Synthesis and structure characterization of a novel series of N-alkylphthalimidylaminocarbonylmethoxylcalix [4] arenes

A novel series of N-alkylphthalimidylaminocarbonylmethoxylcalix[4]arenes with the reaction between 4-(N-bromoacetyla- mino)-phthalimide derivatives and calix[4]arene has been synthesized and structurally characterized by IR,~1HNMR and MS.From their analysis data,it was found that compounds 7a-7d adopted a cone conformation.     

Synthesis and characterization of a novel series of pyrimidinylthiaalkoxycalix[4]arenes

A novel series of pyrimidinylthiaalkoxycalix[4]arenes with the reaction between 4,6-dimethylpyrimidine-2-thiol and thedifferent dibromides calix[4]aryl groups have been synthesized and structurally characterized by IR,1H NMR and MS.From theiranalysis data,it was found that compounds 8,9,11 adopted a cone conformation,while compound 10 existed as a mixture ofconformations.     

Synthesis,crystal structures and magnetic properties of a series of new cyano-bridged complexes derived from templates [Ni(CN)4]2− and [Co(III)(CN)6]3−

Three new cyano-bridged complexes 1 [Ni(tn)₂Ni(CN)₄] (tn?=?1,3-diaminopropane), 2 [Cu^II(dipn)Ni^II(CN)₄], and 3 [Cu(dipn)]₆[Co(CN)₆]₄?·?4H₂O (dipn?=?dipropylenetriamine) have been assembled by the templates [Ni(CN)₄]^2? and [Co(CN)₆]^3?. 1 consists of a one-dimensional linear chain–Ni(tn)₂–NC–Ni(CN)₂–CN–Ni(tn)_2? in which the Ni(II) centers are linked by two CN groups. One 1-D zigzag chain of 2 is formed with–Ni(2)–C–N–Cu(1)–N–C–linkages. A 2D structure of 3 is formed by an alternate array of [Co(CN)₆]^3? and [Co][Cu₆] units. For 1, there is an overall weak antiferromagnetic interaction between Ni(II) ions through the–NC–Ni–CN–bridges of the diamagnetic [Ni(CN)₄]^2? anions. 2 exhibits a weak antiferromagnetic exchange interaction between copper(II) ions mediated by [Ni(CN)₄]^2? diamagnetic bridges. Complex 3 exhibits a weak ferromagnetic interaction between nearest Cu^II and Cu^II atoms through–NC–Co–CN–bridges.     

Subtle difference of [SiMo12O40]4− and [PMo12O40]3− inducing two new distinct Keggin-Ag-(1H-Pyrazole) compounds

Two new inorganic-organic hybrid compounds based on α-Keggin clusters and Ag-(1H-Pyrazole) subunits, [AgL₂]₄[SiMo₁₂O₄₀] (1) and [AgL₂]₃[PMo₁₂O₄₀] (2) (L = pyrazole), have been synthesized under hydrothermal conditions and characterized by single crystal X-ray diffraction. In 1, there are two kinds of chains, the chains linked by two [AgL₂]⁺ clusters and the other linked only by one [AgL₂]⁺, which further connect by sharing [SiMo₁₂O₄₀]^4? anions to construct a 2-D layer. In 2, four-supporting [PMo₁₂O₄₀]^3? anions are fused by [Ag(1)L₂]⁺ subunits to form a 1-D chain. Through weak interactions of Ag?O (3.091 Å) a 2-D supramolecular layer is constructed. Additionally, the electrochemical properties of title compounds and the photocatalytic properties of 2 have been studied.     

Synthesis and characterization of a series of chiral NHC–Pd complexes derived from l-phenylalanine

The synthesis of a series of chiral Pd(L)PyBr₂ (3a–3e) and Pd(L)PyCl₂ (4d and 4e) complexes from l-phenylalanine is presented (L = (S)-3-allyl-4-benzyl-1-(2,6-diisopropylphenyl)-imidazolin-2-ylidene (a), (S)-4-benzyl-1-(2,6-diisopropylphenyl)-3-(naphthalen-2-ylmethyl)imidazolin-2-ylidene (b), (S)-4-benzyl-3-(biphenyl-4-ylmethyl)-1-(2,6-diisopropylphenyl)imidazolin-2-ylidene (c), (S)-4-benzyl-1-(2,6-diisopropylphenyl)-3-(naphthalen-1-ylmethyl)imidazolin-2-ylidene (d) or (S)-4-benzyl-1-(2,6-diisopropylphenyl)-3-(2,4,6-trimethylbenzyl)imidazolin-2-ylidene (e). The complexes were characterized by physicochemical and spectroscopic methods, and the X-ray crystal structures of 3a–3c and 4d are reported. In each case, there is a slightly distorted square-planar geometry around palladium, which is surrounded by imidazolylidene, two trans halide ligands and a pyridine ligand. There are π–π stacking interactions in the crystal structures of these complexes. Complex 3a showed good catalytic activity in the Cu-free Sonogashira coupling reaction under aerobic conditions.     

