The two coordination polymers [Ni(ndc)(lutidine)(2)(H2O)(2)], CPO-3, and [Ni-3(ndc)(3)(pyridine)(4)], CPO-4, were obtained by hydrothermal reactions between 2,6-naphthalenedicarboxylic acid (ndc), 3,4-lutidine and nickel(II) nitrate (CPO-3) and ndc, pyridine and nickel(II) nitrate (CPO-4), respectively. In CPO-3, the combination of octahedral nickel(II) ions and ndc ligands leads to the formation of infinite chains. CPO-4 is based on linear trinuclear building units of octahedral nickel(II) ions that are crosslinked via the ndc ligands to form a 3D-structure. The crystal structure of CPO-3 was solved from synchrotron powder X-ray data, while the crystal structure of CPO-4 was solved from conventional single-crystal X-ray data. Crystal data for CPO-3: monoclinic space group Cc (No. 9), a = 14.8583(2), b = 20.3985(3), c = 10.7258(1) Angstrom, beta = 129.0067(6)degrees, V = 2526.14(5) Angstrom(3) and Z = 4. Crystal data for CPO-4: monoclinic space group P2(1)/c (No. 14), a = 11.491(3), b = 17.917(4), c = 12.781(3) Angstrom, beta = 116.142(7)degrees, V = 2362.2(9) Angstrom(3) and Z = 2. The thermal and magnetic properties of both compounds were investigated. (C) 2003 Editions scientifiques et medicales Elsevier SAS. All rights reserved.