Polish J. Chem., 77, 1059–1077 (2003) REVIEW ARTICLE Equilibrium Study of Iminodi(methylenephosphonic) Acid Complexes with Some Metal Ions by B. Kurzak and A. Kamecka Institute of Chemistry, University of Podlasie, ul. 3 Maja 54, 08-110 Siedlce, Poland (Received December 3rd, 2002; revised manuscript April 25th, 2003) This article discusses coordination preferences of N-substituted iminodi(methylene- phosphonic) acids to the different metal ions in an aqueous solution. These ligands ex- hibit high complexation efficiency towards divalent metal ions. This results from both dinegatively charged phosphonate groups as well as the imino nitrogen present in their structure. A significant preference for an equimolar stoichiometry has been demon- strated in these systems. The only exception is the N-2-methyltetrahydrofurylimino- di(methylenephosphonic) acid with a tetrahydrofuryl moiety, placed in the sterically favoured position that allows its oxygen atom to be an effective metal binding site. Spe- cific interactions between metal ions and furyl oxygen results in higher binding ability of this ligand and a formation of 1:2 species. Coordination properties of iminodi- (methylenephosphonic) acids are important factors to understand the role of the ligands and metal ions in biological systems. A summary presented in this review points on the direction of the research for future work in this area, which should be developed. Polish J. Chem., 77, 1079–1111 (2003) REVIEW ARTICLE Resorcinarenes by W. Œliwa, T. Zujewska and B. Bachowska Institute of Chemistry and Environmental Protection, Pedagogical University, al. Armii Krajowej 13/15, 42-201 Czêstochowa, Poland (Received May 5th, 2003) Selected examples of resorcinarenes are described, concerning their syntheses and reac- tivity. Formation of complexes, host-guest systems and capsules is also presented along with their possible applications. A short comment concerning pyrogalloarenes is added. In the paper references are cited of works that appeared during the years 1998–2003. Polish J. Chem., 77, 1113–1119 (2003) INORGANIC CHEMISTRY Synthesis and Characterization of Mixed Phosphazene–Glycolate Complexes of Antimony(III) by Y. Paul and S.K. Pandey Department of Chemistry, University of Jammu, Baba Saheb Ambedkar Road, Jammu -180 006, (J & K), India (Received March 11th, 2003; revised manuscript April 28th, 2003) Antimony(III)triazadiphosphorine complexes, [N(PPh2NR’)2SbOGO] (where R’ = -Ph or -SiMe3 and G = -CHMeCH2-, -CHMeCH2CMe2-, -CH2CH2CH2-, -CH2CMe2CH2-, -CH2CEt2CH2- or -CMe2CMe2-), have been synthesized by the reaction of bis-phenyl- ated acyclic phosphazene ligand, H[N(PPh2NPh)2], or bis-silylated acyclic phospha- zene ligand, H[N(PPh2NSiMe3)2], with various cycloalkylenedioxyalkoxystibine, [OGOSb(OR)], (where R = -Et or -Pri) under anhydrous and inert conditions. The mixed phosphazene-glycolate derivatives of antimony(III) have been characterized by elemental analysis (C, H, N and Sb), molecular weight determination, mass, IR and NMR (1H, 13C and 31P) spectroscopies. The studies suggested a bidentate mode of bonding by phosphazene ligand that may lead to Y-trigonal bipyramidal coordination around the an- timony. Ahydrolytically stable and rubber like material has been obtained on pyrolysis of [N(PPh2NPh)2SbOCH2CMe2CH2O] which, probably, has an oligomeric composition like {N(PPh2)2(NPh)2Sb}n . Polish J. Chem., 77, 1121–1129 (2003) Synthesis, Spectroscopic Characteristics and Conductometric Investigation of New Tetrachloro- and Tetrabromoferrates(1-) by Z. Warnke, D. Wyrzykowski and G. Wawrzyniak Faculty of Chemistry, University of Gdañsk, 80-952 Gdañsk, Sobieskiego 18, Poland (Received March 11th, 2003; revised manuscript May 29th, 2003) Synthetic pathways have been traced for new tetrachloro- and tetrabromoferrates(1-) of empirical formulae [AH][FeX4], (AH)2FeBr5, (AH)3Fe2Cl9 and (AH)4Fe2Cl10, where A stands for pyridine, quinoline and their derivatives, and X = Cl, Br. The spectroscopic ev- idence (IR, far-IR, Raman and UV-Vis) has shown that the Fe − ions preserve their tetra X4 - hedral structure and that the nitrogen atom in the rings of pyridine and quinoline is protonated. On the basis of conductometric measurements relative stabilities of the an- ions were estimated in methanol (MeOH), dimethyl sulfoxide (DMSO) and dichloro- methane (CH2Cl2), representing both polar (amphiprotic and protic) and non-polar solvents. Dissociation constants of the compounds were calculated based on the ex- panded Pitt’s equation. Results of the conductometric measurements have been sup- ported by electronic spectra. Polish J. Chem., 77, 1131–1134 (2003) Study of Phase Equilibria in the System Nd2O3–Na2O–P2O5. The Quasi-Binary Section Nd(PO3)3–NaPO3 by T. Znamierowska and Sz. Bandrowski