Synthesis of a novel perylene diimide derivative and its charge transfer interaction with C_(60)

A novel organic electron acceptor, N,N′-dipyrimidinyl-3,4,9,10-perylene-tetracarboxylic diimide (DMP), was designed and synthesized. The molecular structure was characterized by FTIR spectrum and elemental analysis. By cyclic voltammetry measurements, DMP was found to possess a lower LUMO energy level than N,N′-diphenyl-3,4,9,10-perylene-tetracarboxylic diimide due to the stronger electron-withdrawing pyrimidinyl group than the phenyl group. Fluorescence quenching is observed in a dual-layer film consisting of a DMP layer and a C60 layer and was attributed to the charge transfer at the interface due to the energy level offset between DMP and C60.     

Synthesis of a new 2,2′：6′,2″-terpyridine derivative and its coordination property

A novel compound, （E）-4′-（4-（but-1-en-3-ynyl）phenyl）-2,2′：6′,2″-terpyridine 1 was synthesized from 4′-（4-bromomethylphenyl）-2,2P：6P,2PP-terpyridine phosphonium salt 2 and propargylaldehyde via Wittig reaction, and characterized by EI-MS and ^1H NMR as well as elemental analysis. The spectral changes of the compound in the presence of transition metal ions, such as Cu（I） or Zn（ID, are investigated.     

Synthesis of a new 2,2'''':6'''',2''''''''-terpyridine derivative and its coordination property

A novel compound, (E)-4'-(4-(but-1-en-3-ynyl)phenyl)-2,2':6',2'-terpyridine 1 was synthesized from 4'-(4-bromomethylphe- nyl)-2,2':6',2'-terpyridine phosphonium salt 2 and propargylaldehyde via Wittig reaction, and characterized by EI-MS and 1H NMR as well as elemental analysis. The spectral changes of the compound in the presence of transition metal ions, such as Cu(Ⅰ) or Zn(Ⅱ), are investigated.     

Synthesis and inclusion capability of a β-cyclodextrin-tetrathiafulvalene derivative

The synthesis of 4,5-ethylenedithio-4′-[6-deoxy-β-cyclodextrin-6-yl-aminocarbonyl]-tetrathiafulvalene 3 is reported. Dominantly, the structure of 3 has been established on the basis of mass spectrometry, ROESY and ¹H NMR spectra, combined with a theoretical MM3 study, indicating an ‘open-cavity structure’. The sensing ability of 3 and the formation constant of the complex [(3)-(1-adamantanol)] have been evaluated experimentally by UV-vis spectroscopy and theoretically by the MM3 docking procedure method.     

Synthesis and curing of a novel amino-containing phthalonitrile derivative

A novel phthalonitrile derivative containing an amino group, 3,5-bis(3,4-dicyanophenoxy)aniline (CPA), was synthesized via a nucleophilic displacement of 4-nitrophthalonitrile and 5-aminoresorcinol hydrochloride. The structure of CPA was confirmed by Fourier transform infrared spectra (FT-IR) and nuclear magnetic resonance (1H NMR). Thermal analysis performed on CPA revealed that the novel phthalonitrile derivative showed a self-promotion curing behavior and the resulting polymer exhibited outstanding heat-resistance.     

Molecular recognition on supramolecular systems (XXXV)——Synthesis of novel β-cyclodextrin derivative bearing pyridinio group and its chiral discrimination of amino acids

A novel p-cyclodextrin derivative 4 bearing a pyridinio group on the primary side was synthesized by the reaction of 2-aminopyridine with 6-p-cyclodextrin monoaldehyde 3, and its complexation stability constants with several aliphatic amino acids have been determined in phosphate buffer solution ( pH = 7.2, 0.1 mol ?L~(-1)) at 25℃by using spectrofluorometric titrations. The stoichiometry is 1 : 1 for the inclusion complexation of amino acids with compound 4. Circular dichroism study indicates that the aromatic moiety was embedded shallowly into the cyclodextrin cavity. As a spectral probe, the pyridinio group in the modified cyclodextrin can recognize not only differences of the size and shape of amino acid molecules, but also the L/D-amino acid chiral iso-mer. As compared with mono-[6-(1-pyridinio)-6-deoxy]-p-cyclodextrin 5, compound 4 switched the enantiomer preference for L- to D-isomer, and showed the highest enantioselectivity of 5.4 for D/L-serine. These results are discussed from the viewpoints of ge     

Synthesis,characterization, and antibacterial activities of two new copper(II) glycinate complexes incorporating 2-(4′-thiazolyl)benzimidazole/2-(2-pyridyl)benzimidazole

