• Title/Summary/Keyword: Coordination compound

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Synthesis, Structure, and Magnetic Properties of 1D Nickel Coordination Polymer Ni(en)(ox)·2H2O (en = ethylenediamine; ox = oxalate)

  • Chun, Ji-Eun;Lee, Yu-Mi;Pyo, Seung-Moon;Im, Chan;Kim, Seung-Joo;Yun, Ho-Seop;Do, Jung-Hwan
    • Bulletin of the Korean Chemical Society
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    • v.30 no.7
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    • pp.1603-1606
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    • 2009
  • A new 1D oxalato bridged compound Ni(en)(ox)-2$H_2$O, (ox = oxalate; en = ethylenediamine) has been hydrothermally synthesized and characterized by single crystal X-ray diffraction, IR spectrum, TG analysis, and magnetic measurements. In the structure the Ni atoms are coordinated with four oxygen atoms in two oxalate ions and two nitrogen atoms in one ethylenediamine molecule. The oxalate anion acts as a bis-bidentate ligand bridging Ni atoms in cis-configuration. This completes the infinite zigzag neutral chain, [Ni(en)(ox)]. The interchain space is filled by water molecules that link the chains through a network of hydrogen bonds. Thermal variance of the magnetic susceptibility shows a broad maximum around 50 K characteristic of one-dimensional antiferromagnetic coupling. The theoretical fit of the data for T > 20 K led to the nearest neighbor spin interaction J = -43 K and g = 2.25. The rapid decrease in susceptibility below 20 K indicate this compound to be a likely Haldane gap candidate material with S = 1.

Synthesis, Characterization and Property Studies on a Dinuclear Copper(II) Complex with Dipyridine Derivate and Acetylacetone

  • Zhao, Pu Su;Guo, Zhi Yan;Sui, Jing;Wang, Jing;Jian, Fang Fang
    • Bulletin of the Korean Chemical Society
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    • v.32 no.1
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    • pp.49-52
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    • 2011
  • A dinuclear copper(II) complex of [$Cu_2(aceace)_4$(dipyph)] [aceace = acetylacetone, dipyph = 1,4-di(4-pyridylethene-2-yl-)benzene] has been synthesized and characterized by elemental analysis, IR and X-ray single crystal diffraction. It crystallizes in the monoclinic system, space group P21/c, with lattice parameters a = 7.9584(16) $\AA$, b = 18.594(4) $\AA$, c = 15.063(4) $\AA$ $\beta=120.97(2)^o$ and $M_r$ = 807.85 ($C_{40}H_{44}Cu_2N_2O_8$), Z = 2. Each of the $Cu^{2+}$ ion adopts a square pyramid geometry and coordinates with four oxygen atoms from two aceace ligands and one nitrogen atom from dipyph bidentate ligand. Magnetic measurement shows that the Weiss constant and Curie constant for the title compound are -0.22 K and 0.1154 emu K/mol, respectively. Thermal stability data indicate that the title complex undergoes two steps decomposition and the residue is $Cu_2O_4$. In the potential range of -1.5 ~ 0.8 V, the title complex represents an irreversible electrochemical process.

Hydrothermal Synthesis, Crystal Structure and EPR Property of Tetranuclear Copper(II) Cluster [Cu4OCl6(C14H12N2)4]

  • Jian, Fang-Fang;Zhao, Pu-Su;Wang, Huan-Xiang;Lu, Lu-De
    • Bulletin of the Korean Chemical Society
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    • v.25 no.5
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    • pp.673-675
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    • 2004
  • The tetranuclear copper(II) cluster compound $[Cu_4OCl_6(C_{14}H_{12}N_2)_4]$ has been synthesized by hydrothermal reaction and studied by X-ray diffraction. The four copper(II) atoms locate four capsheaves of a tetrahedral skeletal structure and a oxygen atom as interstitial atom occupies the center position of the same tetrahedron, and each edge of the Cu-Cu tetrahedron is bridged by one ${\mu}_2$-Cl anion. The copper atom possesses slightly distorted trigonal bipyramidal geometry with three ${\mu}_2$-Cl atoms in equatorial position and the interstitial O atom and one N atom from 3-benzyl-benzimidazole ligand occupying axial position. The Cu-Cu distances are in the range of 3.0986-3.1162 ${\AA}$. The EPR spectrum suggested that the copper(II) ground state $d_{x2-y2}$ and the coordination geometry was trigonal bipyramidal.

