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Electron Resonance Spectroscopy In a fume hood 2.8 g of iron (II) sulphate was dissolved in sulphuric acid (12.

5 cm3, 2 M), to this a mixture of sodium diethyldithiocarbamate trihydrate (5.0 g) and sodium nitrate (0.76 g), the solution was then rapidly stirred for a further 15 minutes. At this point the contents were transferred to a separating funnel with chloroform (30cm3). The organic layer was removed from the aqueous, and the aqueous layer was then washed with more chloroform (5 cm3, twice) and the resulting organic extracts were all combined, and then dried over magnesium sulphate. The magnesium sulphate was then filtered off under gravity and then the solvent volume was reduced by half under rotary evaporation. 20 cm3 of methanol was then added to the solution and it was left to cool in an ice bath to allow crystals to form, these were then filtered off and dried with a Buchner funnel (0.2 g, black crystals, 7.1% yield). The mother liquors were then reduced by half under rotary evaporation and this solution was placed in an ice bath to allow crystals to form which were collected as above (0.6 g, black crystals, 21.4% yield). Total yield of 28.5%. Melting range of first sample: 182-188C Melting range of second sample: 165-173C

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