Two new complexes, [Cu(TBZ)(Gly)(H₂O)]Cl (1) and [Cu(HPB)(Gly)Cl]?·?2H₂O (2) (TBZ?=?2-(4′-thiazolyl)benzimidazole, HPB?=?2-(2-pyridyl)benzimidazole, and Gly?=?glycinate), have been synthesized and characterized by elemental analysis, molar conductivity, UV-Vis, and IR methods. The complexes, structurally characterized by single-crystal X-ray crystallography, show a slightly distorted square-pyramidal coordination geometry in which two nitrogen atoms of TBZ or HPB and the carboxylate oxygen and amino nitrogen of glycinate bind in the plane and a water or chloride coordinated at the axial site. The complexes, free ligands, and copper(II) chloride were tested for their ability to inhibit growth of Bacillus subtilis, Staphylococcus aureus, and Salmonella. The results show that the complexes have good antibacterial activities against the microorganisms compared with their ligands and copper(II) chloride.     

Synthesis and structure of Cu(II) and Pd(II) coordination compounds with chiral α-thiooxime,a derivative of natural terpenoid (−)-α-pinene

The paramagnetic complex Cu(HL)Cl₂(I) (μ_eff = 1.88 μ_B) and the diamagnetic complex Pd(HL)Cl₂(II) with chiral α-thiooxime, a derivative of natural terpenoid (?)-α-pinene (HL), were synthesized. The crystal structures of these complexes were determined from single-crystal X-ray diffraction data (X8 APEX diffractometer, MoK _α radiation, 2975 F _hkl , R = 0.0258 for I and 3270 F _hkl , R = 0.0222 for II). The crystals of complex I are monoclinic, a = 9.3376(3) Å, b = 6.8619(2) Å, c = 14.6540(5) Å, β = 97.814(1)°, V = 930.22(5) ų, Z = 2, ρ_calc = 1.513 g/cm³, space group P2₁. The crystals of complex II are orthorhombic, a = 7.0084(6) Å, b = 9.2113(9) Å, c = 29.081(3) Å, V = 1877.4(3) ų, Z = 4, ρ_calc = 1.651 g/cm³, space group P2₁2₁2₁. The structures are composed of mononuclear molecules. The coordination cores MNSCl₂ (M = Cu, Pd) are tetrahedrally distorted squares. According to NMR data, complex II has a similar structure in a CDCl₃ solution. The intermolecular contacts in structure I generate supramolecular polymeric ribbons lying parallel to axis b. No short intermolecular contacts are present in complex II.     

Synthesis of 2-(2-Thienyl)benzimidazoles by the Reaction of 2-(Mercaptomethyl)benzimidazole With β-Electrophilic Esters

New 2-(2-di- and tetrahydrothienyl)benzimidazole compounds were prepared by the ring closure reactions of 2-(mercaptomethyl)benzimidazole^1,2 (1) and α,β-unsaturated compounds activated with electron-withdrawing groups.     

Optimization of polyacrylonitrile-cysteine resin synthesis and its selective removal of Cu(Ⅱ) in aqueous solutions

Polyacrylonitrile beads(PAN) cysteine(CS) was synthesized from polyacrylonitrile beads(PAN) and cysteine(CS).The content of the functional group and the percentage conversion of the functional group of PAN-CS prepared under the optimum condition using response surface methodology(RSM) for the first attempt were 3.22 mmol/g and 35.78%.The structure was characterized by ET-IR and elemental analysis.The adsorption properties of the resin for Cu(Ⅱ) were investigated by batch and column experiments.Batch adsorption results suggested that PAN-CS had higher adsorption capability for Cu(Ⅱ)than other metal ions and maximum saturated adsorption capacity was 184.7 mg/g.The resin and its metal complexes were studied by FT-IR.Furthermore,the resin can be eluted easily using 1 mol/L HC1.PAN-CS can provide a potential application for selective removal of copper from waste solution.     

Synthesis of ( ) 8-O-Cinnamyl-p-chlorogoniotriol and its Analogues

HowiinolAI',anovellactoneisolatedfromtheethanolicextractsoftherootandsternbarkofGoniolhanlush()TI)iiMerr.(Annoaceae)inourlaboratory.hasbeenshowntopossesssignificantantitullloractivitiestowardhumantumor117vilroandI,71'if'oandfoxytoxlcit}.Recently.wehavesynthesized1anditsderivativeswitllditTerentestergroupsstartingfromcommerciallyavailablea-D-glucoheptonic-y-lactone.Inordertotindtheirrelationshipofstructureandactivityandtosearchfordrugswithmorepotentantitumoractivity.wehavesynthesized( )8-O-…     

Synthesis, fluorescence properties and selective Cr(Ⅲ) recognition of tetraaryl imidazole derivatives bearing thiazole group

Three tetraaryl imidazole derivatives 5a-5c bearing thiazole groups were synthesized in the presence of [Bmin]Br by one-pot reaction and their structures were fully characterized by the 1H NMR, IR, MS and elemental analysis. The results of UV-vis spectra and fluorescent spectra upon metal ions complexation show that compound 5a displays high selectivity and sensitivity for Cr3+ ions. The complexation ratio of compound 5a and Cr3+ is 1:1.     

