Gyula Pályi

Method for preparing glass capillary columns for gas chromatography

Abstract A method is given to prepare glass capillary columns with almost any stationary phase. The method is based on etching the soda-lime glass capillary tubing by dry gaseous hydrochloric acid. Coating the columns by the static method resultsin high-performance apolar and polar columns. The polar columns can be used even for the analysis of highly polar solutes. Studying the etched surface of soda-lime glass, the presence of a uniform layer of microcrystalline NaCl was found.

AsCo3(CO)9, its cyclic trimer, As3Co9(CO)24 and the phosphorus-containing analog P3Co9(CO)24☆

The AsCo3(CO)9 trigonal pyramidal cluster, its cyclic “trimer” As3Co9(CO)24 and the phosphorus-containing analog of the latter, P3Co9(CO)24 have been prepared and characterized. A reversible equilibrium between the arsenic-containing monomer and trimer was found to depend on p(CO). Such an equilibrium could not be observed in the case of P3Co9(CO)24.

Stable alkylcobalt carbonyls: [(alkoxycarbonyl)methyl]cobalt tetracarbonyl compounds ☆

Abstract Stable alkylcobalt carbonyls of the general formula ROOCCH 2 Co(CO) 3 L(R = alkyl, CH 2 Ph; L = CO, EPh 3 ; E = P, As, Sb) were prepared. The molecular structure of PhCH 2 OOCCH 2 Co(CO) 3 (PPh 3 ) was determined by X-ray diffraction.

Preparation and infrared spectra of monosubstituted PR3 and P(OR)3 (R alkyl, aryl) derivatives of (μ2-L)2Co2(CO)6 compounds☆

Abstract (μ 2 -L) 2 Co 2 (CO) 5 PR 3 and (μ 2 -L) 2 Co 2 (CO) 5 P(OR) 3 (R  alkyl, aryl, L 2  P 2 , As 2 , acetylene, L  CO and but-2-en-4-olid-4-ylidene) compounds were prepared. The ν(CO) infrared spectra are in agreement with the expected C s or C 1 symmetry. The results indicate that the PR 3 or P(OR) 3 substituent is in all cases in the axial position.

Transformations of the heteronuclear clusters En[Co(Co)3]4−n (E = P, As; n = 1–3) when treated with soft lewis acids and bases

Abstract The tetrahedral pnigogenic clusters E n [Co(CO) 3 ] 4 - n (EP, As; n = 1–3) react with soft Lewis acids and bases to give products of substitution and transformation of the cluster. Lewis acids promote transformations to clusters containing more cobalt atoms and Lewis basis to clusters containing fewer such atoms.

On the reactivity of μ2-acetylenes coordinated to cobalt : Stereochemistry of the formation of the butene-2-olide-4 complexes: Co2(CO)7(RR′C4O2)

Abstract The relative positions of the R and R′ substituents in the “lactone” complexes, Co2(CO)7(RR′C4O2) (μ2-carbonyl-μ2-spiro-[2,3-substituted-2-butene-4- olide-4-ylidene]-bis[tricarbonylcobalt][CoCo] derivatives) was studied spectroscopically. It was found that the formation of these complexes is stereoselective and is controlled by the bulk of the substituents R and R′.

Phosphido cobalt carbonyl cluster: Co2(CO)6P2 and Co3(CO)9 PS

Abstract Two phosphido cobalt carbonyl cluster Co(CO)6P2 and Co3(CO)9PS have been prepared and characterised.

Reaction of coordinated diphosphorous with metal carbonyl fragments. Crystal structure of [(CO)5Cr][(CO)5W]P2Co2(CO)6

Abstract Either one or two of the metal carbonyl fragments Cr(CO)5, Mo(CO)5, W(CO)5 or Fe(CO)4 can become linked to the coordinated diphosphorous molecule of (μ2-P2)Co2(CO)5L (L = CO, PBu3, PPh3) when the latter species is treated with THF adducts of these fragments. The structure of [(CO)5Cr][(CO)5W]P2Co2(CO)6 has been determined by X-ray diffraction.

Methylidinetricobalt nonacarbonyl compounds : III. Evidence for CoCO(organic) interaction in Co3(CO)9CCHCRCOOR′ (R = H, alkyl, Ph; R′ = H, Me) derivatives

Abstract IR evidence was found for interaction between two cobalt atoms of the cluster and the carboxylic or ester carbonyl in Co 3 (CO) 9 CCHCRCOOR′ (R = H, alkyl, Ph; R′ = H, Me) compounds. The results afford independent proof for assignment of the v (CO) bands of Co 3 (CO) 9 CY complexes according to the selection rules of the C 3 v point group.

μ,μ,-bis(alcoholato)- and μ,μ-bis(phenolato)dirhodium(I) tetracarbonyl complexes

Abstract Rh2(CO)4(OR)2 complexes (R = Me, Et, Pr, i-pent, Ph, p-chlorophenyl) were prepared from Rh2(CO)4Cl2 and sodium alcoholates or phenolates. They are converted by phosphines into the monomeric Rh(CO)(PR′3)2(OR) derivatives (R′ = Bu, Ph) via Rh2(CO)3(PR′3)(OR)2 intermediates.