Spectroscopic Properties of New Indium(III) Phthalocyanine Complexes
Preparation, Crystal Structure and Properties of (Ph4P)2ReCl6.2CH3CN
Małecka J., Jaeger L., Wagner Ch. and Mroziński J.
Interactions between the Components in the Zr-Ag-In System at 870 K
Gulay L.D., Zaremba V.I., Stępień-Damm J. and Kalychak Ya.M.
Synthesis, Spectral, Magnetic and X-ray Powder Diffraction Structural Characterization of [Fe(NCS)3(OPPh3)3]
Ondrejkovicova I., Jorik V. and Mroziński J.
Uptake of Molecular Oxygen by Co(II) Chelates with Peptides in Aqueous Solution. Part X. Diastereoisomeric Dipeptides as Auxiliary Ligands in Oxygen-Free Complexes
Kufelnicki A. and Świątek M.
New Insertion Reactions of Some Carbenoids into Amide- and Sulfonamide-NH Bonds
Mlostoń G., Celeda M., Świątek A., Kaegi M. and Heimgartner H.
Flash Vacuum Pyrolysis of 1,3-Thiazole-5(4H)-thiones
Leśniak S., Mlostoń G. and Heimgartner H.
Reaction of Cyclic Allylic Acetates with Aliphatic Alcohols in the Presence of Cerium(III) Chloride
Uzarewicz A. and Dresler R.
2,2'-Diselenobisbenzoates and 2,2'-Diselenobisbenzenesulfonates: New Chiral Aryl Dis-elenides
Palus J., Młochowski J. and Juchniewicz L.
The Reaction of (Methylthio)acetyliron Complex with Pentose Terminal Aldehydes
Wiśniewski K. and Zamojski A.
Studies on Mechanism of 2-Pyridinecarboxaldehyde Oxidation by Dichromates in Strongly Acidic Aqueous Solutions. The Unusual Reaction Order on Concentration of the Aldehyde
Kita E., Kita P. and Uścińska G.
Interaction of Thymidylate Synthase with 5-Fluoro-Substituted DUMP Analogues in View of the Pyrimidine Ring Structure
Jarmuła A., Cyrański M.K., Leś A., Krygowski T.M. and Rode W.
Calixresorcinarenes as Dynamic Coatings for Modified Stationary RP-18 Phase for HPLC
Pietraszkiewicz M., Pietraszkiewicz O. and Kobiał M.
The Analysis of Resistance Change in Diffusion Controlled Electrode Processes
Gatner K. and Zięba A.
Solubility of n-Alkanes in Ethyl tert-Butyl Ether
Domańska U. and Venkatesu P.
CRYSTAL AND MOLECULAR STRUCTURE
The Crystal Structure of Strontium Complex with 3-Aminopyrazine-2-carboxylic Acid
Leciejewicz J., Ptasiewicz-Bąk H. and Zachara J.
X-ray Structural Investigations of Three 4-Aryl-Substituted [2.2]Paracyclophanes
Jones P.G. and Kuś P.
Crystal Structure of 2-(1,4,5,6-Tetrahydropyrimidin-2-yl)phthalazinone-1 Hydroiodide
Główka M.L., Książek W., Staszewska A., Kozłowska K., Ołubek Z. and Krężel I.
Monomeric Molecules in the Isostructural Calcium(II) and Strontium(II) Complexes with Pyrazine-2-carboxylic Acid
Ptasiewicz-Bąk H., Ostrowski A. and Leciejewicz J.
A Microcalorimetry and Spectroscopy Study on the Interaction of Catalase with Cyanide Ion
Ghadermarzi M., Saboury A.A. and Moosavi-Movahedi A.A.
Stretching the Limits: According to High-Level Ab Initio Calculations C-O Bonds Are Longer than the
Central C-C One in Hypothetical 2-Oxabicyclobutane
Dodziuk H. and Leszczyński J.
New Complex Compounds of Cu(I), Zn(II), Cd(II) and Hg(II) with 3-(2'-Thiothenoyl-amino)dibenzofuran
Muresan V., Reiss A., Sbirna L.S., Muresan N. and Florea S.
Spectroscopic Properties of New Indium(III)
by J. Janczak
(Received February 19th, 1998)
New blue-violet diamagnetic diindium(III) triphthalocyanine and paramagnetic indium(III) diphthalocyanine complexes have been obtained in crystalline form. The UV- -VIS, IR and far IR spectra of the In2Pc3 and InPc2 complexes are presented here for the first time. The spectroscopic data of the both In(III) complexes are discussed in terms of characteristic group frequencies and compared with other phthalocyanines. An empirical vibrational assignment of the observed fundamentals are given. The absorption electronic spectra indicate the proximity of the HOMO and LUMO of the Pc ligand in energy.
