Mn(H 2 dapsox)Cl(H 2 O)]ClÁH 2 O (1) and [Zn(H 2 dapsox)-(H 2 O) 2 ]Cl 2 ÁH 2 O (2) were synthesized from 2,6-diacetylpyridine (dap), oxamic acid hydrazide (sox) and MnCl 2 Á4H 2 O or ZnCl 2 Á2H 2 O in 1:2:1 molar ratio, employing a template approach. Based on elemental analyses, molar conductivity and magnetic susceptibility data, IR, 1 H and 13 C NMR and EA spectra, as well as thermal analyses (DSC and TG), a pentagonal-bipyramidal (PBP) geometry for the complexes was determined. Symmetrically coordinated 2 H ,2 HHH -(2,6-pyridindiyldiethylidene)dioxamohydrazide (H 2 dapsox) is located as a pentadentate ligand in the equatorial plane. The stability of the 3d metal complexes having the PBP geometry is Downloaded by [University of Western Ontario] at 03:41 06 February 2015 discussed. It was found that Co(II) and Mn(II) produce the most stable complexes of this type, while the Zn(II) complex of the same geometry is much less stable. White 61 29.76 4.09 18.63 (29.82 4.04 18.72) 3545 m, 3338 vs, 3240 vs, 3158 vs, 1719 vs, 1684 vs, 1666 vs, 1591 vs, 1520 vs, 1460 m, 1435 s, 1409 vs, 1386 vs, 1374 vs, 1321 m, 1271 vs, 1210 vs, 1176 s, 1103 m, 1076 m, 1020 m, 1003 w, 933 w, 825 m, 803 m, 768 w, 743 m, 672 vs, 562 m, 513 m, 496 m, 445 m, 428 w 145.0 724 SUMAR ET AL.