCl_4$ in a hexagonal phase is studied by $^1H$ MAS NMR, $^{13}C$ CP/MAS NMR, and $^{14}N$ NMR. The changes in the chemical shifts for $^{13}C$ and $^{14}N$ in the hexagonal phase are explained by the structural geometry. In addition, the temperature dependencies of the spin-lattice relaxation time in the rotating frame $T_{1{\rho}}$ for $^1H$ MAS NMR and $^{13}C$ CP/MAS NMR are measured.

Studies of Oxo-Nitrosyl Complexes(Ⅱ) Synthesis and Properties of Tungsten Oxo-Nitrosyl Complexes with Butylamidoxime Derivatives (산소-니트로실 착물의 연구 (제2보) 부틸아미드옥심 유도체의 텅스텐 산소-니트로실 착물의 합성과 특성)

  • Roh, Soo Gyun;Oh, Sang Oh
    • Journal of the Korean Chemical Society
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    • v.39 no.11
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    • pp.856-862
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    • 1995
  • The tungsten oxo-nitrosyl complexes (n-Bu4N)2[W5O12(NO)2{RC(NH2)NHO}2{RC(NH)NO}2] (R=(CH3)2CH, CH3CH2CH2, CH3SCH2) have been synthesized by the reactions of polyoxotungsten complex (n-Bu4N)2[W6O19] and tungsten dinitrosyl monomeric complex [W(NO)2(acac)(CH3CN)2](BF4) with butylamidoxime derivatives. The prepared complexes have been characterized by elemental analysis, infrared, UV-visible, 1H NMR and 13C NMR spectroscopy. The pentanuclear species was formed by the interaction of the electron-withdrawing {W(NO)2}2+ unit between the two dinuclear tungsten {W2O5}2+ cores. We can estimate to exist large proton interactions viewed from the four doublet in 1H NMR spectrum of (n-Bu4N)2[W5O12(NO)2{(CH3)2CHC(NH2)NHO}2{(CH3)2CHC(NH)NO}2]. We also drew informations of the two different coordination mode and symmetry of the complexes because two ligands appear in 13C NMR spectra instead of four. The {W(NO)2}2+ unit has been cis-form and C2v symmetry in geometric structure.

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Synthesis, Structural Characterization and Thermal Behaviour of Block Copolymers of Aminopropyl-Terminated Polydimethylsiloxane and Polyamide Having Trichlorogermyl Pendant Group (Aminopropyl-Terminated Polydimethylsiloxane과 Trichlorogermyl 곁가지 그룹을 갖는 Polyamide 블록공중합체의 합성, 구조분석 및 열적거동)

  • Gill, Rohama;Mazhar, M.;Mahboob, Sumera;Siddiq, Muhammad
    • Polymer(Korea)
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    • v.32 no.3
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    • pp.239-245
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    • 2008
  • Block copolymers of the general formula $[(-CO-R'-CO-HN-Ar-NH-CO-R'-CO)_xNH(CH_2)_3-(Me_2SiO)_y(CH_2)_3NH_2]_n$, [n=18.00 to 1175.0] where $R'=CH_2CH(CH_2GeCl_3)$;$CH_2CHGeCl_3CH_2$; and $Ar=-C_6H_4$;$-(o.CH_3C_6H_4)_2$;$-o.CH_3OC_6H_4)_2$;$-(o.CH_3C_6H_4)$ were prepared by a polycondensation reaction of polyamide containing a pendant trichlorogermyl group and terminal acid chloride $Cl(-CO-R'-CO-NH-Ar-NH-CO-R'-CO-)_xCl$ with aminopropyl-terminated polydimethylsiloxane $H_2N(CH_2)_3(Me_2SiO)_y-(CH_2)_3NH_2]$, (PDMS). These polymers were characterized by elemental analysis, $T_g$, FT-IR, $^1H$-NMR, solid state $^{13}C$-NMR, and molecular weight determination. The thermal stability of these copolymers was examined using thermal analysis techniques, such as TGA and DSC. Their molecular weights as determined by laser light scattering technique ranged $5.13{\times}10^5$ to $331{\times}10^5\;g/mol$. These polymers display their $T_g$ in the range of 337 to $393^{\circ}C$ with an average decomposition temperature at $582^{\circ}C$.

