Compounds 1 and 2 both contain the same 2D corrugated layers bridged by DAMwith different bridging modes to form different 3D structures, exhibiting tcs and (4,6)connected topologies, respectively. The structural differences of 1 and 2 lie in the linkages of DAMbetween the layers. Compound 3 also possesses a 3D architecture with an ant net, which is pillared by 2D (4,4) fan-shaped layers in an -ABABsequence. Compounds 4-6 contain similar 2D layers to 1 and 2. The analogous cationic structures 4 and 5 show a 4-connected sql net and 6 presents a (4,5)-connected network, resulting from the different modes of flag-like DAMabove and below the layers. Compound 7 with identical molecular formula to 6 displays a 2D double-layer, consisting of a couple of (4,4) rectangular grid layers. It exhibits a (3,6)connected network. Additionally, IR and UV-visible spectroscopy, the luminescent properties, and thermogravimetric analyses are discussed.

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