Synthesis,crystal structure and luminescent properties of two complexes containing [Au(CN)2] − building blocks

Two supramolecular complexes, {{Ni(H₂O)(phen)₂[Au(CN)₂]}[Au(CN)₂]?·?1.5H₂O} _n (1) (phen?=?1,10-phenanthroline) and [H₂teta][Au₂(CN)₄]?·?2H₂O (2) (teta?=?5,7,7,12,14,14-hexamethyl-1,4,8,11-tetra-azacyocloteradeca-4,11-diene) have been synthesized and structurally characterized. Complex 1 was a one-dimensional infinite chain constructed by [Au(CN)₂]^? building blocks. In complex 2, there are one cation, one anion, and two water molecules in the asymmetric unit. The two complexes are interconnected through a combination of aurophilic attractions and hydrogen bonds and formed into 3D supramolecular structures. The aqueous solutions of 1 and 2 display interesting luminescence at room temperature.     

Synthesis,crystal structure,and magnetic properties of a salt containing [Cu2Cl7]3− and 4-nitrobenzyl-4′-dimethylaminopyridinium

A new salt, [NO₂BzDMAP]₃[Cu₂Cl₇]?·?H₂O (1), has been synthesized, where [NO₂BzDMAP]⁺ is 1-(4′-nitrobenzyl)-4-dimethylaminopyridinium. Herein, the synthesis, spectral and structural characterization, and magnetic behavior of 1 are reported. It is orthorhombic, with space group Pca2₁, and a?=?26.639(2)?Å, b?=?9.638(1)?Å, and c?=?20.011(2)?Å with V?=?5137.5(7)?ų for Z?=?4. The anion shows a chloride-bridged binuclear structure with Cu?···?Cu distance of 3.872?Å; the two Cu(II) ions have a tetrahedral geometry. The cations stack through p?···?π and π?···?π interactions, and a complicated hydrogen-bonding network structure is formed through C–H?···?Cl and C–H?···?O hydrogen bonds. The variable temperature magnetic susceptibility measurements reveal that 1 exhibits strong antiferromagnetic interaction with J?=??193.0?cm^?1.     

Synthesis and characterization of novel chalcogen and pnictogen coordinated Bi(III) complexes—the first Se,Se′ coordinated Bi metallacycle

Inorganic and organometallic Bi(III) complexes with five-membered heterocycles were studied. The preparation, properties, and spectroscopic characterization (¹H NMR, IR, MS-fragmentation behaviour) of the new compounds are reported. The first member of Se coordinated Bi metallacycles is presented. Bi organyles with the o-aminobenzenethiol ligand system, at present widely investigated, are described as o-aminobenzenethiolate and o-aminobenzenethioldiate derivatives.     

Synthesis and Crystal Structure of the Polyoxometalatebased Complex [Mn（DMSO）5H2O]2SiMo12O40

1 INTRODUCTION The design and assembly of organic-inorganic solid-state materials with active physical properties, such as materials with electrical, magnetic and opti- cal properties, has become a focus of a great deal of interest in recent years[1, 2].…     

A series of new organic–inorganic compounds templated by the [SiW12O40]4− polyanion

