• 제목/요약/키워드: Crystal structure, Nickel(II) complex

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

  • Park, Ki-Young;Choo, Geum-Hong;Suh, Il-Hwan
    • 한국결정학회지
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    • 제13권1호
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    • pp.12-16
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    • 2002
  • [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) 착물을 합성하고 구조를 규명하였다. 이 착물은 사방정계, 공간군 Pcnb, a = 8.764(2) , b = 17.687(2) , c = 19.475(1) , V = 3018.7(8) ³, Z = 4로 결정화 되었다. 이 착물의 구조는 최소자승법으로 정밀화하였으며, 최종 신뢰도 R₁(wR₂)값은 2148개의 회절반점에 대하여 0.0822 및 0.2236이었다. 화합물 1은 수소결합들로 연결된 삼차원의 그물 구조를 갖는다.

Synthesis and Characterization of C-meso and C-racemic Isomers of a Reinforced Tetraaza Macrocycle and Their Copper(II) Complexes

  • Jeong, Gyeong Rok;Kim, Juyoung;Kang, Shin-Geol;Jeong, Jong Hwa
    • Bulletin of the Korean Chemical Society
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    • 제35권7호
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    • pp.2043-2048
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    • 2014
  • Two isomers of a new tetraaza macrotricycle 2,2,4,9,9,11-hexaazamethyl-1,5,8,12-tetraazatricyclo[$10.2.2^{5.8}$]-octadecane ($L^2$) containing additional N-$CH_2CH_2$-N linkages, C-meso-$L^2$ and C-racemic-$L^2$, have been prepared by the reaction of 1-bromo-2-chloroethane with C-meso-$L^1$ or C-racemic-$L^1$ ($L^1$ = 5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane). Both C-meso-$L^2$ and C-racemic-$L^2$ react with copper(II) ion to form $[Cu(C-meso-L^2)]^{2+}$ or $[Cu(C-racemic-L^2)]^{2+}$ in dehydrated ethanol, but do not with nickel(II) ion under similar conditions. Crystal structure of [Cu(C-racemic-$L^2$)($H_2O$)]$(ClO_4)_2$ shows that the complex has distorted square-pyramidal coordination geometry with an apically coordinated water molecule. Unexpectedly, the Cu-N distances [2.016(3)-2.030(3) ${\AA}$] of [Cu(C-racemic-$L^2$)($H_2O$)]$(ClO_4)_2$ are longer than those [1.992(3)-2.000(3) ${\AA}$] of [Cu(C-racemic-$L^1$)($H_2O$)]$(ClO_4)_2$. As a result, $[Cu(C-racemic-L^2)(H_2O)]^{2+}$ exhibits weaker ligand field strength than $[Cu(C-racemic-L^1)(H_2O)]^{2+}$. The copper(II) complexes readily react with CN- ion to yield the cyano-bridged dinuclear complex $[Cu_2(C-meso-L^2)_2CN]^{3+}$ or $[Cu_2(C-racemic-L^2)_2CN]^{3+}$. Spectra and chemical properties of $[Cu(C-meso-L^2)]^{2+}$ and $[Cu_2(C-meso-L^2)_2CN]^{3+}$ are not quite different from those of $[Cu(C-racemic-L^2)]^{2+}$ and $[Cu_2(C-racemic-L^2)_2CN]^{3+}$, respectively.

$[Ni(L)](ClO_4)_2$(L: 2,13-bis(2-pyridylmethyl)-3,14-dimethyl-2,6,13,17-tetraazatricyclo[14,4,$0^{1.18},0^{7.12}$docosane) 착물의 결정구조 (Crystal Structure of $[Ni(L)](ClO_4)_2$ (L: 2,13-bis(2-pyridylmethyl)-3,14-dimethyl-2,6,13,17-tetraazatricyclo[14,4,$0^{1.18},0^{7.12}$]docosane))

  • Park, Ki-Young;Suh, Il-Hwan;Kim, Jing-Gyu;Park, Young-Soo
    • 한국결정학회지
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    • 제10권1호
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    • pp.88-93
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    • 1999
  • The complex [Ni(L)](ClO4)2 (1) (L=2,13-bis(2-pyridylmethyl)-3,14-dimethyl-2,6,13,17-tetraazatricyclo[14,4,01.1807.12]docosane) has been synthesized and characterized by X-ray crystallography. (1) crystallizes in the triclinic, space group P, with a=10.948(2), b=10.948(2), c=14.911(4) , α=93.73(2), β=93.77(2), γ=99.29(2)o, V=1754.8(7) 3, Z=2, R1(wR2) for 5217 observed reflections of [I>2σ(I)] was 0.048(0.099). The coordination environment around nickel(II) ion shows a distorted octahedron with four secondary and tertially amines of the macrocycle and two nitrogen atoms of pyridylmethyl groups.

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