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d-Block transition metal(II)-lanthanide(III) (3d-4f) hetero‐trinuclear [Cu(II) 2 Ln(III)] (Ln = La and Ce) complexes [Cu 2 La(L)( ƞ2 -NO 3 ) 3 (CH 3 OH) 2 ]·2CH 3 OH ( 1 ) and [Cu 2 Ce(L)( ƞ2 -NO 3 ) 3 (CH 3 OH) 2 ]·2CH 3 OH ( 2 ) are described, both of which are formed by a flexible symmetrical bis(salamo)-type ligand H 4 L. The two 3d-4f complexes have been synthesized and characterized by elemental analyses, IR spectra and UV–Vis spectroscopy. The crystal structures of  1  and  2  were determined by single-crystal X-ray diffraction analyses. In  1  and  2 , each Cu(II) ion (Cu1 or Cu2) is located in the N 2 O 2  cavity of an (L) 4−  unit, while the apex is occupied by one oxygen atom of the coordinated methanol molecule, forming a penta-coordinated square pyramidal geometry. The lanthanide(III) (La or Ce) ion is located in the O 6 -donor coordination sphere of the completely deprotonated (L) 4−  unit and coordinated with the other six oxygen atoms of the three nitrate ligands to form a twelve-coordinated icosahedron. At the same time, the supramolecular structures are formed by intermolecular hydrogen bonding interactions and quantitatively determined by Hirshfeld surfaces analyses. Fluorescence properties and DFT calculations of  1  and  2  were also studied.

Coordination-driven self-assemblies of two hetero‐trinuclear [Cu(II) 2 Ln(III)] (Ln = La and Ce) complexes with a flexible bis(salamo)‐type ligand