Lambda 6 spectrophotometer

All reactions were performed under an argon atmosphere with Schlenkware and cannula techniques. All solvents were distilled under argon prior to use. Dichloromethane and hexane were distilled from CaH₂ and sodium/benzophenone, respectively. 4-Cyanopyridine was recrystallized from diethyl ether and imidazole was recrystallized from dichloromethane. Tetramesitylporphyrin was prepared by a modified version of the procedure published by Lindsey et al.[13 ] and iron was inserted into H₂TMP [12 ] by standard techniques [14 ]. [Fe(TMP)OClO₃] was prepared as previously described. [6 ] Caution! These perchlorate salts can detonate spontaneously and should be handled only in small quantities; other safety precautions are also warranted. UV-vis spectra were recorded on a Perkin-Elmer Lambda 6 spectrophotometer. Mössbauer samples were prepared from ground single-crystal samples as mulls in Apiezon L grease, as previously described [7 ]. Mössbauer measurements were made on a constant acceleration spectrometer. The spectra were fitted with Lorentzian line shapes. Isomer shifts are quoted relative to metallic iron at room temperature.