Two different 2D layered metal–organic frameworks (MOFs) have been prepared using a hexanuclear manganese metallamacrocycle and an octanuclear manganese metallamacrocycle as supramolecular building blocks viaa simple change of the solvent used and/or addition of a templating agent. While the sheets in the 2D MOF [Mn6(pshz)6(bpea)2(dma)2]n, 2(where, pshz3−is N-propionylsalicylhydrazidate, bpea is 1,2-bis(pyridyl)ethane, and dma is N,N-dimethylacetamide), built based on a hexanuclear metalladiazamacrocycle are in a staggered orientation, the sheets in the 2D MOF [Mn8(pshz)8(bpea)2(dma)4]n, 3, built based on an octanuclear metalladiazamacrocycle are in an eclipsed orientation. However, both MOFs have the same 3-connected 4.82network topology. [ABSTRACT FROM AUTHOR]