For the preparation of λ 5 -phosphinine dimers connected directly through a C-C bond, that is 6a-b, we first relied on an oxidative coupling strategy (with either FeCl3, MoCl3 or DDQ/MeSO3H) applied directly on DCNP. However, after various unsuccessful tries, we turned to Ni-mediated Yamamoto coupling. After optimization of the conditions, this approach led to the preparation of the targeted dimers 6a and 6b in satisfying yields (Scheme 2).