Synthesis, characterization, and reactivity of a novel μ-η2:η2-diselenidodicopper(II) complex

The first μ-η(2):η(2)-diselenidodicopper(II) complex has been obtained in the reaction of a copper(I) complex with N,N',N″-tribenzyl-cis,cis-1,3,5-triaminocyclohexane and elemental selenium. The structure and reactivity of the complex is described.     

Synthesis and characterization of a novel η 2-iminoacyl monocyclopentadienyl titanium(IV) complex

An unusual complex, [CpTi(η²-(C,N)-2-ArNH–C₆H₄C=NAr)Cl₂] (Ar?=?2,6- ⁱ Pr₂C₆H₃) (1) has been synthesized and characterized by elemental analysis, NMR spectra, and single crystal X-ray diffraction. The ¹³C NMR resonance of the imine carbon atom of 1 at δ?221?ppm is consistent with the η²-(C,N) binding. This was confirmed by single crystal X-ray diffraction study of 1. In the complex, Ti atom is five-coordinate with a η²-bound iminoacyl ligand and one Cp ligand occupying the axial position in a distorted square pyramid.     

Synthesis and crystal structure of dinuclear nickel (Ⅱ) complex

The crystal structure of Ni(Ⅱ) complex with 3-hydroxyl-1, 5-diazacycloheptane-N, N'-diacetate was determined by X-ray diffraction method. Crystal data for Ni2 (C9H14N2O5)2·2H2O: monoclinic, space group P21/n, a = 1.1717(5), b = 0.9794(3), c = 1.2971(2) nm, β= 96.62(3), V= 1.4786(7) nm3, Dc = 1.377 g/cm3, Z = 2,μ=13.321 cm-1 (Mo-Kα), F(000)=640. The final R and Rw are 0.075 and 0.089 respectively. The Ni(Ⅱ) ion forms 2:2 complex with ligand. Two ligands are bridged by two Ni(Ⅱ) atoms which are bridged by two O atoms. Every Ni(Ⅱ) is coordinated by two N atoms and four 0 atoms. The coordination polyhedron of the Ni(Ⅱ) ion is a distorted octahedron.     

Synthesis,characterization, and crystal structure of Ni(II) and Cu(II) complexes with N-furoyl-N′,N′-diethylthiourea: antifungal activity

The complexes cis-bis(N-furoyl-N′,N′-diethylthioureato-k ²O,S)nickel(II) and cis-bis(N-furoyl-N′,N′-diethylthioureato-k ²O,S)copper(II) were prepared by the reaction of metal acetate with the corresponding acylthiourea derivative. The complexes were characterized by IR, ¹H-NMR, ¹³C-NMR, and single-crystal X-ray diffraction. Both complexes show two furoylthiourea ligands bonded to metal to form a four-coordinate complex with square-planar geometry. The antifungal activity of the prepared complexes was studied against the phytopathogenic fungi Botrytis cinerea and Colletotrichum gloeosporioides, responsible for important plant diseases.     

Synthesis,crystal structure,and magnetism of a dinuclear nickel(II) complex [Ni2(MOBPT)2(N3)4] · 2H2O

A dinuclear nickel(II) complex, [Ni₂(MOBPT)₂(N₃)₄] · 2H₂O (MOBPT = 4-(p-methoxyphenyl)-3,5-bis(pyridine-2-yl)-1,2,4-triazole), has been synthesized and characterized by elemental analysis, UV, IR, ESI-MS, and single crystal X-ray crystallography. The complex crystallizes in triclinic system, space group P 1 with a = 9.877(2) Å, b = 10.396(2) Å, c = 11.975(3) Å, α = 71.638(3)°, β = 74.968(3)°, γ = 64.747(3)°, V = 1044.2(4) ų, Z = 1, R = 0.0371 for 5774 observed reflections. The crystal structure determination shows that the dinuclear Ni₂N₈ unit is almost planar with each Ni²⁺ coordinated by four nitrogens from two MOBPT ligands and two axial azides in a distorted octahedral geometry. Magnetic measurements reveal weak antiferromagnetic exchange in the complex.     

Synthesis,structure and magnetism of a hydrogen-bond-linked three-dimensional network of a novel nickel(II)–cobalt(II)–nickel(II) complex containing a new macrocyclic mononuclear complex ligand

A novel trinuclear complex, [Co(NiL)₂(H₂O)₂](ClO₄)₂ · 2C₂H₅OH, was prepared by self-assembly using [NiL] as a new complex ligand; L is the dianion of dimethyl 5,6,7,8,15,16-hexahydro-6,7-dioxodibenzo[1,4,8,11]tetraazacyclotetradecine-13,18-dicarboxylate. The structure of the trinuclear complex was determined by X-ray crystallography. The Co^II ion is at the center of the trinuclear complex cation and occupies a distorted octahedral O₆ environment, approximating to O _h with a ⁴ T _1g ground state for Co^II that has an unquenched spin–orbit coupling reflected in the magnetic properties. Two Ni^II ions reside in completely same and slightly distorted square-planar N₄ coordination geometries. Co^II and each Ni^II are bridged by an oxamido group from one of the two macrocyclic ligands (L). O—H...O and ... interactions link the trinuclear fragments, perchlorate ions and C₂H₅OH molecules to form a three-dimensional supramolecular architecture.     

