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

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Synthesis and Characterization of Nickel(II) Tetraaza Macrocyclic Complex with 1,1-Cyclohexanediacetate Ligand

  • Lim, In-Taek;Kim, Chong-Hyeak;Choi, Ki-Young
    • 대한화학회지
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    • 제62권6호
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    • pp.427-432
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    • 2018
  • The reaction of [$[Ni(L)]Cl_2{\cdot}2H_2O$ (L = 3,14-dimethyl-2,6,13,17-tetraazatricyclo[$14,4,0^{1.18},0^{7.12}$]docosane) with 1,1-cyclohexanediacetic acid ($H_2cda$) yields mononuclear nickel(II) complex, [$Ni(L)(Hcda^-)_2$] (1). This complex has been characterized by X-ray crystallography, electronic absorption, cyclic voltammetry and thermogravimetric analyzer. The crystal structure of 1 exhibits a distorted octahedral geometry with four nitrogen atoms of the macrocycle and two 1,1-cyclohexanediacetate ligands. It crystallizes in the triclinic system P-1 with a = 11.3918(7), b = 12.6196(8), $c=12.8700(8){\AA}$, $V=1579.9(2){\AA}^3$, Z = 2. Electronic spectrum of 1 also reveals a high-spin octahedral environment. Cyclic voltammetry of 1 undergoes one wave of a one-electron transfer corresponding to $Ni^{II}/Ni^{III}$ process. TGA curve for 1 shows three-step weight loss. The electronic spectra, electrochemical and TGA behavior of the complex are significantly affected by the nature of the axial $Hcda^-$ ligand.

Synthesis and Structure Analysis of α and β Forms of [12] Metallacrown-6 Nickel(II) Complex: [Ni6(SCH2CH2CH3)12]

  • Xiao, Hai Lian;Jian, Fang Fang;Zhang, Ke Jie
    • Bulletin of the Korean Chemical Society
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    • 제30권4호
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    • pp.846-848
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    • 2009
  • Two modifications of the ${\alpha}\;and\;{\beta}$ forms of propyl mercaptan nickel(II) cluster, [$Ni_6(SCH_2CH_2CH_3)_{12}$], have been synthesized and their crystal structures have been determined by single-crystal X-ray diffraction. The alkyl groups are away from $Ni_6$ ring in $\alpha$ form whereas they are near to the Ni atom in $\beta$ form. The distance of Ni-H in $\beta$ form [2.576(5) $\AA$] is much shorter than that in $\alpha$ form [3.101(2) $\AA$]. In the crystal lattice of $\beta$ form, the whole structure forms a flower shape.

$[Ni(C_2N_2H_8)_3]\cdotCrO_4$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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Synthesis and Characterization of New Tetraaza Macrocycles Bearing Two or Four N-Methoxyethyl Pendant Arms and Their Copper(II) and/or Nickel(II) Complexes

  • Kang, Shin-Geol;Kim, Hyun-Ja;Kwak, Chee-Hun
    • Bulletin of the Korean Chemical Society
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    • 제31권9호
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    • pp.2701-2704
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    • 2010
  • This work shows that both L2 and L3 bearing two and four N-$(CH_2)_2OCH_3$ groups, respectively, can be prepared selectively by the reaction of $L^1$ with 1-bromo-2-methoxyethane. The di-N-substituted macrocycle $L^2$ readily forms its copper(II) and nickel(II) complexes. The N-$(CH_2)_2OCH_3$ groups in $[CuL^2]^{2+}$ are coordinated to the metal ion, whereas those in $[NiL^2]^{2+}$ are not involved in coordination. Interestingly, $L^3$ reacts with $Cu^{2+}$ ion to form $[Cu(HL^3)]^{3+}$, in which one tertiary amino group is not involved in coordination.

