pH-Variable hydrothermal reactions of Pb(II) with dicarboxylic acids in the presence of 1,10-phenanthroline led to new solid-state compounds [Pb2(C12H8N2)4(C4H2O4)](NO3)2 (1),[Pb2(C12H8N2)4(CO3)(C4H2O4)]n.6nH2O (2), [Pb2(C12H8N2)(C4H2O4)2]n (3), and [Pb(C12H8N2)(C4H2O4)]n .2nH2O (4). All compounds were characterized by elemental analysis, FT-IR, CP-MAS-NMR, and single crystal X-ray diffraction. The collective chemical reactivity in the ternary Pb(II)-phenanthroline-dicarboxylate systems unravels seldom seen metal-assisted ligand malate/maleate to fumarate transformations, which in the presence of Pb(II) and 1,10-phenanthroline contribute to the assembly of 2D (2) and 3D lattice networks (3-4). All distinct assemblies in 1-4 reveal interwoven crystal lattice connections, reflecting unique physicochemical properties.