90 RADIOCHEMISTRY, STABLE ISOTOPES, NUCLEAR ANALYTICAL METHODS, GENERAL CHEMISTRY Congress. Part A. Ed. P. Vincenzini. Techna Srl, Faenza 2003, pp.341-352. [2]. Deptuła A., Olczak T., Łada W., Sartowska B., Chmielewski A. G., Alvani C., Carconi P.L., Di Bartolomeo A., Pierdominici F., Casadio S.: J. Sol-Gel Sci. Technol., 26, 207 (2003). [3]. Deptuła A., Olczak T., Łada W., Chmielewski A.G., Alvani C., Carconi P.L., Di Bartolomeo A., Pierdominici F., Casadio S.: J. Mater. Sci., 37, 1 (2002). [4]. Renoult O., Boilot J.-P., Korb J.-P., Boncoeur M.: J. Nucl. Mater., 223, 126 (1995). [5]. Wen Z., Gu Z., Huang S., Yang J., Lin Z., Yamamoto O.: J. Power Sources, 146, 670 (<strong>2005</strong>). [6]. Kavan L., Grätzel M.: Solid State Lett., 5, A39 (2002). [7]. Moshopoulou E.G.: J. Am. Ceram. Soc., 82, 3317 (1999). [8]. Bohnke C., Duroy H., Fourquet J.L.: Sens. Actuators, B89, 240 (2003). [9]. Vijayakumar M., Nghi Pham Q., Bohnke C.: J. Eur. Ceram. Soc., 25, 2973 (<strong>2005</strong>). [10]. Kosewa I., Chaminade J.P., Gravereau P., Pechev S., Pechev P., Etoumeau J.: J. Alloys Compd., 389, 47 (<strong>2005</strong>). [11]. Berbenni V., Marini A.: J. Mater. Sci., 39, 5279 (2004). [12]. Okayama J., Takaya I., Nashimoto K., Sugahara Y.: J. Am. Ceram. Soc., 85, 2195 (2002). [13]. Shendo R., Krueger D.S., Rossetti G.A. Jr., Lombardo S.J.: J. Am. Ceram. Soc., 84, 1648 (2001). [14]. Janes R., Knightley L.J.: J. Mater. Sci., 39, 2589 (2004). [15]. Yang J., Li D., Wang X., Lu L.: J. Mater. Sci., 38, 2907 (2003). [16]. Mazdyiasni K.S, Dolloff R.T., Smith J.: J. Am. Ceram. Soc., 52, 523 (1969). [17]. Phule P.P., Risbud S.H.: Adv. Ceram. Mater., 3, 183 (1988). [18]. Chaput F., Boilot J.P., Beauger A.: J. Am. Ceram. Soc., 73, 942 (1990). [19]. Phule P.P., Risbud S.H.: J. Mater. Sci., 25, 1169 (1990). [20]. Hu M.Z.C., Miller G.A., Payzant E.A., Rawn C.J.: J. Mater. Sci., 35, 2927 (2000). [21]. Cheung M.C., Chan H.L.W., Choy C.L.: J. Mater. Sci., 36, 381 (2001). [22]. Beck H.P., Eisner W., Haberkorn R.: J. Eur. Ceram. Soc., 21, 2319 (2001). [23]. Kumar S., Messing G.L., White W.B.: J. Am. Ceram. Soc., 76, 617 (1993). [24]. Takeuchi T., Tabuchi M., Ado K., Honjo K., Nakamura O., Kageyama H., Suyama Y., Ohtori N., Nagasawa M.: J. Mater. Sci., 32, 4053 (1997). [25]. Deptuła A., Łada W., Olczak T., Lanagan M., Dorris S.E., Goretta K.C., Poeppel R.B.: Polish Patent No. 172618. [26]. Deptuła A., Rebandel J., Drozda W., Łada W., Olczak T.: Mater. Res. Soc. Symp. Proc., 270, 277 (1992). [27]. Deptuła A., Łada W., Olczak T., LeGeros R.Z., LeGeros J.P.: Bioceramics, 9, 313 (1996). [28]. Łada W., Deptuła A., Sartowska B., Olczak T., Chmielewski A.G., Carewska M., Scaccia S., Simonetti E., Giorgi L., Moreno A.: J. New Mater. Electrochem. Syst., 6, 33 (2003). [29]. Chatterjee M., Naskar M.K., Ganguli D.: J. Sol-Gel Sci. Technol., 16, 143 (1999). [30]. Ueyama R., Harada M., Ueyama T., Yamamoto T., Shiosaki T., Seo W.S., Kuribayashi K., Koumoto K.: J. Mater. Sci.: Mater. Electron., 11, 139 (2000). [31]. Holland T.J.B., Redfern S.A.T.: Mineral Mag., 61, 65 (1997). STUDY OF GLUCOFURANOSE-BASED GEL NANOSTRUCTURE USING THE SAXS METHOD Helena Grigoriew, Roman Luboradzki 1/ , Dagmara K. Chmielewska, Monika Mirkowska 2/ 1/ Institute of Physical Chemistry, Polish Academy of Sciences, Warszawa, Poland 2/ Warsaw University of Technology, Poland The glucofuranose-based gels were synthesized by the method described in [1]. The gelator of chemical formula: 1,2-O-(1-ethylpropylidene)-α-D-glucofuranose is built of furanose ring and contains three unprotected -OH groups. Its concentrations of 3, 1, 0.5 and 0.1% in toluene were chosen. The measurements were carried out with a ULTRA-SAXS