Infinite 1-D and 3-D Nets with Two Different Zinc and Terbium Coordination Polymers.

  • 민동원;이연경;이순원
    • Proceedings of the Korea Crystallographic Association Conference
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    • 2002.11a
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    • pp.31-31
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    • 2002
  • The hydrothermal reaction of Zn(NO₃)₂6H₂O with benzene-1,3-dicarboxylic acid (or isophthalic acid, 1,3-BDCH₂) and pyridine led to the formation of a 1-dimensional coordination polymer with the empirical formula of [Zn₄(1,3-BDC)₃(Py)₂(O/sup 2-/)] (1). On the other hand, the hydrothermal reaction of Tb(NO₃)₃5H₂O with benzene-1,3-dicarboxylic acid (or isophthalic acid, 1,3-BDCH₂) and pyridine gave a 3-D compound [Tb₃(1,3-BDC)₂(H₂O₃] (2). The structures of both compounds have been determined by X-ray diffraction. 1 crystallizes in the monoclinlc space group P2₁/n, a = 10.344(3) Å, b = 18.030(3) Å, c = 18.033(3) Å, = 90.46(2)°, V = 3363.1(13) ,ų, Z = 4. 2 crystallizes in the monoclinic space group C2/n, a = 22.253(5) Å, b = 18.672(4) Å, c = 11.5812 Å, = 101.40(2)°, V = 4717.3(21) ų, Z = 8.

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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.

Effect of Metal Complexes as a Catalyst on Curing Behavior and Mechanical Properties of Silica Filled Epoxy-Anhydride Compounds (촉매로서 금속 착화합물이 실리카가 충전된 에폭시-산무수물 복합체의 경화 거동 및 물성에 미치는 영향)

  • Seo, Byeongho;Lee, Dong-Hoon;Lee, Noori;Do, Kiwon;Ma, Kyungnam;Kim, Wonho
    • Elastomers and Composites
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    • v.49 no.1
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    • pp.59-65
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    • 2014
  • In this study, in order to complete curing reaction of the molding compound comprising an epoxy/anhydride at $71^{\circ}C$ for 40 hours, metal coordination complexes such as cobalt (II) acetylacetonate, potassium acetylacetonate, iron (III) acetylacetonate and chromium (III) octoate as a catalyst were applied to the epoxy/anhydride compounds respectively. The weight ratio of an epoxy part/an anhydride part was adjusted to improve the mechanical properties of the molding compound. According to the experimental results, an epoxy/anhydride compound containing chromium (III) octoate showed a high conversion at $71^{\circ}C$ for 40 hours as well as a proper processability at room temperature among the several metal coordination complexes. For the mechanical properties of the cured epoxy/anhydride compound, the compounds containing weight ratio from 0.9/1 to 0.5/1 of the epoxy part/anhydride part with chromium (III) octoate showed the high flexural strength, and higher compressive strength was shown with increasing of the hardener part.

Synthesis and Structural Analysis of the Diaquabis(ethylenediamine)nickel(II) Bis(p-toluenesulfonate) Monohydrate (Diaquabis(ethylenediamine)nickel(II) Bis(p-toluenesulfonate) Monohydrate 층상 화합물의 합성과 구조 분석)

  • Kim, Chong-Hyeak;Lee, Sueg-Geun
    • Analytical Science and Technology
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    • v.15 no.3
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    • pp.317-320
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    • 2002
  • The layer structure of the title compound, $[Ni(en)_2(H_2O)_2](CH_3C_6H_4SO_3)_2(H_2O)$ (en = ethylenediamine), consists of discrete cations, anions, and solvate water molecules linked by a hydrogen bonding network. The central Ni atom of the cation layer has a slightly distorted octahedral coordination geometry with the ethylenediamine ligands functioning as a N,N'-bidentate and the water ligands bonding through oxygen in a trans arrangement. The p-toluenesulfonate of the anion layer has an alternate sulfonate group directed toward opposite side of the cation layer. This layer structure is stabilized by a hydrogen bond involving the O atoms of the sulfonate, the water ligand, solvate water molecule, and the N atoms of the ethylenediamine.

