Four novel hybrid d10 metal complexes [Zn(H2MDIP)(4,4′-bpy)0.5]n1
(4,4′-bpy = 4,4′-bipyridine, H4MDIP = methylenediisophthalic acid), [Zn2(MDIP)(bix)·H2O]n2
[bix = 1,4-bis(imidazol-1-ylmethyl)-benzene], {[Cd(H2MDIP)(H2O)]2·H2O}n3, {[Cd2(MDIP)(H2O)2(en)2]·2H2O}n4
(en = ethylenediamine) based on tetracarboxylate acid were synthesized and their structures were determined by X-ray single-crystal diffraction. Complexes 1–2 are 2D grid and undulated structures with four-coordinated Zn2+ ions, respectively; 3–4 are 2D grid and double-sheet structures with six-coordinated Cd2+ ions, respectively. MDIP in complexes 1 and 3 act as V-shaped and Y-shaped ligands, respectively, yet in 2 and 4 MDIP act as similar X-shaped ligands. Diverse topologies, thermal and luminescent properties of complexes 1–4 have also been investigated.