and 17.7 ppm and confirmed by 2D-experiments. 4c has been prepared previously, and the spectroscopic data matches that reported by Hill and co-workers. The study was expanded to include reaction of corresponding zinc hydride complex 2 with methylidene cycloalkanes (Scheme 1). In all cases, addition of 2 to 3b-d resulted in analogous reactivity and insertion of the alkene into the Zn-H bond. Reaction of 2 with 3b, 3c or 3d at 100 °C for 39 h yielded single alkene insertion products in high selectivity and good isolated yields (>70 %). Again Crystals of 5b and 5c suitable for single crystal X-ray diffraction were grown from n-pentane solution (Figure ). Both structures show the expected three-coordinate geometry at zinc supported by the diketiminate ligand and a hydrocarbon fragment that contains the intact carbocycle. The bond lengths to Zn are consistent with related structures and largely unremarkable. The sum of the N-Zn-N, N-Zn-C, and C-Zn-N bond angles for both is close to 360 ° for both 5b (359.96 °) and 5c (359.99 °)