Four　divalent　transition　metal　carboxyarylphosphonates,　[Ni(4,4′-bipy)H2L1(HL1)2(H2O)2]·2H2O　1,　[Ni2(4,4′-bipy)(L2)(OH)(H2O)2]·3H2O　2,　Mn(phen)2(H2L1)2　3　and　Mn(phen)(HL2)　4　(H3L1=p-H2O3PCH2-C6H4-COOH,　H3L2=m-H2O3PCH2-C6H4-COOH,　4,4′-bipy=4,4′-bipyridine,　phen=1,10-phenanthroline)　were　synthesized　under　hydrothermal　conditions.　1　features　1D　linear　chains　built　from　Ni(II)　ions　bridging　4,4′-bipy.　In　2,　neighboring　Ni4　cluster　units　are　connected　by　pairs　of　H3L2　ligands　to　form　1D　double-crankshaft　chains,　which　are　interconnected　by　pairs　of　4,4′-bipy　into　2D　sheets.　3　exhibits　2D　supramolecular　layers　via　the　R22(8)　ringed　hydrogen　bonding　units.　4　has　1D　ladderlike　chains,　in　which　the　4-membered　rings　are　cross-linked　by　the　organic　moieties　of　the　H3L2　ligands.　Additionally,　2D　FTIR　correlation　analysis　is　applied　with　thermal　and　magnetic　perturbation　to　clarify　the　structural　changes　of　functional　groups　from　H3L1　and　H3L2　ligands　in　the　compounds　more　efficiently.　©　2010　Elsevier　Inc.　All　rights　reserved.