in toluene Mo2(O-i-Pr)6 was dissolved in toluene uner N2, and the mixt. was cooled to -78°C. Iodotrimethylsilane was added dropwise. The soln. was allowed to warm to room temp.. After 3 h at room temp. the mixt. was warmed to 55°C and stirred (2 d).; The soln. was reduced in vol. by half and cooled to -15°C. After 2 d a ppt. was isolated by filtration and dried in vacuo.;

in toluene Mo2(O-i-Pr) was dissolved in toluene under N2. At room temp. acetyl bromide was added and the react. vessel shaken vigorously.; After the soln. turned green it was cooled to 0°C for 24 h, which yielded many crystals. The soln. was then cooled further to -15°C. After 2 d, many large crystals were isolated by filtration and dried in vacuo. Elem.anal.;

in toluene Mo2(O-i-Pr) was dissolved in a min. amt. of toluene. This soln. was cooled to -196°C. Acetyl fluorid was condensed into the react. vessel. The vessel was warmed to -20°C (2 d) and then cooled to -78°C. (7 d).; Filtration. Elem.anal.;

in toluene Mo2(O-i-Pr)6 was dissolved in toluene under N2. At room temp., acetyl chloride was added and the mixt. was shaken vigorously. After the mixt. stood at room temp. for 2 h, the color appeared to darken.; The soln. was cooled to 0°C for 24 h, which yielded many crystals. The soln. was then cooled slowly further to -15°C. After 2 d, many large crystals were isolated by filtration and dried in vacuo. Elem.anal.;

in hexane Mo2(O-i-Pr)6 was dissolved in a min. amt. of hexane under N2. At room temp., acetyl chloride was added and the mixt. shaken vigorously. The mixt. was then allowed to stand undisturbed for several hours.; On most occasions, small crystals formed at room temperature. The mixt. was then cooled to -15°C. After 2 d many large crystals were collected by filtration and dried in vacuo. Elem.anal.;

in hexane Mo2(O-i-Pr)6 was dissolved in a min. amt. of hexane under N2. At room temp., acetyl bromide was added and the mixt. was shaken vigorously. The color changed from yellow to burgundy, and enough heat was evolved that the flask was very hot to touch.; The flask was then allowed to stand to cool to room temp. undisturbed for several h. After 2 h crystals were present. The soln. was then cooled to -15°C. After 1 d crystals were collected by filtration and dried in vacuo. Elem.anal.;

in hexane Mo2(O-i-Pr)6 was dissolved in hexane under N2. At room temp., chlorotrimethylsilane was added. The mixt. was then kept at 38°C (12 h).; The vol. of the soln. was reduced by half and cooled to -15°C. Crystals were obtained after 3 d. A second crop of crystals was obtained by reducing the vol. of the filtrate and cooled to -15°C.;

in hexane Mo2(O-i-Pr)6 was dissolved in hexane soln. under N2. At room temp., bromotrimethylsilane was added with stirring. After 2 h the soln. had changed color from yellow to burgundy, indicating the formation of Mo4Br3(O-i-Pr)9.; The vol. of the soln. was reduced by half and cooled to -15°C. Crystals were obtained after 3 d. A second crop of crystals was obtained by reducing the vol. of the filtrate and cooling to -15°C.;

in hexane Mo2(O-i-Pr)6 was dissolved in hexane. This soln. was cooled to -21°C, and then a hexane soln. of iodotrimethylsilane was added to the stirring soln.. The soln. was stirred at -21°C for 2 h.; The soln. was then allowed to warm to room temp. and stirred another 4 h, to yield a microcrystalline ppt.. The mixt. was then cooled to -15°C, and small crystals were isolated after 1 d.;

in toluene Under N2, Mo2(O-i-Pr) was dissolved in toluene, and the mixt. was cooled to -78°C. Iodotrimethylsilane was added, and the react. mixt. was stirred and warmed to 0°C. After 2 h the soln. was allowed to warm to room temperature.; The soln. was reduced in vol. by half and cooled to -15°C for 24 h, which yielded crystals. After 2 d, crystals were isolated by filtration and dried in vacuo. Traces of Mo4O2I2(O-i-Pr)6 present in Mo4I4(O-i-Pr)8; detd. by (1)H-NMR.;