BW-4 wiggler beamline of the HASYLAB synchrotron. The obtained data were subjected to pie integration and, after normalization, to subtraction of the background which was the SAXS curve of the solvent. For each sample, two measurements with sample-detector distances of 4 and 12 m were performed and joined using OTOKO program [2] Table. Structural parameters vs. gelator concentration. to get a bigger range of the data. The complex method of SAXS data processing was applied, to find structural parameters of the gelator in gel, such as: the mass fractal, d m , and surface fractal, d s , dimensions, radius of gyration, R g , distance distribution function, p(r), and dummy atom models [3-5]. The results (Table and Figs.1 and 2) of all methods make it possible to assume that two types of aggregates exist in the gel. The differences between them are: the first type (for 3% gel) – the aggregate is smaller, compact, of well-defined smooth surface and a rod-like shape, and the second type (for 0.1% gel) – aggregate is bigger, looser, of rough surface and a disk-like shape. The aggregate change at in-
RADIOCHEMISTRY, STABLE ISOTOPES, NUCLEAR ANALYTICAL METHODS, GENERAL CHEMISTRY 91 termediate concentration is gradual and there, especially for 0.5%, a mix of both types is detected. The results suggest the appearance of structural Fig.2. Model aggregate for (a) 0.1% gel and (b) 3% gel. Fig.1. Fractal analysis, log-log curves with fitted straight-line segments. transformation caused by the change of gelator concentration. The transition acts gradually with concentration change. The process of glucofuranose-based gels formation occurred not caused by the same kind of self-assembly of aggregates but its course is dependent on the concentration of the gelator molecules in solvent. This work was supported by the Polish Ministry of Scientific Research and Information Technology under contract No. 3 IO9A 136 27 and by the European Community – Research Infrastructure Action under the FP6 “Structuring of the European Research Area” Programme (through the Integrated Infrastructure Initiative “Integating Activity on Synchrotron and Free Electron Laser Science”). References [1]. Luboradzki R., Pakulski Z.: Tetrahedron, 60, 4613-4616 (2004). [2]. Koch M.H.J.: OTOKO – program package, release 01.90 EMBL-DESY. [3]. Svergun D.I.: J. Appl. Crystallogr., 25, 495 (1992). [4]. Svergun D.I.: Biophys. J., 76, 2875 (1999). [5]. Svergun D.I.: J. Appl. Crystallogr., 33, 530 (2000). CRYSTAL CHEMISTRY OF COORDINATION COMPOUNDS WITH HETEROCYCLIC CARBOXYLATE LIGANDS. PART LIV. THE CRYSTAL AND MOLECULAR STRUCTURE OF BIS[HEXAQUAMAGNESIUM(II)] PYRAZINE-2,3,5,6-TETRACARBOXYLATE TETRAHYDRATE Michał Gryz 1/ , Wojciech Starosta, Janusz Leciejewicz 1/ Office for Registration of Medicinal Products, Medical Devices and Biocides, Warszawa, Poland Triclinic unit cell [space group P1(bar)] of the title compound contains two hexaquamagnesium(II) cations, one fully deprotonated pyrazine-2,3,5,6-tetracarboxylate (2,3,5,6-PZTC) anion with its geometrical centre situated at the inversion centre and four solvation water molecules. Figure 1 shows the relevant ions with atom numbering scheme, Fig.2 – the content of the unit cell. The magnesium(II) ion is sorrounded by six water molecules with their oxygen atoms located at the apices of a fairly regular octahedron. Mg-O bond distances range from 2.036(1) to 2.115(1) Å (mean 2.065 Å). The pyrazine ring of the anion is planar (rms 0.0001 Å), the carboxylate groups are inclined to the pyrazine ring by 22.8 and 99.1 o . A three-dimensional network of hydrogen bonds with d(O-H...O)>2.70 Å is oper-
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