Heterobimetallic drive and cooperativity lead to a striking scenario for C-H bond activation and heteroaggregation involving Mo(III) dimers. Reaction of (RO)(3)Mo[triple bond]Mo(OR)(3) with molar excess of ZnMe(2) at-78 degrees C affords the novel mixed Zn, Mo oxo clusters [Mo(2)(MeZn)(6)(mu(2)-Me)(mu(3)-CH(2))(2)(OR)(7)] 1 (R = neopentyl) and 2 (R = cyclohexyl) preserving the Mo[triple bond]Mo triple bond, while the same reaction performed at ambient temperature gives rise to the related cluster [Mo(2)(MeZn)(6)(mu(2)-CH(2))(mu(3)-CH(2))(2)(OR)(6)] 3. These complexes represent the first examples of heterobimetallic Mo[triple bond]Mo complexes with bridging methyl and methylene groups and agostic C-H-->Mo interactions, as well as penta-coordinate carbon. The complexes 1-3 were characterized by elemental analyses, multinuclear NMR and single-crystal X-ray diffraction analysis.
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