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We report the synthesis of a Cp*Rh complex bearing a pyridyl azine ligand with a free amine (NH 2 ) group. The reaction of [Cp*RhCl 2 ] 2  with ligand ( L ) formed a cationic complex with the formula [Rh III (η 5 -C 5 Me 5 )( L )к 2(N,N’) Cl]SbF 6  ( 1 ) that was characterized by IR, UV-Vis,  1 H,  13 C{ 1 H} NMR,  etc . The SC-XRD analysis of the complex revealed the condensation of an acetone molecule with the azine NH 2  group, thus forming an imine –C=N– bond in the ligand, giving [Rh III (η 5 -C 5 Me 5 )( L’ )к 2(N,N’) Cl]SbF 6  ( 2 ). The coordination geometry around rhodium in  2  is pseudo-tetrahedral with coordination sites occupied by a Cp* moiety in an η 5  manner, a terminal chloride, and a pyridyl azine ligand in a bidentate N,N’ fashion through N (pyridine)  and N (azine)  nitrogen atoms occupying the four vertices of the tetrahedron. The crystal packing is mainly directed by moderate and weak hydrogen bonds including C–H⋯F, C–H⋯Cl, N–H⋯Cl and C–H⋯N interactions. The overall crystal packing and the significant role of hydrogen bonding in the supramolecular assembly has been discussed by performing Atoms-In-Molecules (AIM) and Natural Bond Orbital (NBO) analyses.

Synthesis, crystal structure and hydrogen bonding of a Cp*Rh(III) complex bearing pyridyl azine ligands: a combined experimental and DFT approach