The reaction of M(NO 3 ) 2 ·6H 2 O (M=Co or Ni), N,N-diethyl-ethylenediamine (deen) and sodium dicyanamide (dca) afforded the complex {[M(deen)(μ 1,5 -dca) 2 ]} n (where for 1, M=Co and for 2, M=Ni). The complexes have been characterized structurally and magnetically. X-ray analysis reveals that the isomorphous complexes 1 and 2 feature similar infinite three-dimensional scaffolding-like structure to generate the fascinating molecular assembly. All the {N(CN) 2 } − ligands present in the complexes are connected to the symmetry related metal centers in an end-to-end fashion through bent {N(CN) 2 } − ligands. The zigzag linkage propagates parallel to three crystallographic axes to form a fully interlocked 3D structure. The variable temperature (4–300K) magnetic susceptibility measurements showed that the magnetic interaction between the metal centers in the complex 1 is dominantly antiferromagnetic. However, the compound 2 is a simple paramagnet. The N 2 sorption analysis reveals that the complexes 1 and 2 are porous.