Three isomeric ligands, and four d10 metal CPs were synthesized, varying from 1D to 2D, together with achirality to chirality variation.

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Two new metal complexes, {[Cd2(μ2‐H2pdc)2(H2O)8]·[Cd2(H2pdc)4(H2O)2(μ2‐Cl)2]}·2H2O (1), and [Ba2(H2pdc)4(H2O)8]·2H2O (2) (H3pdc = 3, 4‐pyrazoledicarboxylic acid), were synthesized and characterized by elemental analysis, IR spectroscopy, and single‐crystal X‐ray diffraction. The crystal structures show that compound 1 is an independent unit consisting of two discrete dinuclear complex ions [Cd2(μ2‐H2pdc)2(H2O)8]2+ cation and [Cd2(H2pdc)4(H2O)2(μ2‐Cl)2]2– anion, and the two kinds of ions are linked by hydrogen bonds and electrostatic interactions to generate a 3D supramolecular network. Complex 2 is a common dinuclear structure, which is further assembled to a 3D supramolecular network through intermolecular hydrogen bonds and π–π stacks. The hydrogen bonding interactions involving lattice water or coordinated water molecules all exist in complexes 1 and 2. Notably, three coordination modes of 3, 4‐pyrazoledicarboxylic acid were observed. The thermal and photoluminescent properties of complexes 1 and 2 in the solid state were also investigated.

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Reaction of H2L1/H2L2/H2L3 with corresponding main group metal salts generated five complexes, [Mg(L1)(phen)(H2O)3]⋅5H2O (1, mononuclear), [Sr(CH3OH)(L1)2Sr(H2O)2]2n⋅nH2O (2, 2D), [Ba(L2)(H2O)3]n (3, 2D), [Pb(L2)(2,2′‐bpy)]2n⋅9nH2O (4, 1D) and [Pb(L3)(phen)]2⋅2DMF (5, dinuclear) (H2L1=1,1'‐methylenebis(5‐methyl‐pyrazole‐4‐carboxylic acid, H2L2 = 2'‐methylenebis(3‐methyl‐pyrazole‐4‐carboxylic acid, H2L3=1,1'‐methylenebis(3‐methyl‐pyrazole‐4‐carboxylic acid; 2,2’‐bpy=2,2′‐bpyridine and phen=1,10‐phenanthroline). In the zwitterionic complex 1, a loop‐loop water‐water hydrogen bonded chain presented in the 3D supramolecular network, which was constructed by π⋅⋅⋅π interactions and hydrogen bonds. In CPs 2 and 3, the 1D inorganic M–O–M connectivity was built from Sr2O16 and BaO9 polyhedra, respectively. The similar 24‐membered Pb2(L2)2/Pb2(L3)2 macrocycle occurred in both 1D polymer 4 and dinuclear complex 5, with two 2,2’‐bpy molecules located inside or two phen molecules outside each macrocycle respectively. The thermal and photoluminescent properties of 1–5 in the solid state have also been investigated.