The reactions of acetone and of diacetone alcohol with [Mo{HB(3,5-Me2C3HN2)3}(NO)I2]. The formation of [Mo{HB(3,5-Me2C3HN2)3}(NO)I(OEt)] and the structures of [{Mo[HB(3,5-Me2C3HN2)3](NO)I}2O] and a bicyclic salt [C6H3Me5N2(OH)][I½(I3)½]

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Abstract
The complex [Mo{HB(Me2pz)3}(NO)I2](Me2pz = 3,5-dimethylpyrazolyl) reacted with boiling acetone and with diacetone alcohol (4-hydroxy-4-methyl-2-pentanone) over several days, giving low yields of the salt of the cation [C6H3Me5N2(OH)]+, [{Mo[HB(Me2pz)3](NO)I}2O], and [Mo{HB(Me2pz)3}(NO)I(OEt)]. The structure of an iodide salt of the organic cation, and of the bimetallic species have been determined crystallographically. The organic salt is a bicyclic species derived by fusion of a C3 fragment (possibly derived from diacetone alcohol) across the N–N bond of 3,5-dimethylpyrazole. The bimetallic species can be described as two distorted, eclipsed octahedra sharing the bridging O atom, where the Mo–O distances are 1.86 and 1.93 Å, and the Mo–O–Mo angle is 171°. Possible routes to the formation of these compounds are discussed.

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