Two couples of new compounds templated by the polyanion [SiW₁₂O₄₀]^4?,[Hbix][Cu^I(bix)]₃[SiW₁₂O₄₀]·4H₂O (1) and [Cu^II(H₂O)(Hbix)₂(bix)]₂[Cu^II(H₂O)₂(Hbix)₂(bix)][SiW₁₂O₄₀]₃·4H₂O (2) (bix = 1,4-Bis(imidazol-1-ylmethyl)benzene), [Cu^I(bbi)]₄[SiW₁₂O₄₀]·2H₂O (3) and [Cu^II(bbi₂)]₂[SiW₁₂O₄₀] (4) (bbi = 1,1′-(1,4-butanediyl)bis(imidazole)) were hydrothermally synthesized, and characterized by elemental analyses, IR spectroscopy, thermogravimetric analyses and single X-ray diffraction. Compounds 1 and 2 were synthesized from the same reactants but exhibited distinct structures which could be ascribed to the different ratios of the reactant bix to Cu^II. In compound 1, the higher ratio of bix results in the transformation of the Cu^II to Cu^I, the [SiW₁₂O₄₀]^4? templates direct the Cu^I–bix coordination polymers to form a 3D supramolecular framework with grid-like channels along two directions. The [SiW₁₂O₄₀]^4? templates in compound 2 locate in the voids of the 3D supramolecular network constructed by Cu^II–bix coordination polymers, which exhibits the interdigitation fashion in both the formation of the 2D layer and the 3D framework. Compounds 3 and 4 were synthesized similar to 1 and 2, except for the change of bix to bbi. In compound 3, the Cu^I–bbi polymers form a supramolecular metal–organic host framework with rhombic channels in which the SiW₁₂ templates reside. Compound 4 shows a framework with hexagonal channels constructed by Cu^II–bbi coordination polymers which accommodated the SiW₁₂ templates.     

Hydrothermal syntheses, crystal structures and properties of 0-D, 1-D and 2-D organic-inorganic hybrid borotungstates constructed from Keggin-type heteropolyanion [α-BW12O40] and transition-metal complexes

Three novel organic-inorganic hybrid borotungstates {[Ni(phen)₂(H₂O)]₂H(α-BW₁₂O₄₀)}·4H₂O (1), [Cu^I(2,2'-bipy)(4,4′-bipy)_0.5]₂{[Cu^I(2,2′-bipy)]₂Cu^I(4,4′-bipy)₂(α-BW₁₂O₄₀)} (2) and {[Cu^I(4,4′-bipy)]₃H₂(α-BW₁₂O₄₀)}·3.5H₂O (3) (phen=1,10-phenanthroline, 2,2′-bipy=2,2′-bipyridine, 4,4′-bipy=4,4′-bipyridine) have been hydrothermally synthesized and structurally characterized by elemental analyses, IR, UV spectra, powder X-ray diffraction (PXRD), thermogravimetric analysis (TGA), single-crystal X-ray diffraction, X-ray photoelectron spectroscopy (XPS) and photoluminescence. The structural analysis reveals that 1 consists of a 0-D bisupporting polyoxometalate cluster where two [Ni(phen)₂(H₂O)]²⁺ cations are grafted on the polyoxoanion [α-BW₁₂O₄₀]^5- through two terminal oxygen atoms, 2 shows a 1-D infinite chain constructed from [α-BW₁₂O₄₀]^5- polyoxoanions and {[Cu^I(2,2′-bipy)]₂Cu^I(4,4′-bipy)₂}³⁺ cations by means of alternating fashion, and 3 displays an unprecedented 2D extended structure built by [α-BW₁₂O₄₀]^5- polyoxoanions and -Cu^I-4,4′-bipy- linear chains, in which each [α-BW₁₂O₄₀]^5- polyoxoanion acts as a tetradentate inorganic ligand and provides three terminal oxygen atom and one two-bridging oxygen atom. The presence of Ni^II and W^VI in 1, Cu^I ions and W^VI in 2 and 3 are identified by XPS spectra. The photoluminescence of 2 and 3 are also investigated.     

Synthesis, crystal structure, and thermal analysis of hexahydrogen dodecavanadate of composition [NH3 · H2O]6 · H6[Ca4V12O40] · 6H2O

Dihydrogen dodecavanadate of composition [NH₃ · H₂O]₆ · H₆[Ca₄V₁₂O₄₀] · 6H₂O was synthe-sized and studied by X-ray crystallography and TGA analyses. The crystals are cubic, space group I $\bar 4$ 3m;; unit cell parameters: a = 13.518(2) ?, V = 2470.4(3) ?³, ??_calc = 2.2334 g/cm³, Z = 2.     

