A new example of a structurally characterized conjugated bis-guanidinate (CBG) supported zinc(I) dimer, , LZnZnL (3) (L = {(ArNH)(ArN)-CN-C(NAr)(NHAr)}; Ar = 2,6-Et-CH) with a Zn-Zn bond is reported. Moreover, homoleptic (3) and heteroleptic (Cp*ZnZnL, 2, (Cp* = 1,2,3,4,5-pentamethyl cyclopentadienide)) zinc(I) dimers are used as precatalysts in the dehydroborylation of a wide array of terminal alkynes. Furthermore, the active catalyst, CBG zinc acetylide (LZn-CC-Ph-4-Me), (5), is isolated which is confirmed by X-ray crystal structure analysis. A series of stoichiometric experiments have been performed to propose a plausible reaction mechanism.
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