Synthesis and Crystal Structure of Two Succinato-Bridged Macrocyclic Nickel(II) Complexes
01 Jan 2013-Zeitschrift für anorganische und allgemeine Chemie (WILEY‐VCH Verlag)-Vol. 639, Iss: 1, pp 158-162
TL;DR: Two dinuclear succinato-bridged nickel(II) complexes were synthesized and characterized by EA, Circular dichroism (CD), as well as IR and UV/Vis spectroscopy as discussed by the authors.
Abstract: Two dinuclear succinato-bridged nickel(II) complexes [Ni(RR-L)]2(μ-SA)(ClO4)2 (1) and [Ni(SS-L)]2(μ-SA)(ClO4)2 (2) (L = 5, 5, 7, 12, 12, 14-hexamethyl-1, 4, 8, 11-tetraazacyclotetradecane, SA = succinic acid) were synthesized and characterized by EA, Circular dichroism (CD), as well as IR and UV/Vis spectroscopy Single crystal X-ray diffraction analyses revealed that the NiII atoms display a distorted octahedral coordination arrangement, and the succinato ligand bridges two central NiII atoms in a bis bidentate fashion to form dimers in 1 and 2 The monomers of {[Ni(RR-L)]2(μ-SA)}2+ and {[Ni(SS-L)]2(μ-SA)}2+ are connected by O–H···O and N–H···O hydrogen bonds into a 1D right-handed and left-handed helical chain along the b axis, respectively The homochiral natures of 1 and 2 are confirmed by the results of CD spectroscopy
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01 Jan 2015
TL;DR: In this paper, two complexes with formulas [NiL][(NiL)(IPA)2]·8H2O (1) and [(NiL), H2O(2)], respectively, were synthesized and characterized by elemental analyses and IR spectra.
Abstract: Two complexes with formulas [NiL][(NiL)(IPA)2]·8H2O (1) and [(NiL)(H2O)2] [(NiL)(PMA)]·4H2O (2) (L = 5,5,7,12,12,14-hexamethyl-1,4,8,11tetraazacyclotetradecane, IPA = isophthalic anion, PMA = 1,2,4,5-benzenetetracarboxylic anion) were synthesized and characterized by elemental analyses and IR spectra. The crystal structures were determined by X-ray diffraction. In complex 1, the [NiL] bridged IPA to give [(NiL)(IPA)2] monomer, and the [NiL] bridged PMA to form a one-dimensional chain [(NiL)(PMA)]n in complex 2. The [NiL] and [(NiL)(IPA)2]/[(NiL)(PMA)] are connected through intermolecular hydrogen bonding to generate three-dimensional supramolecular structures.
1 citations
TL;DR: In this article , the triclinic trichloric tricline is defined as follows: a = 11.180(2) Å, b = 12.320(3)Å, c= 12.754(3), α = 98.263 (2)°, β = 97.524(2 )°, γ = 99.470(2 Ã
Abstract: Abstract C27H49ClN4NiO12, triclinic, P 1 ‾ $\overline{1}$ (no. 2), a = 11.180(2) Å, b = 12.320(3) Å, c = 12.754(3) Å, α = 98.263(2)°, β = 97.524(2)°, γ = 99.470(2)°, V = 1693.1(6) Å3, Z = 2, Rgt(F) = 0.0423, wRref(F2) = 0.1238, T = 296(2) K.
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TL;DR: In this article, a monoclinic C2/c (no. 15), a = 25.731(5) Å, b = 9.940(2)
Abstract: Abstract C50H92Cl2N12Ni2O14, monoclinic, C2/c (no. 15), a = 25.731(5) Å, b = 9.940(2) Å, c = 26.574(5) Å, β = 114.825(4)°, V = 6169(2) Å3, Z = 4, Rgt(F) = 0.0675, wRref(F2) = 0.2209, T = 173(2) K.
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1,116 citations
TL;DR: The Dawson anion P2W18O626− has been used as a noncoordinating polyoxoanion template for the construction of two metal−organic frameworks as discussed by the authors.