Synthesis,spectral characterization and antibacterial activity of O,O’-dialkyl and alkylene dithiophosphatogold (III)dichloride; crystal structure of [S2POCMe2CMe2O]AuCl2

Abstract

O, O’-Dialkyl and alkylene dithiophosphatogold (III)dichloride complexes of the type [(RO)₂PS₂]AuCl₂ and [S₂POGO]AuCl₂, where R?=?Et, nPr, iPr, iBu, Ph, cyclohexyl and cyclopentyl, where G?=?CMe₂CMe₂-, have been synthesized in 80-90% yields by reaction of the corresponding acid or sodium salts of the appropriate dithiophosphoric acids in 1:1 ratio with gold (III) chloride in dry dichloromethane at room temperature. The compounds have been characterized by elemental analyses, IR and (¹H, ^l3C, and ³¹P) NMR. The crystal structure of [S₂POCMe₂CMe₂O]AuCl₂, was determined. These new complexes have shown their growth inhibiting potential against various bacterial strains with moderate to good activity.     

Preparation, characterization and crystal structure of Na4[Mn(NCS)6]·13H2O

Na₄[Mn(NCS)₆] · 13H₂O was prepared and characterized by chemical analysis, magnetic susceptibility, thermal dehydration reactions, and single crystal X-ray structure analysis. The crystals are triclinic with a=9.310(1)Å, b=9.367(1)Å, c=9.730(2)Å, = 89.89(1)°,=75.33(1)°, =70.72(1)°, space group P¯I.Z=1. The structure is built up from Na(H₂O)₅ S, Na(H₂O)₆, and Mn(NCS)₆, octahedra. All water molecules are coordinated to Na⁺ -ions in terminal as well as bridging fashion. They form O-H···O as well as O-H···S hydrogen bonds.Dedicated to Professor Dr. rer. nat. Dr. h.c. Hubertus Nickel on the occasion of his 65th birthday     

Synthesis,characterization and properties of the α-K7[GaW11Ti(O2)O39]·11H2O heteropolyanion

The peroxotitanium-substituted heteropolytungstate -K₇[GaW₁₁Ti(O₂)O₃₉]·11H₂O has been prepared and characterized by elemental analysis, i.r., u.v., ¹⁸³W-n.m.r. and by electrochemistry. The ¹⁸³W-n.m.r. spectrum consists of six lines with intensity ratio 2:2:1:2:2:2, indicating that the TiO₂ occupies the empty octahedral site of the -K₉[GaW₁₁O₃₉]·xH₂O anion forming a polyanion with C _s symmetry. The characteristic charge-transfer absorption band O^2– ₂ Ti at 385 nm occurs in the u.v. spectrum. The polargraphic reduction potential of O^2– ₂ at ca. + 0.95 V has been determined.     

Synthesis, structure and characterization of binuclear copper(Ⅱ) complexes

At room temperature, dibenzoyl peroxide undergoes oxidative addition reaction with metallic copper powder and pyridine N-oxide (triphenylphosphine oxide or 2,9-dimethyl-4,7-diphenyl-1,10-phenanthrolin) which affords the last products as binuclear copper(II) complexes, [Cu(C5H5NO)-(C6H5COO)2]2(1), [Cu(OPPh3)(C6H5COO)2]2(2) and [Cu(C6H5COO)(C26H2oN2)](3, C26H2oN2 is 2,9-dimethyl-4,7-diphenyl-1,10-phenanthrolin). The structure of the complexes were characterized by elemental analyses, IR spectra, TG-DTA and magnetic property. Crystals(1) are triclinic, space group P1,a=0.92617(36),b=1.06973(17), c=1.08813(29) nm, a=59.60(2)°, β=74.83(3)°,γ=72.80(2)°, V=0.880 nm3, Dc=1.520 g/cm3, Z=1, R=0.044, Rw=0.048, Mr=805.78, 3477 reflections with I > 3σ(I). Each copper(Ⅱ) ion is coordinated by two bridging bidentate benzoate ligands and one pyridine N-oxide or triphenylphosphine oxide to form dimeric binuclear molecules. The structure of the compound(1) shows a clear centre of symmetry.     

Synthesis and structure characterization of novel calix[4]（aza）crown derivatives

Three novel calix[4](aza)crown deravatives have been synthesized,including a new [2]pseudorotaxane in which calix[4]- azacrown behaves as a stopper,a novel‘tren’type calix[4]azacrown and a novel‘spiro’type calix[4]azacrown containing morpholine unit.The structures of these compounds have been confirmed by NMR and MS.     

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.     

Synthesis and structure of osmium complexes [Ph3PR]2[OsCl6]·4DMSO

Russian Journal of General Chemistry - Reaction of sodium hexachloroosmate(IV) dihydrate with (2-oxopropyl)- and (2-carboxyethyl)-triphenylphosphonium chlorides in dimethyl sulfoxide afforded...