Metal-organic frameworks are coordination polymers comprised of rigid organic linkers bearing coordinating functional groups connected by inorganic nodes. This class of compounds has numerous applications ranging from gas storage/separation, catalysis, luminescence, chemical sensing and even drug delivery. Three new coordination polymers have been prepared using the rigid ligand 2',3',5',6'tetramethyl-[1,1',4',1''-terphenyl]-4,4''-dicarboxylate and La(III), Nd(III)and Ho(III) under solvothermal conditions. Single-crystal X-ray diffraction has shown that these isoreticular coordination polymers are non-interpenetrated, tightly packed 3D metal-organic networks. The complexes exhibited an excellent thermal stability, as revealed by thermogravimetric analysis. IR spectroscopy, energy dispersive X-ray analysis and powder X-ray diffraction were used to further characterize the hybrid networks. In addition, the specific surface area was determined bynitrogen adsorption measurements. The luminescent properties of these coordination polymers were also evaluated.