Hydrophenylation of internal alkynes with boronic acids catalysed by a Ni-Zn hydroxy double salt-intercalated anionic rhodium(III) complex

[Rh(OH)(6)](3-) intercalated Ni-Zn mixed basic salt (Rh/NiZn) acts as an efficient catalyst for the hydrophenylation of internal alkynes with arylboronic acids under mild conditions. The turnover number per Rh site approached 740 in the reaction between 4-octyne and phenylboronic acid. The catalytic monomeric Rh.III) complex is stabilised within the NiZn interlayers, attributable to a strong electrostatic interaction, promoting its re-use.