The attempt to prepare SF₅NOsO₃ by the reaction of OsO₄ and SF₅NH₂ in diethyl ether was not successful. The product obtained was a pale yellow crystalline substance which was identified as OsO₄ by infrared spectra and mass spectrometric data. No indication of SF₅NOsO₃ was observed. Several attempts to prepare Hg(NSF₂)₂ by the treatment of Hg(NCO)₂ with SF₄ in a solvent, such as THF, DMSO, (CH₃)PO₄ or CHCl₃, have failed, apparently due to interfering side reaction and decomposition. In THF and (CH₃)₃P0₄ systems, COF₂ was produced, but no Hg(NSF₂)₂ was produced in the solid product as shown by the infrared spectrum that there was no absorption band at 1313 cm⁻¹ as reported by Glemser for νS=N. No reaction was observed in CHC1₃ at room temperature or 100ºC. The reaction between Mo(CO)₆ and hot ethanol produced a green solution and a dark brown precipitate, for which the C and H analyses were not in agreement with the formula postulated by Buslaev as Mo(OC₂H₅)(OH)₃. The product of the reaction of the green solution and CsF was a light brown precipitate which showed no carbonyl group absorption in the. region at 2000 cm⁻¹. This should be observed for the compound to be postulated as Cs₃Mo₂(CO)₄F₄(OH)₃ by Buslaev. / Master of Science