Porous coordination polymers are unique in terms of their good crystallinity, designable porosity and structural flexibility and play an important role in numerous application areas including gas storage, selective adsorption/separation, catalysis, luminescence, sensing, drug delivery, etc [1]. Being in line with these investigations we report herein the products of interaction of Co(II) or Zn(II) tetrafluoroborate with or 1,2-bis(4-pyridyl)propane (bpp) in the presence of 1,3,5-benzenetricarboxylic acid (H3btc) which represent two novel polymeric compounds with the compositions {[Co4( μ 3-OH)2(btc)2(H2О)8]·4H2O}n (1) and {[Zn4(bpp)4(Hbtc)3((Me)btc)]·2(Me)2Hbtc·2H2O}n (2). These materials were obtained in similar solvo-thermal synthesis conditions and were characterized by single crystal X-ray method. Both compounds crystallize in centrosymmetric space groups: triclinic P-1, a=7.7923(9), b=8.7102(7), c=10.7369(11) Å, α=101.043(8), β=92.284(9), γ=95.237(7)° for 1; orthorhombic Cmcm, a=35.555(2), b=14.9805(10), c=19.9824(6) Å for 2. The structural determination revealed that the coordination geometries around the metal centers are distorted octahedral for Co(II) and tetrahedral for Zn(II). Compound 1 consists of a tetranuclear Co4(μ3-OH)2 cores bridged by btc3- anions and are assembled to form a 2D coordination layer with Co···Co separations equal to 7.905 and 11.144 Å. In compound 2 each Zn(II) cation coordinates two bridging bidentate Hbtc2- anions or one Hbtc2- and one (Me)btc2- anions and two neutral double-stranded bridge fashion bpp molecules with Zn···Zn separation of 11.677 Å, which are then linked by Hbtc2- anions in a quadruple-stranded fashion with Zn···Zn separations equal to 8.305 and 10.585 Å with the formation of 1D ladder coordination polymer.