Russian Chemical Bulletin, International Edition, Vol. 50, No. 3, pp. 1, March, 2001 1 1066-5285/00/5003-1$25.00 ©2001 Plenum Publishing Corporation Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 3, pp. 386394, March, 2001. Complex formation between azacrown derivatives of dibenzylidenecyclopentanone and alkali-earth metal ions À. Î. Doroshenko, a« À. V. Grigorovich, a Å. A. Posokhov, a V. G. Pivovarenko, b À. P. Demchenko, c,d and A. D. Sheiko b a Kharkov V. N. Karazin National University, 4 pl. Svobody, 61077 Kharkov, Ukraine. Fax: (38 057 2) 45 7130. E-mail: andrey.o.doroshenko@univer.kharkov.ua b Taras Shevchenko National University, 64 ul. Volodimirskaya, 02033 Kiev, Ukraine. Fax: (38 044) 224 6166. E-mail: pvg@mail.univ.kiev.ua c A. V. Paladin Institute of Biochemistry, 9 ul. Leontovicha, 02030 Kiev, Ukraine d TUBITAK Marmara Research Center, P.O. Box 21, 41470 Gebze-Kocaeli, Turkey. Fax: (90 262) 641 2309. E-mail: dem@rigeb.tubitak.gov.tr, adem@paladin.biochem.kiev.ua The complex formation of 2,5-bis[4-(1,7,10,13-tetraoxa-4-azacyclopentadec-4-yl)benzyl- idene]cyclopentanone and several model compounds, prospective metal-sensitive fluorescent probes, with Mg 2+ , Ca 2+ , and Ba 2+ ions in acetonitrile was studied. The azacrown derivatives of dibenzylidenecyclopentanone have two complex formation centers, azacrown cycle and carbonyl group. The sequence of binding to these sites is different for different ions. The efficient ejection of the Ca 2+ and Ba 2+ ions from their complexes with azacoronands was observed in the excited state, whereas in the case of the Mg 2+ ion, this process occurred only partially. Key words: bis(azacrown) derivatives of dibenzylidenecyclopentanone, ketocyanine dyes, electronic spectra, sequence of complex formation, fluorescent probes, carbonyl group, crown ethers, Kiprianov effect. The problem of development of ion-selective fluores- cent sensors for medical biological research has become urgent due to an increasing need for studying processes related to a change in the concentration of alkali and alkali-earth metal ions in biological objects. 1,2 Crown- containing organic luminophores are promising in this respect, and their spectral parameters change substan- tially when a metal binds to the macrocycle. 35 The related probes sensitive to the ion concentration allow monitoring of the microparameters of a biological object associated with the polarity of the microenvironment of the probe and also the microelectric parameters (for example, the surface potential of biomembranes related to the concentration of ions in the near-surface layer). 6 Organic aminocarbonyl compounds have long ago and widely been used as fluorescent probes. Since their molecules contain the electron-donating (alkyl)amino group and electron-withdrawing carbonyl group, the electron density redistribution between these groups dur- ing electron excitation results in a considerable increase in the dipole moment in the S 1 state. This determines the observed substantial solvatochromic and solvato- fluorochromic properties 7 of similar molecules. We assumed that symmetric dyes with two similar interacting chromophores and two complex formation centers can provide somewhat higher spectral sensitivity to metal ions. According to the Kiprianov theory, 8 when the chromophoric fragments are cleaved, the long-wave absorption band of similar compounds is split to a doublet, whose components are arranged at both sides from the position of this band in the initial mono- chromophoric compound. Binding of one ion should decompose the symmetry of the dye molecule. Accord- ing to the theory of interaction of chromophores, this should result in a noticeable hypsochromic shift of the absorption band. Symmetric bis(azacrown)ketocyanine dyes based on dibenzylidenecyclopentanone are appro- priate objects to check this hypothesis. The nitrogen atoms of the azacrown fragments in these compounds participate in conjugation with the π-electron system of the molecule, which suggests a noticeable dependence of the spectral parameters on the coordination of the metal ions with the crown ether groups. The following compounds were chosen as objects for the study: 2,5-bis[4-(1,7,10,13-tetraoxa-4-aza- cyclopentadec-4-yl)benzylidene]cyclopentan-1-one (1), 2-[4-(1,7,10,13-tetraoxa-4-azacyclopentadec-4-yl)ben- zylidene]-5-(4-diethylaminobenzylidene)cyclopentan-1- one (2), 2,5-bis[(4-dimethylamino)benzylidene]cyclo- pentan-1-one (3), 1,5-bis(4-dimethylaminophenyl)penta-