• 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.

• Bulletin of the Korean Chemical Society
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• 제35권11호
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• pp.3357-3359
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• 2014

• 대한화학회지
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• 제9권3호
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• pp.121-123
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• 1965

Ni(II)-Monoethanolamine(MEA)錯鹽의 水銀電極表面에 있어서의 還元反應의 反應機構를 폴라로그라프법을 써서 解明하였다. 이 錯鹽의 電極環元의 可逆程度를 直流 및 交流 폴라로그람으로 檢討하였더니 pH가 9.0보다 낮은 範圍에서는 錯鹽의 反應電流로 推測되는 非可逆性波를 나타니고 pH $9.5{\sim}11.0$ 사이에서는 Cd(II)波에 相當하는 比較的 可逆的인 well defined wave를 얻었다. MEA의 濃度와 pH를 變함으로서 얻은 波를 檢討한 結果 還元波는 이를 ligands와 빠른 平衡에 있는 Ni錯鹽에 基因하고 이 錯鹽의 化學式은 $Ni(MEA)_3OH$이고 總安定度常數는 約 $10^{20}$임을 밝혀내었다.

• 한국결정학회지
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• 제8권2호
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• pp.124-126
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• 1997

[Ni(L)](ClO4)2(L:3,5,10,12-tetramethly-1,4,8,11-tetraazacyclotetradecane), C14H32Cl2N4NiO8, 착물은 NiN4 평면4각구조를 가지며 열력학적으로 가장 안정한 trans-III구조를 하고 있다.

• 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.

• 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.

• Bulletin of the Korean Chemical Society
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• 제27권10호
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• pp.1705-1707
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• 2006

• Bulletin of the Korean Chemical Society
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• 제34권10호
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• pp.2889-2894
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• 2013

A new complex [$Ni(phen)(C_9H_8Br_2NO_3)_2{\cdot}2CH_3OH{\cdot}2H_2O$] [phen: 1,10-phenanthroline $C_9H_8Br_2NO_3$: 3,5-dibromo-L-tyrosine] was synthesized and characterized by IR, elemental analysis and single crystal X-ray diffraction. X-ray crystallography shows that Ni(II) ion is six-coordinated. The Ni(II) ion coordinates with four nitrogen atoms and two oxygen atoms from three ligands, forming a mononuclear Ni(II) complex. The crystal crystallizes in the Orthorhombic system, space group $P2_12_12$ with a = 12.9546 ${\AA}$, b = 14.9822 ${\AA}$, c = 9.9705 ${\AA}$, V = 1935.2 ${\AA}$, Z = 1, F(000) = 1008, S = 0.969, ${\rho}_{calcd}=1.742g{\cdot}cm^{-3}$, ${\mu}=4.688mm^{-1}$, $R_1$ = 0.0529 and $wR_2$ = 0.0738 for 3424 observed reflections (I > $2{\sigma}(I)$). Theoretical study of the title complex was carried out by density functional theory (DFT) method and the B3LYP method employing the $6-3l+G^*$ basis set. The energy gap between HOMO and LUMO indicates that this complex is prone to interact with DNA. CCDC: 908041.

• 대한화학회지
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• 제51권6호
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• pp.499-505
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• 2007

세자리 비스(이미노)알릴 (N,C,N-집게발) 리간드를 가진 단핵 Ni(II) 착물을 발표하고자 한다. 새로운 착물(2,6-(ArN=CH)2C6H3)NiBr (Ar=2,6-dimethylphenyl (1), 2,6-diisopropylphenyl (2))은 산화성 첨가반응에 의해 Ni(COD)2 (COD=1,5-cyclooctadiene)와 1,3-(ArN=CH)2C6H3Br (bis(N-Ar)-2-bromoisophthalaldimine: Ar=Ph-2,6-Me2, Ph-2,6-iPr2) 으로부터 높은 수율로 합성하였다. 리간드와 니켈 착물에 대한 개선된 합성경로에 대하여 설명하고자 한다. 니켈(II) 착물 1, 2는 적외선 분광학, 수소-핵자기공명, 그리고 원소분석에 의해 구조를 밝혔다. 합성한 니켈 착물을 촉매로 사용하여 에틸렌 중합반응을 시도하였으나 목적하는 에틸렌고분자는 얻어지지 않고 소량의 올리고머가 형성되었다. 본 연구에서 합성한 니켈 착물이 에틸렌고분자 촉매반응에 활성을 보이지 않는 이유는 아마도 집게발 착물의 높은 경직성과 리간드의 비치환성 때문에 반응에 필요한 적합한 조건을 제공하지 못 했다고 사료된다.

• Bulletin of the Korean Chemical Society
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• 제12권4호
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• pp.368-370
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• 1991

The electrochemical behavior and the complex formation between N$i^{2+}$ and 1,7-diazs-15-crown-5 and 1,10-diaza-18-crown-6 in acetonitrile solution have been studied by DC polarography, differential puke polarography and cyclic voltammetry. Nickel(Ⅱ) complexes gave a single well-defined wave. The formation constants of their complexes were 1$0^{4.89} and 10^{3.86}$, respectively. Nickel(Ⅱ) ion was found to form complexes of 1-to-1 composition with 1,7-diaza-15-crown-5 and 1,10-diaza-18-crown-6. In addition, reduction steps were irreversible and the reduction current were diffusion controlled. The electrochemical reduction mechanism of Ni(Ⅱ)-macrocyclic diaza-crown complexes in acetonitrile solution is estimated.