Synthesis of Na[Fe(EDTA)]3H2O Dissolve 0.4 g (0.01 mol) of NaOH in 10 cm3 of water, and then add 3.8 g (0.

01 mol) of Na2H2EDTA2H2O. Gently heat the solution until the solid dissolves to give a clear solution. Dissolve 2.5 g (0.009 mol) of iron(III) chloride hexahydrate in 5 cm3 of water, which is then added to the EDTA solution with swirling. Gently boil off the water until most of the yellow powder precipitates out. Cool down the solution and collect the precipitate by suction filtration. Wash the product thoroughly with ice water until it is free of iron(III) ions. Wash the product with ethanol twice and dry it with filter paper.

Sinteza 2 EDTA disodium salt dihydrate (Na2EDTA 2H2O) was added to the FeCl3 solution in at a molar ratio of 1:1 (Fe:EDTA). The FeCl3 solution is, however, too acidic for direct addition of the Na2EDTA 2H2O. Direct addition of this salt to the FeCl3 solution at these low pH values would result in the precipitation of EDTA. The Na2EDTA 2H2O is consequently predissolved in 2 ml of a 5 mm NaOH, prepared with double-deionized sterile water. This solution is added dropwise to the FeCl3 while swirling continuously. A brown coloration forms as the NaOHNa2EDTA solution makes contact with the FeCl3 solution in the flask, and then quickly disappears with mixing. This brown residue is owing to the formation of an iron (III) hydroxo complex, which forms in the immediate contact area of the NaOH, owing to the higher pH of this solution. An excessively high final pH value (pH >6) of the final reaction mixture would result in a precipitation of iron (III) hydroxide, which can be easily rectified by the addition of HCl. The resulting NaFe(III)EDTA solution was made up to the desired concentration (10 mg Fe/ml) with double-distilled deionized sterile water. Should a powder be required for use in the bioavailability study to follow, drying the product solution under a nitrogen stream may be carried out without any product degradation or loss in product purity.

2.1. Preparation of K[Fe(Hedta)(Cl)] H 2 O (1)

Ethylenediaminetetraacetic acid (H4edta) (2.92 g, 0.01 mol) and 2.70 g (0.01 mol) FeCl36H2O were stirred in 20 ml on a stirring plate with heating. A clear yellow solution resulted after about 10 min. Now, 1.44 g (0.03 mol) KHCO3 was added in small portions and the color of the solution changed to orange. During standing in the refrigerator over several days, yellow crystals precipitated. These were removed by suction and washed with cold water and acetone. Recrystallization was carried out from a water-acetone mixture. Yield: 3.5g (80%). Anal. Calc. for C10H15ClFeKN2O9 (437.6): C, 27.44; H, 3.45; N, 6.40. Found: C, 27.30; H, 3.50; N, 6.35%. Single crystals suitable for X-ray structure determination were prepared in the following way: a concentrated, aqueous solution of 1 was gently layered with the threefold volume of acetone in a large reagent glass. After several days, yellow crystals formed, which were removed by hand picking. 2.2. Preparation of K[Fe(edta)(H 2 O)] 1.5H 2 O (2)

The same procedure as described for the synthesis of 1 was carried out except that 1.92 g (0.04 mol) KHCO3 were added to neutralize all 4 protons of the ligand. The reaction solution was mixed with the fourfold volume of acetone and stored over several days in the refrigerator. The yellow brown precipitate that formed on standing was removed by suction and washed with methanol and acetone. Single crystals were prepared in the same way as described above. Yield: 3g (70%). Anal. Calc. for C10H17FeKN2O10.5 (428.2): C, 28.05; H, 4.00; N, 6.54. Found: C, 27.95; H, 4.08; N, 6.50%.