Synthesis and crystal structure of a novel tri-nuclear nickel(II) complex derived from N,N′-(2-hydroxypropane-1,3-diyl)bis(salicylaldimine)

A novel tri-nuclear nickel(II) complex, [Ni₃L₂(μ₂-η¹:η¹-OAc)₂(μ₁-η¹:η⁰-OAc)₂] · H₂O (H₂L is N,N′-(2-hydroxypropane-1,3-diyl)-bis(salicylaldimine), was prepared. The complex was characterized by elemental analysis, IR spectra, and single crystal X-ray determination (CIF file CCDC no. 993163). Crystal of the complex crystallizes in the monoclinic space group P2₁/n. The unit cell parameters: a = 12.5602(9), b = 13.2104(10), c = 15.0329(10) Å, β = 113.194(2)°, V = 2292.7(3) ų, Z = 2, R ₁ = 0.0506, wR ₂ = 0.1342, S = 1.067. The complex possesses crystallographic inversion center symmetry. The Ni atoms are in octahedral coordination spheres. The Ni?Ni distances are 3.022(1) Å.     

Synthesis and structural characterization of a novel μ 3-CO3 2− bridging trinuclear copper(II) complex

A novel ₃-CO₃ ^2– bridging trinuclear copper(II) complex, formulated as {[Cu₃(2,2-bpy)₆( ₃-CO₃)]₂(ClO₄)₈ · H₂O} (3), has been synthesized by fixation of atmospheric CO₂. The X-ray single crystal determination of (3) reveals that each Cu^II center is penta-coordinated by two 2,2-bipyridine molecules and one oxygen atom of the ₃-carbonato anion forming a distorted pyramid.     

Synthesis,characterization, and crystal structure of one zinc(II) complex with 4-Hydroxypyridine-2,6-Dicarboxylic acid and 4,4′-bipyridine

A new zinc(II) coordination polymer, {[Zn(HCAM)(4,4′-Bipy)_0.5] · H₂O} _n (I) (H₃CAM = 4-hydroxypyridine-2,6-dicarboxylic acid; 4,4′-Bipy = 4,4′-bipyridine), has been synthesized by hydrothermal reaction of Zn(OAc)₂, H₃CAM and 4,4′-Bipy. It has been structurally characterized by element analysis, IR-spectra. X-ray single-crystal analysis was carried out for I (CIF file CCDC no. 974199), which crystallizes in the orthorhombic system, space group Pbca. The single X-ray diffraction studies reveal that I shows a new 2D wave-like plane with 3-connected net. Furthermore, the thermal stability of compound I was studied.     

Synthesis,crystal structure,and characterization of energetic complex Pb(ATZ)(phen)2 · 3H2O

A new energetic complex, Pb(ATZ)(phen)₂·3H₂O (1) (ATZ = 5,5′-azotetrazolate), was synthesized and characterized by single crystal X-ray diffraction. Crystal data: monoclinic, P2(1)/n space group, a = 8.4545(1) Å, b = 25.846(2)Å, c = 13.096(2)Å, and β = 102.873(2)°. In addition, elemental analysis, IR, and thermogravimetric analysis are presented. Furthermore, the complex was also explored as an additive to promote thermal decomposition of ammonium perchlorate.     

Synthesis,characterization, crystal structure,and DNA binding of two copper(II)–hydrazone complexes

Two new Cu(II)–hydrazone complexes, [Cu(L)(Hbpe)ClO₄]·ClO₄·[Cu(L)Cl] (1) and [Cu(HL)₂]·1.5ClO₄·0.5OH (2) (where HL?=?(E)-N′-(1-(pyridine-2-yl)ethylidene)benzohydrazide and bpe = trans-1-(2-pyridyl)-2-(4-pyridyl)ethylene), have been synthesized and characterized by physicochemical methods. The structures of the complexes have been established by single-crystal X-ray diffraction direct methods, which reveal that the metal ions have distorted square-pyramidal and square-planar geometries in 1, and a distorted octahedral geometry in 2. DNA binding of HL, 1, and 2, performed by UV–vis titration in tris-buffer medium, yielded binding constants, which are 9.5 × 10³, 1.88 × 10⁴, and 4.66 × 10⁴ M^?1, respectively. Viscosity measurements suggest a surface or groove-binding mode of interaction between CT-DNA with HL, 1, and 2.     