Department of Inorganic Chemistry, Faculty of Engineering and Economics, Wroc³aw University of Economics, Komandorska 118/120, 53-345 Wroc³aw, Poland (Received May 29th, 2003; revised manuscript July 1st, 2003) The quasi-binary section Nd(PO3)3–NaPO3 has been investigated by thermoanalytical methods (DTA, TG, DTG) and X-ray powder diffraction and its phase diagram was pro- posed. It was found that initial metaphosphates react at a 1:1 molar ratio, forming the in- termediate compound NaNd(PO3)4. It was confirmed, that it melts incongruently at about 866°C, giving Nd(PO3)3 and a liquid rich in NaPO3. The phosphate NaNd(PO3)4 is stable to room temperature and does not exhibit polymorphic transitions. Polish J. Chem., 77, 1135–1140 (2003) ORGANIC CHEMISTRY Structure of the Polysaccharide O-Antigen of Salmonella Aberdeen (O : 11) by J. Szafranek1, M. Kaczyñska1, Z. Kaczyñski1, J. Gajdus1, M. Czerwicka1, H. Dziadziuszko2 and R. G³oœnicka2 1Faculty of Chemistry, University of Gdañsk, 80-952 Gdañsk, Sobieskiego 18, Poland 2Institute of Maritime and Tropical Medicine, 81-519 Gdynia, Powstania Styczniowego 9b, Poland (Received February 24th, 2003; revised manuscript June 9th, 2003) O-specific polysaccharide (OPS) of Salmonella Aberdeen was obtained from bacterial cell mass by water-phenol extraction procedure of lipopolysaccharide (LPS) followed by its mild acid hydrolysis and gel filtration of soluble carbohydrate material. Rhamnose, galactose, N-acetyl-glucosamine and mannose were detected and their linkages were es- tablished. Sugar configurations, D or L, were determined for (S)-(+)-2-butyl glycosides on an achiral capillary column. The structure of OPS was determined by analysis of spec- tra of 1H and 13C NMR and homonuclear and heteronuclear correlations spectra. Anomeric configurations were tentatively assigned by chromium trioxide oxidation and later proved by anomeric proton chemical shifts, H1-H2 coupling constants and pro- ton coupled 13C spectra. Sugar sequences were established from comparisons of specific carbon shifts with those from literature, two-dimensional nuclear Overhauser effect spectroscopy (NOESY) and heteronuclear multiple-bond correlation experiments (HMBC). The repeating unit of S. Aberdeen OPS has the structure: ®3)-b-D-GlcpNAc-(1®3)-[ b-D-Manp-(1®4)-]a-D-Galp-(1®4)-a-L-Rhap-(1® Polish J. Chem., 77, 1141–1147 (2003) A Facile Synthesis of 4-Aryl-1H-pyrazolo[3,4-b]quinolines by K. Chaczatrian, G. Chaczatrian, A. Danel and P. Tomasik Department of Chemistry, University of Agriculture, Mickiewicz Ave. 21, 31-120 Cracow, Poland (Received April 24th, 2003; revised manuscript June 9th, 2003) A novel synthesis of 1H-pyrazolo[3,4-b]quinolines, luminophores for electroluminescent devices, was developed. Conventional heating (180–190°C in ethylene glycol) or micro- wave exposure of a three-component mixture of an aromatic aldehyde, 3-substituted 1-phenyl-4,5-dihydro-1H-pyrazol-5-one and aromatic amine produced 4-aryl-1H-pyra- zolo[3,4-b]quinolines. Polish J. Chem., 77, 1149–1155 (2003) A Facile Synthesis of Annulated 2,2¢-Bipyridine Ligands with Alkylsulfanyl and Alkylsulfonyl Substituents in the 6 and 6’ Positions [1] by D. Branowska and J. Kielak Department of Chemistry, University of Podlasie, 3-go Maja 54, 08-110 Siedlce, Poland (Received June 6th, 2003; revised manuscript June 17th, 2003) 3,3¢-Bis(isopropylsulfanyl)-5,5¢-bi-1,2,4-triazine 2 is easily transformed into annulated 2,2¢-bipyridines 4 and 6 with fused cycloalkene rings via [4+2]cycloaddition/retro cycloaddition reaction with cyclic enamines 3a–d. Oxidation of 4 and 6 with potassium permanganate under phase transfer catalysis conditions provided a series of the corres- ponding sulfonyl derivatives 7 and 8. Polish J. Chem., 77, 1157–1161 (2003) Aromatic Nucleophilic Substitution in 1,2,4-Triazine 4-Oxides with Grignard Reagents by A.M. Prokhorov, D.N. Kozhevnikov, V.L. Rusinov and O.N. Chupakhin Urals State Technical University, 620002, Ekaterinburg, Russian Federation Fax: +7 3432 740458, E-mail: [email protected] (Received July 8th, 2003) Addition of the Grignard reagents to 1,2,4-triazine 4-oxides followed by aromatization of the intermediatesH-adducts by dehydrogenation or dehydration was used for synthesis of 5-alkyl- or 5-aryl-substituted 1,2,4-triazines and their 4-oxides. Polish J. Chem., 77, 1163–1173 (2003) PHYSICAL CHEMISTRY Sweetness-Vibrational Spectra Relationship in Aldopyranoses and Sucrose/Galactosucrose System by W. Pietrzycki Department of Chemistry, H. Ko³³¹taj University of Agriculture, Mickiewicz Avenue 21, 31-120 Kraków, Poland (Received January 29th, 2003; revised manuscript May 14th, 2003) Correlation of the RS relative sweetnesses of 6 aldopyranoses, maltose and lactose on the structures of their PM3 vibrational