Synthesis of a β-cyclodextrin derivative bearing an azobenzene group on the secondary face

An oxidative coupling Sonogashira-type reaction has been used to synthesize a β-cyclodextrin derivative bearing an azobenzene group on the secondary face for the first time starting from a β-cyclodextrin propargylated at one of its C-2 positions. The de-O-propargylation reaction and the formation of an oxidative homocoupling dimer were found to compete with the desired product under several Sonogashira-type reaction conditions. However, the use of a diluted reductive atmosphere of H₂ avoided the former and diminished the latter.     

Synthesis, structure, and solution properties of [(mim-TASN)FeCl2]+ and its μ-oxo derivative

A series of iron(III) complexes based on the tetradentate ligand 4-((1-methyl-1H-imidazol-2-yl)methyl)-1-thia-4,7-diazacyclononane (L) has been synthesized, and their solution properties investigated. Addition of FeCl(3) to methanol solutions of L yields [LFeCl(2)]FeCl(4) as a dark red solid. X-ray crystallographic analysis reveals a pseudo-octahedral environment around iron(III) with the three nitrogen donors of L coordinated facially. Ion exchange reactions with NaPF(6) in methanol facilitate chloride exchange resulting in a different diastereomer for the [LFeCl(2)](+) cation. X-ray analysis of [LFeCl(2)]PF(6) finds meridional coordination of the three nitrogen donors of L. Electrochemical studies of [LFeCl(2)](+) in acetonitrile display a single Fe(III)/(II) reduction potential at -280 mV versus ferrocenium/ferrocene. In methanol, a broad cathodic wave is observed because of partial exchange of one chloride for methoxide with half-potentials of -170 mV and -440 mV for [LFeCl(2)](+/0) and [LFeCl(OCH(3))](+/0), respectively. The equilibrium constants for chloride exchange are 7 × 10(-4) M(-1) for Fe(III) and 2 × 10(-8) M(-1) for Fe(II). In aqueous solutions chloride exchange yields three accessible complexes as a function of pH. Strongly acidic conditions yield the aqua complex [LFeCl(OH(2))](2+) with a measured pK(a) of 3.8 ± 0.1. Under mildly acidic conditions, the μ-OH complex [(LFeCl)(2)(OH)](3+) with a pK(a) of 6.1 ± 0.3 is obtained. The μ-oxo complex [(LFeCl)(2)(O)](2+) is favored under basic conditions. The diiron Fe(III)/Fe(III) complexes [(LFeCl)(2)(OH)](3+) and [(LFeCl)(2)(O)](2+) can be reduced by one electron to the mixed valence Fe(III)/Fe(II) derivatives at -170 mV and -390 mV, respectively. From pH dependent voltammetric studies, the pK(a) of the mixed valent μ-OH complex [(LFeCl)(2)(OH)](2+) is calculated at 10.3.     

2-(2′-Pyridyl) benzimidazole complexes of dioxouranium(VI) and thorium(IV)

The bidentate ligand, 2-(2′-pyridyl) benzimidazole (PBH), forms a variety of complexes with dioxouranium(VI) and thorium(IV) of the type, UO₂(PBH)_xX₂ (n = 1, X = Cl, I, NO₃, 0.5SO₄; n = 2, X = NCS), UO₂(PBH)₃(ClO₄)₂, Th(PBH)₂X₄=Cl, NCS, NO₃) and Th(PBH)₄(ClO₄)₄. Microanalysis, electrical conductivity in various non-aqueous media, electronic and IR (down to 200 cm⁻¹) spectra, mass spectra and the TGA, DTA measurements on the complexes are reported.     

