Abstract
The reaction of ReH 9 2− with Mo(diglyme)(CO) 3 leads to the formation of the mixed metal cluster trianion, ReMo 3H 4(CO) 12 3−. This species has been characterized analytically, spectroscopically and through X-ray diffraction analysis. A pseudo-tetrahedral arrangement of M(CO) 3 fragments is adopted, such that each set of three carbonyl ligands eclipses the adjacent three tetrahedral edges, an apparent result of the location of the hydride ligands on the tetrahedral faces. Variable temperature NMR studies revealed a fluctional process for some of the carbonyl ligands, but not for the hydrides. Crystal data for [Me 4N] 3[ReMo 3H 4(CO) 12]·THF; space group P2 1/ n, a = 12.157(2), b = 21.480(4), c = 15.964(3) A ̊ , β = 98.26(1)°, Z = 4, R = 0.067 and R w = 0.076 .
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