Cobalt(II) hexaiododimercurate(II) complex with ε-caprolactam: Synthesis and crystal structure

The conditions of synthesis of a new binary complex salt [Co(Cpl)₆][Hg₂I₆] (Cpl is ε-caprolactam ε-C₆H₁₁NO) have been developed, and its structure has been characterized. The salt crystallizes in triclinic system, space group \(P\bar 1\), a = 10.1078(4) Å, b = 12.2680(5) Å, c = 13.0782(5) Å, α = 62.872(2)°, β = 72.394(2)°, γ = 76.834(2)°, V = 1367.98(9) ų, Z = 1, and ρ_calc = 2.297 g/cm³. The structure is insular and consists of isolated ions.     

Synthesis,crystal structure,antibacterial activities,and DNA-binding studies of a new μ-oxamido-bridged binuclear copper(II) complex

A new μ-oxamido-bridged dicopper(II) complex, Cu₂(heap)(NO₃)₂ (1), where heap is the dianion of N,N′-bis(N-hydroxyethylaminopropyl)oxamide, has been synthesized and characterized by elemental analysis, molar conductivity, IR and electronic spectral studies, and X-ray single-crystal diffraction. The complex consists of a neutral centro-symmetric binuclear copper(II) unit with an inversion center at the midpoint of the Cl?Clⁱ bond. The copper(II) has square-pyramidal coordination geometry and the bridging heap adopts a bis-tetradentate conformation. The binuclear units are linked into a 3-D framework by N?H ··· O, O?H ··· O, and C?H ··· O hydrogen bonds. Due to weak coordination between copper(II) and nitrate, the neutral dicopper(II) units are present as binuclear cations and nitrate anions in solution. Antibacterial assays indicate that the complex shows better activity than the ligand. Interactions of the complex with herring sperm DNA (HS-DNA) have been investigated by using cyclic voltammetry, UV absorption titrations, ethidium bromide fluorescence displacement experiments, and viscometry measurements. The results suggest that the binuclear copper(II) complex interacts with HS-DNA by electrostatic interaction with intrinsic binding constant of 3.33 × 10⁴ M^?1.     

Synthesis and characterization of a dipeptide–copper(II)– 2-aminomethylbenzimidazole ternary complex

A new ternary complex [Cu(glygly)(AMBZ)(H₂O)]Cl·H₂O (1) (glygly?=?glycylglycine anion, AMBZ?= 2-aminomethylbenzimidazole) has been prepared and characterized by single-crystal X-ray diffractometry and ESR, electronic and IR spectroscopy. The copper(II) ion has a slightly distorted square-pyramidal coordination, being equatorially coordinated by the bidentate 2-aminomethylbenzimidazole and the bidentate glycylglycine anion and axially by a water molecule. The individual complex molecules are hydrogen bonded to their neighbors, forming a polymeric hydrogen-bonded lattice. Spectroscopic data are in accordance with the crystal structure.     

Synthesis, crystal structure and magnetic properties of bimetallic complex of Ni2Co(TTHA)·12H2O

The bimetallic complex of Ni₂Co(TTHA)·12H₂O (TTHA = triethylene tetraminehexaacetic acid) was synthesized and characterized structurally and magnetically. The title complex crystallizes in the triclinic space group P ī with a = 0.7316(2), b = 0.8624(2), c = 1.5041(4) nm; α = 73.38(2), β = 83.97(2), γ = 70.50(2)°. The crystal structure is built up of [Ni₂(TTHA)(H₂O)₂]²⁻, Co(H₂O)₆²⁺ and water molecules. The variable magnetic measurement shows that there is strong antiferromagnetic interaction between two Ni(II) ions in [Ni₂(TTHA) (H₂O)₂]²⁻ with J _Ni−Ni = −141.64 cm⁻¹, g _Ni = 2.21 and that the constant of spin-orbit coupling of Co(II) ion is −134.8 cm⁻¹. __________ Translated from Acta Scientiarum Naturalium Universitatis Nankaiensis, 2007, 40(1): 6–10 [译自: 南开大学学报(自然科学版)]     

Synthesis, crystal structure and magnetic properties of a novel manganese(II)-nitronyl nitroxide-azido(μ_(1,1) and μ_(1,3)) one-dimensional complex

A novel one-dimensional manganese(Ⅱ) complex containing nitronyl nitroxide radical [Mn2(IM2-py)2(Ac)2((μ1.1-N3)(μ1,3-N3) . EtOH]n was synthesized and characterized structurally and magnetically. It crystallizes in the monoclinic space group p21/n. Each Mn(Ⅱ) ion is six-coordinated in a distorted octahedral environment. The two N atoms of the nitronyl nitroxide radical and the two O atoms of acetate ligands are in the equatorial plane, whereas the two different azido bridging ligands are in trans axial position. Mn(Ⅱ) ions are linked by nitrogen atom of μ1,1-azido and oxygen atoms of two carboxy groups to form a Mn-Mn unit. Mn-Mn units are linked by azido ligands through u1,3 bridging style to form a one-dimensional chain. The compound is connected by the coordination bonds,π-π interactions and hydrogen bonds as a three-dimensional structure. Magnetic susceptibility data support that there are stronger antiferromagnetic interactions between the radical and Mn(Ⅱ) ion, weak antiferromagnetic inter