The coordination-driven self-assembly of a series of discrete 2D metallomacrocycles from a rigid
diphosphine donor linker and Pd/Pt-containing 90° acceptors is described. All these assemblies are
characterized by multinuclear NMR and, in four cases, X-ray crystallography. The selective formation
of a diphosphine bridged macrocycle, [(en)Pd(μ-trans-PPh2CHCHPPh2)2Pd(en)]4+, from a 1:1:1 mixture
of cis-Pd(en)(NO3)2, trans-Ph2PCHCHPPh2, and 1,2-bis(4-pyridyl)ethane is also established