Preparation, Crystal Structure and Properties
by J. Małecka1, L. Jaeger2, Ch. Wagner2 and J. Mroziński1
(Received March 27th, 1998)
(Ph4P)2ReCl6.2CH3CN 1 crystallizes as colourless single crystals from the acetonitrile solution of (Ph4P)2ReCl6 in ether. The crystals are monoclinic in space group P21/c with unit cell constants of a = 9.5507(12) ; b = 19.724(3) ; c = 15.033(2) ; = = 90o; ß = 8.451(14)o; V = 2801.1(7) 3; Z = 2. In the octahedral anion the Re-Cl bond lengths are 2.368 in average. The FIR region indicates two deformation bands (Cl-Re-Cl) at 162 cm-1 (F2g) and 175 cm-1 (F1u) and stretching band niu(Re-Cl) at 309 cm-1 (F1u). For 1 very weak antiferromagnetic super-exchange is observed; the effective magnetic moment at room temperature is 3.57 B.M.
Interactions between the Components
by L.D. Gulay1, V.I. Zaremba1, J. Stępień-Damm2
and Ya.M. Kalychak1
(Received February 18th, 1998; revised manuscript April 8th, 1998)
The interactions between the components in the ternary Zr-Ag-In system were studied. An isothermal section at 870 K was established by X-ray analysis. Two unknown ternary compounds have been found: ZrAg0.4In2.6-AuCu3 structure type (space group Pm3m, a = 4.3644(4) ) and Zr5AgIn3-Hf5CuSn3 structure type (space group P63/mcm, a = 8.735(3) , c = 5.948(2) ). Their crystal structures were determined by powder X-ray analysis.
Synthesis, Spectral, Magnetic and X-ray
by I. Ondrejkovicova1, V. Jorik1
and J. Mroziński2
(Received March 3rd, 1998; revised manuscript April 10th, 1998)
The autocatalytic oxidation of PPh3 with dioxygen in the systems containing some iron compound and NCS- anions in acetonitrile leads to the formation of the complex [Fe(NCS)3(OPPh3)3], where OPPh3 is triphenylphosphine oxide. The complex is also formed by direct interaction of Fe(NCS)3 with OPPh3. This high-spin iron(III) complex acts as an oxidation catalyst of PPh3. On the basis of elemental analysis, spectral data and X-ray powder diffraction have been proved that the samples of the complex have not only the same composition but possess the same crystal structure irrespective of the preparation method.
Uptake of Molecular Oxygen by Co(II)
by A. Kufelnicki and M. Świątek
(Received January 26th, 1998; revised manuscript April 20th, 1998)
Co(II) complexes with a group of diastereoisomeric dipeptides consisting of alanine and leucine in various chiral forms have been studied in aqueous solution. The equilibria were determined by potentiometric and spectrophotometric methods, using least-squares fitting procedures. The results were compared with those for glycine dipeptides containing only one asymmetric atom.
New Insertion Reactions of Some Carbenoids
by G. Mlostoń1, M. Celeda1, A. Świątek1,
M. Kaegi2 and H. Heimgartner2
(Received February 27th, 1998)
In the presence of catalytic amounts of Rh2(OAc)4 in toluene, dimethyl diazomalonate (1) decomposed with evolution of N2 to form a carbenoid of type 8 which reacted with carboxamides 2 and toluenesulfonamide (4) to give 2-(acylamino)- and 2-(sulfonylamino)malonates 3 and 5, respectively. In an analogous reaction, -diazo ketone 6 and 4 yielded N-(2-oxo-1,2-diphenylethyl)toluenesulfonamide (7).
Flash Vacuum Pyrolysis of 1,3-Thiazole-5(4H)-thiones
by S. Leśniak1, G. Mlostoń1 and H.
(Received March 16th, 1998)
Flash vacuum pyrolysis of 2-phenyl-1,3-oxazol-5(4H)-one (5) at 600oC/1.5.10-3 Torr proceeded via CO2-elimination to give 3-phenyl-2H-azirine (6) as the only detectable product which was isolated in 34% yield. Under similar conditions, 4,4-dimethyl-1,3- thiazole-5(4H)-thiones 7a and 7b yielded isomeric 1,4,2-dithiazole derivatives 8a,b as main products. Desulfurization leads to 2-(2-propylidene)-1,3-thiazetes 9 as minor products, and in the case of 7a, disulfide 10a is formed as a second minor product.
