Grafted-Type Compound from FeOCl

Direct reaction of FeOCl with methanol does not occur up to a temperature of 100°. In contrast, the reaction of FeOCl(apy)i/4 is a facile one due primarily to the expanded interlayer distance which permits penetration of the methanol molecules. 

The intercalation compound FeOCl(apy)i/4, 80 mg, is soaked in 2 mL of methanol (previously dried over 3A molecular sieves for 3 days) in a sealed Pyrex glass tube, which is typically 10 cm long and 0.8 cm in diameter, with a wall thickness of 2.0 mm. The tube is maintained at 100° and shaken twice daily for 10 days. (If difficulty is encountered in obtaining intercalation, it may be helpful to add a small amount of APy.) The resulting brown solid is collected by filtration, washed with several volumes of dry methanol, then stored in a desiccator with silica gel. 

The interlayer distance in FeO(OCH3) is 9.97 A. The infrared spectrum shows a C-0 stretching vibration around 1050 cm , but no 0-H stretching vibration. A study of the Mossbauer effect at room temperature indicates that the isomer shift and the quadrupole splitting are 0.37 and 0.60 mm/s, respectively. 

The basal spacing of FeO(02C2H4) is 14.5 A when the product is still in ethylene glycol, but it shrinks to 10.98 A on washing with acetone. Mossbauer isomer shift and quadrupole splitting are respectively 0.38 and 0.59 mm/s at room temperature. 

R GRAFTED-TYPE COMPOUND FROM FeOCl 1. Methanol-Grafted Compound FeO(OCH3) 

The interlayer distance in FeCKOCHj) is 9.97 A. The infrared spectrum shows a C—O stretching vibration around 1050 cm but no O—H stret- 

---