Acetonitrile molybdenum complex

The resulting dark emerald green solution is filtered and the filtrate is concentrated to near dryness in vacuum. Diethyl ether (40 mL) is added and the solution is vigorously stirred to cause precipitation of the dark green molybdenum complex. The solution is filtered and the solid washed with two 5-mL portions of diethyl ether. The precipitate is dried in vacuum (10" 3 torr, 25 °C) to afford 3.36 g (90%) of dark emerald green cis-tetrakis(acetonitrile)-dinitrosylmolybdenum(II) bis[tetrafluoroborate(l —)]. 

I) Simple Monomeric Molybdenum Complexes. The first report on the synthesis of simple Mo dithio complexes appeared in 1971 when Mo(IV)(R2Dtc)4 complexes were obtained by CS2 insertion into Mo(NR2)4 complexes (68). Shortly after this report, the synthesis of these complexes from MoC14 and NaR2Dtc in acetonitrile was reported (88). A variety of tetrakis R2Dtc complexes of Mo(IV) also were obtained by the oxidative decarbonyla-tion of Mo(CO)6 with tetraalkyl thiuram disulfide (481,482, 609). 

Similarly, metathetical exchange of the labile acetonitrile ligands in the octahedral molybdenum complex (CO)2(MeCN)2BrMo( 3-C3Ph3) with a variety of bidentate amines led to the corresponding amino complexes (equation 267)311. These form crystalline acetonitrile solvates suitable for X-ray determination, which confirm the octahedral structure of these complexes and the occurrence of the cyclopropenyl and bromide groups in a tram-relationship. 

The [Fe3S4(SEt)4]3 undergoes conversion into the [4Fe-4S] cluster in acetonitrile with FeCl2 alone or in the presence of NaSEt.752 The molybdenum complex [Mo3S4(SCH2CH2S)3]2 contains the Mo3S44+ core, and shows similarity in its resonance Raman spectrum with [3Fe-4S] proteins.812... 

Acetonitrile, molybdenum and tungsten complexes, 26 122, 133 osmium complex, 26 290 palladium complex, 26 128 ruthenium complex, 26 356 ruthenium(II) complex, 26 69... 

Cobaltaie(l -), dodecacarbonylirontri-, tetraethylammonium, 27 188 Cobaltate(l -), dodecacarbonylirontri-, (triphenylphosphine)gold(l -(-), 27 188 -------, dodecacarbonylrutheniumtri-, tetraethylammonium, 26 358 Copper, (acetonitrile)dodecacarbonyltrico-balt ruthenium-, 26 359 Crystal growth, 26 377 Cyanate, tungsten complex, 26 42 Cycloheptatriene, molybdenum complex, 27 4... 

C2H,N, Acetonitrile, cobalt, copper, and ruthenium complexes, 26 356, 359 molybdenum, palladium, and tungsten complexes, 26 128-133 osmium complex, 26 290, 292 ruthenium(II) complexes, 26 69-72 C2H4, Ethene, molybdenum complex, 26 102-105... 

Huttner obtained molybdenum complex 215 upon treatment of ligand 115 with butyllithium, followed by BHs THF, tris(acetonitrile)tricarbonylmolybdenum, iodine, and l,4-diazabicyclo[2.2.2]octane (DABCO), in 76% yield as a mixture of two isomers (Scheme 37). Irradiation of 215 with a mercury high-pressure lamp caused ligand exchange with chelation of the remaining phosphane sidearm to give 216 in 72% yield. Oxidation of 215 with O2 under irrradiation resulted in a decarbonylation to give cationic oxomolybdenum complex 217 in 65% yield. 

Arene tricarbonyl molybdenum complexes are yellow, often crystalhne compounds. They are weakly air-sensitive in the sohd state and have to be stored under inert atmosphere and out of hght. They are best purified by crystaUization. In solution, they are unstable to air. The trait that has most hampered development of the use of (arene)Mo(CO)3 complexes in organic synthesis, however, is the lability of the arene metal bond. Lewis basic solvents such as THF, DMF, DM-SO, acetone and acetonitrile rapidly displace benzene in (benzene)Mo(CO)3. This lability of the arene-Mo bond, while making handling difficult, holds promise for the catalytic use of this class of compounds. 

A molybdenum complex contains one molybdenum (18.6%) and two iodines (49.2%), as well as carbonyl (CO) and acetonitrile (CH3CN) ligands. The combustion analysis gives C 16.3%, H 1.2% and N 5.4%. Determine the empirical formula. Assuming that the molecular formula is the same as the empirical formula, determine the number of acetonitrile and carbonyl ligands. 

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