Hydro/solvothermal synthesis, crystal structure, and thermal behaviour of piperazine-templated nickel(II) and cobalt(II) sulfates

  • Kim, Chong-Hyeak;Park, Chan-Jo;Lee, Sueg-Geun
    • 분석과학
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    • 제19권4호
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    • pp.309-315
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    • 2006
  • Two piperazine-templated metal sulfate complexes, $(C_4N_2H_{12})[Ni(H_2O)_6](SO_4)_2$, I and ($C_4N_2H_{12}$) $[Co(H_2O)_6](SO_4)_2$, II, have been synthesized by hydro/solvothermal reactions and their crystal structures analyzed by single crystal X-ray diffraction methods. Complex I crystallizes in the monoclinic system, $P2_1/n$ space group, a=12.920(3), b=10.616(2), $c=13.303(2){\AA}$, ${\beta}=114.09(1)^{\circ}$, Z=4, $R_1=0.030$ for 3683 reflections; II: monoclinic $P2_1/n$, a=12.906(3), b=10.711(2), $c=13.303(2){\AA}$, ${\beta}=114.10(2)^{\circ}$, Z=4, $R_1=0.032$ for 4010 reflections. The crystal structures of the piperazine-templated metal(II) sulfates demonstrate zero-dimensional compound constituted by diprotonated piperazine cations, metal(II) cations and sulfate anions. The structures of complex I and II are substantially isostructural to that of the previously reported our piperazine-templated copper(II) sulfate complex $(C_4N_2H_{12})[Cu(H_2O)_6](SO_4)_2$. The central metal(II) atoms are coordinated by six water molecules in the octahedral geometry. The crystal structures are stabilized by three-dimensional networks of the $O_{water}-H{\cdots}O_{sulfate}$ and $N_{pip}-H{\cdots}O_{sulfate}$ hydrogen bonds between the water molecules and sulfate anions and protonated piperazine cations. Based on the results of thermal analysis, the thermal decomposition reactions of the complex I was analyzed to have three distinctive stages whereas the complex II proceed through several stages.

Synthesis and Characterization of Dinuclear Ni(II) Complexes with Tetraazadiphenol Macrocycle Bearing Cyclohexanes

  • Kim, Ki-Ju;Jung, Duk-Sang;Kim, Duk-Soo;Choi, Chi-Kyu;Park, Ki-Min;Byun, Jong-Chul
    • Bulletin of the Korean Chemical Society
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    • 제27권11호
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    • pp.1747-1751
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    • 2006
  • The dinuclear tetraazadiphenol macrocyclic nickel(II) complexes [$Ni_2$([20]-DCHDC)]$Cl_2$ (I), [$Ni_2$([20]-DCHDC)]$(ClO_4)_2{\cdot}2CH_3CN $ (II(b)) and [$Ni_2$([20]-DCHDC)$(NCS)_2$] (III) {$H_2$[20]-DCHDC = 14,29-dimethyl-3,10,18,25-tetraazapentacyclo-[25,3,1,$0^{4,9}$,$1^{12,16}$,$0^{19,24}$]ditriacontane-2,10,12,14,16(32),17,27(31), 28,30-decane-31,32-diol} have been synthesized by self-assembly and characterized by elemental analyses, conductances, FT-IR and FAB-MS spectra, and single crystal X-ray diffraction. The crystal structure of II(b) is determined. It crystallizes in the monoclinic space group P2(1)/c. The coordination geometries around Ni(II) ions in I and II(b) are identical and square planes. In complex III each Ni(II) ion is coordinated to $N_2O_2$ plane from the macrocycle and N atoms of NCS- ions occupying the axial positions, forming a square pyramidal geometry. The nonbonded Ni…Ni intermetallic separation in the complex II(b) is 2.8078(10) $\AA$. The FAB mass spectra of I, II and III display major fragments at m/z 635.1, 699.4 and 662.4 corresponding to [$Ni_2$([20]-DCHDC)(Cl + 2H)]$^+$, [$Ni_2$([20]-DCHDC)$(ClO_4\;+\;2H)]^+$ and [$Ni_2$([20]-DCHDC)(NCS) + 6H]$^+$, respectively.