Reaction of Cyclic Allylic Acetates with Aliphatic
by A. Uzarewicz and R. Dresler
(Received February 5th, 1998; revised manuscript March 30th, 1998)
The reactions of selected allylic acetates with methanol, ethanol, n-propyl alcohol, isopropyl alcohol and tert-butyl alcohol in the presence of catalytic amounts of cerium(III) chloride are described. Allylic alkyl ethers, bis-allylic ethers and 1,3-dienes were obtained depending on the structure of the acetates.
by J. Palus, J. Młochowski and L. Juchniewicz
(Received March 13th, 1998; revised manuscript April 2nd, 1988)
The synthesis of chiral 2,2'-diselenobisbenzoates (3) from 2-aminobenzoic acid and chiral alcohols was elaborated. Similar method was applied for the preparation of chiral 2,2'-diselenobisbenzenesulfonates (4) from 2-aminobenzenesulfonic acid. Ester 3a was an efficient catalyst for chemoselective hydrogen peroxide oxidation of sulfides into sulfoxides but no stereoselectivity of the reaction was observed.
The Reaction of (Methylthio)acetyliron Complex
by K. Wiśniewski and A. Zamojski
(Received April 2nd, 1998)
The reaction between anion generated from (methylthio)acetyliron complex (1) and four stereoisomeric dialdo-1,4-furanoses was performed. Each aldehyde led to mixtures (6-8) of stereoisomeric aldols. Aldols were separated and their configuration was determined. Decomplexation of these products was studied with oxidative (NCS, Cl2, I2, CuCl2) and reducing (BH3.Me2S and NaBH4) reagents. Sugar derivatives were isolated and their structures were deduced.
Studies on Mechanism of 2-Pyridinecarboxaldehyde
by E. Kita, P. Kita and G. Uścińska
(Received January 21st, 1998, revised manuscript March 2nd, 1998)
2-Pyridinecarboxaldehyde (pyad) has been oxidized by Cr2O72- ion at pH range 0-1 to 2-pyridinecarboxylic acid (pyac). The produced Cr(III) exists in the form of three complex ions: [Cr(pyac)(H2O)4]2+, [Cr(pyac)2(H2O)2]+ and [Cr(H2O)6]3+. The reaction follows unusual mixed fourth-order rate law: first-order on concentrations of Haq+ and Cr(VI) and second-order on concentration of the aldehyde. Mechanism of the reaction has been discussed.
Interaction of Thymidylate Synthase with
by A. Jarmuła1, M.K. Cyrański2, A.
Leś2, T.M. Krygowski2 and W. Rode1
(Received February 19th, 1998; revised manuscript March 26th, 1998)
To explain the mechanism of the influence of fluorine substituent on the FdUMP activity in thymidylate synthase reaction, the aromaticity based on X-ray determined structures, factor analysis applied to structural data from CSD and ab initio RHF calculations were employed. It was found that fluorine substitution dearomatizes the pyrimidine ring, stabilizing the local double C(5)=C(6) bond and making them more susceptible to nucleophilic addition from the thymidylate synthase side. The effect of local strain occurs in the ipso region in relation to the substituent. The effect is rather asymmetrical: the C(5)=C(6) bond is more strongly affected by the substituent than the C(4)-C(5) bond. This suggests a possibility of a further affinity increase of FdUMP system regarding the enzyme.
Calixresorcinarenes as Dynamic Coatings for
by M. Pietraszkiewicz, O. Pietraszkiewicz and M. Kobiał
(Received January 19th, 1998; revised manuscript April 6th, 1998)
Lipophilic calixresorcinarenes, derived from lauryl aldehyde and resorcinol, are strongly adsorbed on the modified silica gel RP-18 during HPLC. This technique leads to the column with an excellent time stability and good reproducibility at the retention characteristics of substituted phenols as analytes.
The Analysis of Resistance Change
by K. Gatner and A. Zięba
(Received August 18th, 1997; revised manuscript April 8th, 1998)
The resistance changes in diffusion limited electrode processes are given and compared with experimentally determined by high frequency resistometry (HFR) combined with potentiostatic, galvanostatic and cyclic voltammetry methods. The general shape of resistance-time dependence is similar to current time transients in potentiostatic and potential time transients in galvanostatic experiments. The resistance-potential depen-dence in cyclic resistometry exhibits a sigmoidal shape, similar to the convolutive CV current function. The greatest change of the electrolyte resistance takes place near the electrode surface. High frequency resistometry provides independent parameters to those obtained from other electrochemical methods.
