Synthesis of FeOCl TTF

Figoie 1. Schematic drawing of the reaction flask used for intercalation reaction. 

The materials and methods used are identical to those described above for FeOCl(TTF)i/8 5. A flask is charged with 0.200 g (1.80 mmol) FeOCl and 0.400 (1.6 mmol) perylene (Aldrich Chemical Co.). Freshly distilled dimeth-oxyethane 20.0 mL is then added by syringe. Because of the poor solubility of perylene in the solvent, much of the intercalant is suspended in the solvent at this point. The flask is then evacuated and purged with dry nitrogen several times and sealed at the vapor pressure of the solvent. The flask is then wrapped in A1 foil, and heated in an oilbath at 85 ° for 30 days. After this time, the solid is collected on a glass frit, washed with 3(X) mL CH2CI2 in 30 mL portions, and 100 mL DME, and dried in vacuo. 

The product is characterized by X-ray powder diffraction diffraction lines d(A) = 16.68(s), 8.332(m), 2.718(w), 1.889(s), 1.835(w), 1.658(w), 1.244(w) a = 3.321(1) k,b = 3.782(2) A, c = 33.38(9) A. FT-IR 490(vs), 696(m), 819(s), 1186(s), 1348(m), 1541(s, broad). Elemental analysis consistent with stoichiometry FeOCl(perylene)i/9. In many cases DME is found to cointercalate with perylene into FeOCl, resulting in the compound FeOCl(perylene)i/9 DMEi/20 chemical ionization mass spectrum miz = 253 (perylene) and w/z = 91 (DME). However, DME deintercalates at lower temperatures ( 160-200°) than does perylene ( 300-400°) and can be selectively removed from the interlayer region of the host by heating in vacuo (190°, 10 torr, 2 days) with no signihcant changes in structural or physical properties. 

Halbert, in Intercalation Chemistry, M. S. Whittingham and A. J. Jacobson (eds.). Academic Press, Orlando, 1982, Chapter 12. 

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