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The solid-state structure of the rhodium complex (dimethylamine–dimethylaminoborane–borane-κ2H,H′)dihydridobis(triisopropylphosphane-κP)rhodium(III) tetrakis[3,5-bis(trifluoromethyl)phenyl]borate, [RhH2(C4H18B2N2)(C9H21P)2](C32H12BF24), is reported. The complex contains the linear diborazine H3B·NMe2BH2·NMe2H, a kinetically important intermediate in the transition-metal-mediated dehydrocoupling of H3B·NMe2H, ultimately affording the dimeric amino-borane [H2BNMe2]2. The structure of the title complex contains a distorted octahedral RhIII centre, with mutually trans phosphane ligands and cis hydride ligands. The diborazine is bound through two Rh—H—B σ-bonds and exhibits a gauche conformation with respect to the B—N—B—N backbone.