A new family of 3D heterometallic 3d-4f organodisulfonate complexes based on the linkages of 2D [Ln(nds)(H2O)]+ layers and [Cu(ina)2]− chainsElectronic supplementary information (ESI) available: Further characterisation data. CCDC reference numbers 768850, 768848, 772500, 768851, 768853, 768854, 768849. For ESI and crystallographic data in CIF or other electronic format see DOI: 10.1039/c0ce00077a

Seven novel 3D heterometallic coordination compounds, LnCu(nds)(ina) 2 ·H 2 O [Ln = Eu ( 1 ), Ce ( 2 ), Er ( 3 ), Gd ( 4 ), Sm ( 5 ), Tb( 6 ), Dy( 7 ); nds = 2,6-naphthanlenedisulfonate; ina = isonicotinic acid], have been synthesized under hydrothermal conditions and characterized by elemental analysis, infrared spectra, thermogravimetric analysis and single-crystal X-ray diffraction analysis. These compounds are isostructural and constructed by the linkages of 2D [Ln(nds)(H 2 O)] + layers and Cu(ina) 2 − chains, which represent the first examples of 3D heterometallic coordination polymers created by the organodisulfonate ligands. Moreover, the complexes exhibit a novel (3,6)-connected net. The luminescence properties of complexes 1 , 5 and 6 and the magnetic property of 4 were also investigated. Seven novel 3D heterometallic coordination compounds have been synthesized under hydrothermal conditions and characterized by elemental analysis, infrared spectra, thermogravimetric analysis and single-crystal X-ray diffraction analysis.