Complex Formation of Substituted Benzo-1,4,7,10,13-pentaoxacyclopentadecane (B15C5) with Nd(Ⅲ) (Nd(Ⅲ)과 치환된 Benzo-1,4,7,10,13-pentaoxacyclopentadecane (B15C5)와의 착물 형성에 관한 연구)

  • Kim, Hae-Joong;Kim, Jeong;Kim, Si-Joong
    • Journal of the Korean Chemical Society
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    • v.39 no.6
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    • pp.440-445
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    • 1995
  • The chemical compositions and stability constants, thermodynamic parameters for the neodymium(Ⅲ) complexes of substituted benzo-1,4,7,10,13-pentaoxacyclopentadecane(B15C5) have been determined by spectrophotometry and conductometry in methanol solution at various temperatures. As substituents, CH3, Br, CHO, NO2, and 3,4-(NO2)2 were used. In methanol solution the ratios of neodymium(Ⅲ) to the ligands in the complexes are 1 : 1. The stability constants were increased in order of B15C5-3,4-(NO2)2 < B15C5-NO2 < B15C5-CHO < B15C5-Br < B15C5 < B15C5-CH3. This observation can be explained in terms of the substituent effect. The order of stability constants was dimethylsulfoxide < acetone < acetonitrile in solution and the magnitudes were found to be inversely proportional to the solvents donicities. These results could be understood in terms of solvent basicity, ligand basicity, solvation of the cation, and entropy changes of complex formation.

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Interpretation of Origin and Methanogenic Pathways of Coalbed Gases from the Asem-Asem Basin, Southeast Kalimantan, Indonesia (인도네시아 칼리만탄 남동측에 위치하는 아셈-아셈분지 석탄층 가스의 기원과 메탄생성경로 해석)

  • Chun, Jong-Hwa;Hwang, In Gul;Lee, Wonsuk;Lee, Taehun;Kim, Yuri
    • Economic and Environmental Geology
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    • v.55 no.3
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    • pp.261-271
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    • 2022
  • Six gas samples were collected from coal and coaly shale from core AA-1, which was acquired from the Asem-Asem Basin, southeast Kalimantan, Indonesia. These coalbed gas samples were analyzed for the molecular composition, carbon isotope (δ13CCH4, δ13CC2, and δ13CCO2), hydrogen isotope (δDCH4), hydrocarbon index (CHC), and carbon dioxide-methane index (CDMI) to document their origin and methanogenic pathways. Core AA-1 successively consists of lower clastic sedimentary rocks (Sedimentary Unit-1, SU-1) containing coal and coaly shale, and upper limestone (Sedimentary Unit-2, SU-2), unconformably underlain by serpentinized basement interpreted as part of the Cretaceous Meratus subduction complex (MSC). The coal and coaly shale (SU-1) were deposited in a marshes nearby a small-scale river. Compositions of coalbed gases show that methane ranges from 87.35 to 95.29% and ethane ranges from 3.65 to 9.97%. Carbon isotope of coalbed methane (δ13CCH4) ranges from -60.3 to -58.8‰, while hydrogen isotope (δDCH4) ranges from -252.9 to -252.1‰. Carbon isotope of coalbed ethane (δ13CC2) ranges from -32.8 to -31.2‰, carbon isotope of coalbed carbon dioxide (δ13CCO2) ranges from -8.6 to -6.2‰. The coalbed CO2 is interpreted to be an abiogenic origin based on a combination of δ13CCO2 and CDMI and could have been transported from underlying CO2 bearing MSC through faults. The methanogenic pathways of coalbed gases are interpreted to have originated from primary methyl-type fermentation and mixed with CO2 reduction, affecting thermogenic non-marine coal-type gases based on analyses of isotopic ratios and various indexes.

Phase Equilibria and $^{13}C$ NMR Analysis of the Double Semi-Clathrates Containing TBAB (TBAB를 포함하는 혼합 하이드레이트의 상평형 및 $^{13}C$ NMR 분석)

  • Lee, Seung-Min;Park, Sung-Min;Lee, Young-Jun;Lee, Sung-Won;Seo, Yong-Won
    • Korean Chemical Engineering Research
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    • v.49 no.3
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    • pp.367-371
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    • 2011
  • TBAB (tetra-n-butyl ammonium bromide) forms a semi-clathrate with water under atmospheric pressure conditions and recently has attracted great attention due to its usage as a thermodynamic promoter in gas storage and separation process using gas hydrate formation. In this study, we measured the three-phase (hydrate (H) - liquid water ($L_{w}$)-vapor (V)) equilibria of the ternary $CH_{4}$+TBAB+water and $CO_{2}$+TBAB+water mixtures at the TBAB concentrations of 5 and 32 wt% to investigate promoting characteristics of TBAB. The greater promotion effect of TBAB was observed at 32 wt% than at 5 wt%. This result was in good agreement with that from pure TBAB semi-clathrate phase diagram under atmospheric pressure conditions. Through $^{13}C$ NMR analysis of the $CH_{4}$+TBAB semi-clathrate, it was found that $CH_{4}$ molecules are enclathrated in the cages of the double semi-clathrate and the position of resonance peak from encaged $CH_{4}$ molocules in the double semi-clathrate is the same as that from encaged $CH_{4}$ molocules in the pure $CH_{4}$ hydrate of structure I.