Solubility of n-Alkanes in Ethyl tert-Butyl Ether
by U. Domańska and P. Venkatesu
(Received February 4th, 1998; revised manuscript April 9th, 1998)
The solid-liquid equilibrium (SLE), of 11 binary
mixtures of n-alkanes (octadecane, nonadecane, eicosane, heneicosane,
docosane, tricosane, tetracosane, pentacosane, hexa-
The Crystal Structure of Strontium Complex
by J. Leciejewicz1, H. Ptasiewicz-Bąk1
and J. Zachara2
(Received February 10th, 1998; revised manuscript March 6th, 1998)
In the crystals of trans-diaquobis(mu-3-aminopyrazine-2-carboxylato-N,O,O,O)strontium(II) the Sr ion is eightfold coordinated: by two aminopyrazinate (APZA) ligands via their (N,O) bonding moieties [Sr-O 2.5189(15) , Sr-N 2.7280(18) ], two other carboxylate oxygen atoms donated by the adjacent APZA molecules [Sr-O 2.5989(16) ] bridging the Sr(APZA)2 units into molecular ribbons and two water molecules [Sr-O 2.5556(18) ]. The ribbons are interconnected by hydrogen bonds involving the water molecules and the carboxylate oxygens [O-H...O 2.71(1) ], as well as the amino group nitrogen atoms and the heteroring nitrogen atoms [N-H...N 3.08(1) ].
X-ray Structural Investigation
by P.G. Jones1 and P. Kuś2
(Received March 16th, 1998)
The low-temperature crystal structures of 4-methylphenyl[2.2]paracyclophane (1), C23H22, orthorhombic, Pbca, a = 12.880(2), b = 7.4234(12), c = 34.425(6) , Z = 8; 2,6-dimethylphenyl[2.2]-paracyclophane (2), C24H24, orthorhombic, P212121, a = 8.593(3), b = 12.550(4), c = 15.745(4) , Z = 4, and 2,4,5-trimethylphenyl[2.2]paracyclophane (3), C25H26, monoclinic, P21/c, a = 13.737(2), b = 17.883(2), c = 15.230(2) , ß = 103.423(8), Z = 8 (two independent molecules) have been determined. Surprisingly, only small differences from the normal paracyclophane structure were found in the three sterically hindered species; the paracyclophane rings are mutually rotated and twisted by a few degrees, and the torsion angle between paracyclophane and aryl rings is slightly increased in 2 and 3 compared to 1.
Crystal Structure of
by M.L. Główka1, W. Książek1,
(Received February 26th, 1998; revised manuscript March 23rd, 1998)
X-ray crystal study of the 2-(1,4,5,6-tetrahydropyrimidin-2-yl)phthalazinone-1
hydroiodide showed different hydrogen bonding network and packing
than those observed in the crystals of two other phthalazinones-1,
comprising either smaller (4,5-dihydro-
Monomeric Molecules in the Isostructural
by H. Ptasiewicz-Bąk1, A. Ostrowski2
and J. Leciejewicz1
(Received October 15th, 1997; revised manuscript April 7th, 1998)
The crystals of cis-tetraquobis(pyrazine-2-carboxylato-O,N)calcium(II) contain monomeric molecules, in which the calcium ion has a distorted dodecahedral coordination, formed by four water molecules (mean Ca-O = 2.441 , two oxygen atoms from monodentate carboxylic groups of two pyrazinic acid molecules (mean Ca-O = 2.458 ) and two nitrogen atoms located next to the above carboxylic groups (mean Ca-N = 2.619 ). In the crystals of cis-tetraquobis(pyrazine-2-carboxylato-O,N)strontium(II) the coordination of the Sr2+ ion is identical with that of the calcium complex, the corresponding mean distances being Sr-O(water) 2.572 , Sr-O 2.588 , Sr-N 2.751 . The monomeric molecules of both compounds are linked via a network of hydrogen bonds.
A Microcalorimetry and Spectroscopy Study
by M. Ghadermarzi, A.A. Saboury and A.A. Moosavi-Movahedi
(Received November 12th, 1997; revised manuscript March 18th, 1998)
Stretching the Limits: According to High-Level Ab Initio Calculations C-O Bonds Are Longer than the Central C-C One in Hypothetical 2-Oxabicyclobutane
by H. Dodziuk1 and J. Leszczyński2
New Complex Compounds of Cu(I), Zn(II), Cd(II) and Hg(II) with 3-(2'-Thiothenoylamino)dibenzofuran
by V. Muresan, A. Reiss, L.S. Sbirna, N. Muresan and S. Florea
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