Two novel lanthanide-sulfate compounds, [Ln2(SO4)3(H2O)8] (Ln = Tb (1) and Dy (2)), have been synthesized under hydrothermal reactions. X-ray crystal structure analyses reveal that 1 and 2 are isomorphous and crystallize in monoclinic C2/c pace group, showing a layered structure. The layers bear a rare quasi-honeycomb metal arrangement, which is fastened by μ3= η1:η1:η1and μ2= η1:η1sulfates. If assigning the μ3= η1:η1:η1sulfate as a 3-connected node and the Ln3+ion as a 4-connected node, the network can be rationalized as a binodal (3,4)-connected V2O5topology with a Schäfli symbol of (42·63·8) (42·6). In addition, the infrared, thermogravimetric analysis and luminescent properties were also studied. Complexes 1 and 2 exhibit outstanding thermal stability and characteristic terbium and dysprosium luminescence.
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