Abstract: The Dawson anion P2W18O626− has been used as a noncoordinating polyoxoanion template for the construction of two metal−organic frameworks, namely, [M2(bpy)3(H2O)2(ox)][P2W18O62]2(H2-bpy)·nH2O (M = Co(II), n = 3 (1); M = Ni(II), n = 2 (2)) (bpy = 4,4′-bipyridine; ox = C2O42−). Single-crystal X-ray analysis reveals that both of the structures exhibit 3D host frameworks constructed from the oxalate-bridged binuclear superoctahedron secondary building units (SBUs) and bpy linkers and the voids of which are occupied by Dawson anions, guest bpy, and water molecules. Magnetic studies reveal that there are antiferromagnetic exchange interactions among the transition-metal centers in compounds 1 and 2. Furthermore, a compound 1-modified carbon paste electrode (1-CPE) displays good electrocatalytic activity toward the reduction of nitrite.
138 citations
TL;DR: Compounds 3 and 4 are isostructural and exhibit network topologies similar to that of 1 with open channels occupied by disordered trans-3-(3-pyridyl)acrylic acid and water guest molecules.
Abstract: Three-dimensional open frameworks [Co2(nicotinate)4(μ-H2O)]·CH3CH2OH·H2O, 1, and [Ni2(nicotinate)4(μ-H2O)]·CH3CH2OH·H2O, 2, were obtained by hydro(solvo)thermal reactions between 3-cyanopyridine and cobalt(II) nitrate and nickel(II) perchlorate, respectively. Both 1 and 2 exhibit complicated 3-D structures based on [M2(nicotinate)4(μ-H2O)] (M = Co or Ni) building blocks and possess open channels that are occupied by removable solvent molecules. 3-D open frameworks [M2L4(μ-H2O)]·HL·(H2O)x (where M = Co, x = 2, 3, and M = Ni, x = 1, 4, and L = trans-3-(3-pyridyl)acrylate) were similarly prepared with trans-3-(3-pyridyl)acrylic acid in place of 3-cyanopyridine. Compounds 3 and 4 are isostructural and exhibit network topologies similar to that of 1 with open channels occupied by disordered trans-3-(3-pyridyl)acrylic acid and water guest molecules. Crystal data for 1: triclinic space group P1, a = 10.534(1) A, b = 11.907(1) A, c = 14.046(1) A, α = 106.645(1)°, β = 101.977(1)°, γ = 112.078(1)°, and Z = 4. Cry...
85 citations
TL;DR: In this paper, an end-to-end azido-NiII complex was synthesized and structurally characterized by spectroscopic techniques, X-ray crystallography, and variable-temperature magnetic measurements.
Abstract: Azido–NiII complexes of dinuclear, [Ni2(trpn)2(μ1,3-N3)2](ClO4)2 (1), and monodimensional structures cis-[Ni(abap)(μ1,3-N3)]n(ClO4)n (2) and cis-[Ni(Me6trien)(μ1,3-N3)]n(ClO4)n·nH2O (3a) as well as the monomer [Ni(Me6trien)(N3)]ClO4 (3b) {trpn = tris(3-aminopropyl)amine; abap = N-(2-aminoethyl)-N,N-bis(3-aminopropyl)amine; Me6trien = 1,1,4,7,10,10-hexamethyltriethylene tetramine} were synthesized and structurally characterized by spectroscopic techniques, X-ray crystallography, and variable-temperature magnetic measurements. In the complexes 1–3a, the ClO4– groups are counterions and the Ni2+ centers are bridged by the azido ligands in an end-to-end bonding fashion. The coordination geometry around the NiII ions is six-coordinate with a distorted octahedral environment achieved by the four N atoms of the tetradentate amines and two terminal N atoms of the azide groups. Complex 1 consists of dinuclear units with doubly bridged azido groups whereas in 2 and 3a, a polymeric 1D chain is formed in which the adjacent azido groups link the NiII centers in a cis arrangement. In complex 2, the structural parameters of the two adjacent azido bridging ligands are different and an alternating 1D system with two different end-to-end azido bridges is produced. Complex 3a is a uniform 1D system where the strong steric hindrance imposed by the methyl groups of the Me6trien ligand [diagonal N(azide)–Ni–N(amine) bond angles] causes pronounced deviation from the ideal octahedral geometry. Complex 3b exhibits a distorted square pyramidal geometry. The complexes 1–3a show antiferromagnetic coupling. In complex 1, the exchange coupling constant was J = –64(1) cm–1, whereas in the polynuclear species 2 and 3a, the calculated values were J1 = –63.7(2) (α = 0.52) and J = –26.8(1) cm–1, respectively. The magnetic parameters have been correlated to the structural data.(© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2007)
84 citations