Cycloplatinated Complexes of Thiosemicarbazones. Synthesis and Crystal Structure of [$Ph_2PC_6H_4CHNNC(S)NHCH_3PtCl$]

  • 유동원;강상욱;고재정;최문근
    • Bulletin of the Korean Chemical Society
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    • v.18 no.3
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    • pp.305-310
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    • 1997
  • The synthesis and characterization of the platinum heterocyclic carboxaldehyde thiosemicarbazone complexes [NC5H4CRNNC(S)NHR'PtCl] (R=H, R'=CH3(1); R=CH3, R'=CH3(2); R=CH3, R=H(3)) and diphenylphosphinophenyl carboxaldehyde thiosemicarbazone complexes [Ph2PC6H4CHNNC(S)NHRPtCl] (R=CH3(5); R=iC3H7(6); R=Ph(7)) are described. Compounds 1-3 were prepared by reaction of Pt(SEt2)2Cl2 with 2-acetylpyridine-4-alkylthiosemicarbazone in the presence of NEt3. Compounds 5-7 were prepared using Pt(SEt2)2Cl2 in toluene with diphenylphosphinophenyl carboxaldehyde alkylthiosemicarbazone. The compounds have been characterized by microanalysis, NMR (1H, 13C, 31P) spectroscopy, and single-crystal X-ray diffraction. X-ray single crystal diffraction analysis reveals that compound 5 is a mononuclear platinum compound with P,N,S-coordination mode.

Self-assembly Coordination Compounds of Cu(II), Zn(II) and Ag(I) with btp Ligands (btp = 2,6-bis(N'-1,2,4-triazolyl)pyridine):Counteranion Effects

  • Kim, Cheal;Kim, Sung-Jin;Kim, Young-Mee
    • Korean Journal of Crystallography
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    • v.16 no.2
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    • pp.107-127
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    • 2005
  • Five Cu(II) compounds were obtained from different copper salts with btp ligands, and their structures were determined by X-ray crystallography. The structure of coordination polymer 2 contains btp-bridged tetranuclear Cu(II) units weakly connected by nitrate ions, and the structure of a discrete Cu(II) molecule 1 contains acetates and btp ligands. With perchlorate anions, two btp ligands bridge Cu(II) ions to form a double zigzag chain 3, while a single zigzag chain 4 is created with sulfate anions. The reaction of $Cu(NO_{3})_{2}$ containing $NH_{4}PF_{6}$ with btp ligands also produced a polymeric compound 5 containing $Cu(H_{2}O)_{2}^{2+}$ and $Cu(NO_{3})_{2}$ units alternatively bridged by btp ligands with H-bonds between copper bonded water and nitrate oxygen atoms. Five Zn(II) compounds were obtained from different zinc salts with btp ligands, and the structures of polymeric compounds (6, 7 and 8) and monomeric compounds (9 and 10) were determined by X-ray crystallography. With nitrate, chloride and bromide anions, btp ligands bridge Zn(II) ions to form polymeric compounds (6, 7 and 8), but btp ligands coordinate to a Zn(II) ion to form monomeric complexes (9 and 10) with $PF_{6}^{-}$ and perchlorate anions. Four silver salts and btp ligands produced two kinds of structures, dinuclear 20-membered rings and one-dimensional zigzag chain depending on different anions. For $ClO_{4}^{-}$ and OTf anions, weak interactions between Ag(I) and anions make dinuclear 20-membered rings construct polymeric compounds (11 and 13). For $PF_{6}^{-}$ anion, there are also weak interactions between Ag(I) and $F(PF_{6}^{-})(12)$, but they do not construct a polymeric compound. For $O_{2}CCF_{3}^{-}$ anion, btp ligands bridge Ag(I) atoms to make one-dimensional zigzag chain (14), and there are also interactions between Ag(I) and anions.