The crystal structures of hexa-&mgr;-propionato-1:2kappa(6)O:O';1:3kappa(6)O:O'-diquinoline-2ka ppaN,3kappaN-calcium(II)dizinc(II), [CaZn(2)(C(3)H(5)O(2))(6)(C(9)H(7)N)(2)], and hexa-&mgr;-pivalato-1:2kappa(6)O:O';1:3kappa(6)O:O'-diquinoline-2kapp aN,3kappaN-calcium(II)dicobalt(II), [CaCo(2)(C(5)H(9)O(2))(6)(C(9)H(7)N)(2)], are described. Both contain a linear array of one Ca(II) ion and two M(II) (M = Zn, Co) ions connected by two sets of three carboxylate ligands in syn-syn bridging modes. The distorted tetrahedral geometry around the M(II) ion is completed by a quinoline N atom. The central Ca(II) ion occupies a crystallographic inversion centre and is octahedrally coordinated by six carboxyl O atoms in each structure. The Zn(II). Ca(II) and Co(II).Ca(II) distances are 3.8504 (9) and 3.7929 (5) A, respectively.