A　novel　polyoxometalate　(POM)　Na-2(H(2)en)(2){(VO)(10)[B14O30(OH)(2)](2)}　{Mn-4(C2O4)　[B2O4(OH)(2)](2)}Mn(H2O)(2)center　dot(H3O)(12)(H2O)(19)　1　(en　=　ethylenediamine),　which　is　a　layer-like　transition　metal　(TM)　oxalate　templated　polyoxovanadium　borate,　has　been　synthesized　under　hydrothermal　conditions　and　characterized　by　EPR,　elemental　analysis,　thermal　analysis,　single　crystal　X-ray　diffraction　and　2D　IR　correlation　spectroscopy　studies,　respectively.　This　compound　crystallized　in　the　triclinic　space　group　P1　with　a　=　14.3842(4)　angstrom,　b　=　14.6837(3)　angstrom,　c　=　15.8681(4)　angstrom,　a　=　64.48(1)degrees,　beta　=　64.68(1)degrees,　gamma　=　63.93(1)degrees,　V　=　2596.80(11)　angstrom(3)　and　Z　=　2.　The　cluster　anion　with　an　open　central　cavity　has　a　central　band　of　ten　edge-sharing　VO5　square　pyramids,　which　is　capped　top　and　bottom　by　two　crown-like　polyborate　ligands　of　formula　[B14O30(OH)(2)](20-).　There　is　a　fragment　of　{Mn-4(C2O4)[B2O4(OH)(2)](2)}(2-)　fixed　in　the　central　cavity　as　a　guest　part.　The　cluster　units　are　connected　to　form　a　two-dimensional　(2D)　framework　by　octahedral　Mn(II)　and　Na+　sites.　In　addition,　we　first　introduce　the　generalized　2D　correlation　spectroscopy　to　explore　the　POMs　and　obtain　the　dynamic　information　about　structural　changes　of　POMs.　(c)　2005　Elsevier　Inc.　All　rights　reserved.