A new Gd 26 cluster based 3D framework, {[Gd 26 (μ 6 -CO 3 ) 9 -(NIC) 32 (μ 3 -OH) 26 ](NO 3 ) 2 ·3(H 2 O)} n (1) (NIC = nicotinato anion) has been prepared through hydrothermal synthesis and characterised by single-crystal X-ray diffraction. The Gd 26 clusters are formed by the combination of five distorted cubane cores attached to each other through six Gd 3+ ions.