Synthesis and structures of 3-chloro-N′-(2-hydroxy-benzylidene)benzohydrazide and its oxovanadium(V) complex

A new Schiff-base 3-chloro-N ′ -(2-hydroxybenzylidene)benzohydrazide (H₂BBH) and its oxovanadium(V) complex [VO(BBH)(OCH₃)]₂ have been synthesized and characterized by elemental analysis, infrared (IR) spectra, and single-crystal X-ray determination. Both the ligand and the complex crystallized in the monoclinic space group P2₁ /c. The Schiff-base coordinates to V through the phenolate O, the imine N, and the enolic O. In the centrosymmetric dimeric oxovanadium(V) complex, the V atom is six-coordinate in an octahedral geometry. The bond lengths related to the donor atoms in the complex are different from those in the ligand. The coordination of the ligand to V is also supported by IR spectra.     

Synthesis, characterization and crystal structures of manganese (Ⅱ) complexes containing nitronyl nitroxide and its reduced derivative

Two novel adducts of formula Mn(hfac)2( NITPhCl )2 (1) and [Mn(hfac)2(IMHPhCl)]2(NIT-PhCl)·0.5H2O (2), where hfac = hexafluoroacetylacetonate, NITPhCl = 2-(3-chlorophenyl)-4,4,5,5-tetram-ethylimidazolyl-1-oxyl-3-oxide, IMHPhCl = 2-(3-chlorophenyl)-4, 4, 5, 5-tetramethylimidazolyl-3-oxide, have been prepared by the reaction of Mn(hfac)2·2H2O with NITPhCl. Compound 1 is triclinic, space group P-1with a = 1.3003(3) nm, 6 = 1.3138(3) nm,c = 1.4931 (3) nm, α = 83.74(3)°, β = 77.77(3)°, γ = 60.59(3)°, V=2.171(1)nm3, Z = 2. Compound 2 is triclinic, space group P-1 with a = 1.2994(3) nm, b = 1.4841(3) nm, c = 2.1031 (4) nm, a = 92.30(3)° ,p = 98.68(3)°, γ = 97.89(3)°, V= 3.964(2)nm3, Z = 2. Each manganese atom is hexacoordinated in both compounds and compound 2 is organized inchains by hydrogen bonds between neighboring pairs of NITPhCl and IMHPhCl.     

Proton-Template Synthesis of a П─Conjugated Macrocycle and Structure of its Ni_2(Ⅱ)—Complex

Robson-typemacrocycliccomplexesareplanarbinuclearcomplexesderivedfromSchiff'sbasecondensation0f2,6-diformyl-4-alkylphenolwithalkylenediamineinthepresenceofmetal;".Inthepastmorethan2Oyearsal0tofsuchcomplexesweresgnthesisedinthiswayandinvestigated':'>.Butthecomplexesofsuchamacrocyc1ewith1,2-phenylenediaminebridgewereneverrePOrteduntilveryrecentlyBrychcyetal.havegotsomeofthemalsobymetal-templatemethed`&,J.Sinceall-ring-systemoftheligandisconugated,itScomplexeshavemoreinterestfortheirexpectedun…     

Synthesis and Crystal Structure of catena-Poly[bis-(benzimidazole)cobalt(Ⅱ) μ- Phthalato]

The title polymeric complex [Co(C8H4O4)(C7H6N2)2]n has been prepared and its crystal structure was determined by X-ray diffraction method. The crystal belongs to monoclinic,space group C2/c with a = 7.7865(12), b = 20.4215(18), c = 13.4880(14) (A),β = 103.298(2)°, V = 2087.3(4) (A)3, Mr = 459.32, Z = 4, Dc= 1.462 g/cm3,μ = 0.859 mm-1, F(000) = 940, R = 0.0636 and wR = 0.1639 for 1278 observed reflections (I ＞ 2σ(Ⅰ)). The complex assumes a distorted tetrahedral coordination geometry, formed by two phthalate anions and two benzimidazoles (bzim). The phthalate anions bridge the neighboring Co(Ⅱ) atoms to form the polymeric chains. The centroid distance of 3.471(3) (A) between the parallel bzim rings of adjacent polymeric chains suggests the existence of π-π stacking.     

Synthesis and Structure of 〔Cu(Hcdta)〕(H_2O)

1mTRODUCTION.Theimportantprogressinmagnetostructuralchemistryinthepastfewyearsisthesystematicdevel0pmentofstructurallyorderedbimetalliccompound"'.Thefami-liesofcrystallineandam0rphouscomplexes[MM'(cdta)j.xH,O(M,M'maybethefirsttransitionmetalorthesecondmaingroupelements)haveprovidedniceex-amplesofstructuralversatilityinmagneticstudiest2-6i,wherequiteafewstructuresmentionedabove,includingbimetallicandhomometalliccompoundscomprisingcop-per0rothermetalatoms,havebeeninvestigated"-".Ontheother…