A　polyoxovanadium　borate　(H2dap)6H[V12B16O54(OH)4]·12H2O(dap=1,2-diaminopropane)　with　novel　structure　was　hydrothermally　synthesized　and　characterized　by　the　single　crystal　X-ray　diffraction.　It　crystallizes　in　triclinic　system　with　space　group　Pīand　unit　cell　parameters　a=19.027(4),　b=16.142(3)　Å,　c=26.679(5)　Å,　α=90°,　β=101.06(3)　°,　γ=90°,　V=8042(3)　Å3,　Z=4,　Dc=1.962　g·cm-3,　μ=1.456　mm-1,　F(000)=4　776,　the　final　R1=0.062　6,　wR2=0.192　7,　S=1.　003,　for　7　635　observed　reflectionswith　I>2σ(I).　It　is　showed　that　the　compound　1　is　composed　of　V12B16　clusters　unit　and　dap　which　is　as　a　counter　ion,　and　a　two-dimensional　layered　structure　is　obtained　by　the　effect　of　hydrogen　bonding　between　the　cluster　units　and　dap,　and　between　the　layers　via　strong　hydrogen　bonds　to　form　a　three-dimensional　supramolecular　structure.　The　compound　1　were　also　characterized　by　IR,　two-dimensional　infrared　(2D　IR)　correlation　spectroscopy　with　magnetic　and　thermal　perturbation,　UV/Vis　DRS　spectra.　The　relationship　between　the　structure　and　spectroscopy　properties　was　discussed.　The　IR　spectrum　showed　that　the　antisymmetric　stretching　vibration　absorption　peak　νas(V-Oμ)　and　symmetric　stretching　vibration　absorption　peaks　νs(V-Oμ)　appeared　at　775　and　683　cm-1　respectively,　whereas　the　vibration　absorption　peak　in　ν(B-O)　of　BO3　and　the　vibration　absorption　peak　in　ν(B-O)　of　BO4　appeared　at　1　350　and　1　050　cm-1　respectively.　The　response　of　the　stretching　vibrations　of　B-O　and　V-O　was　detected　in　the　2D　IR　correlation　spectra　with　magentic　perturba-tion.　In　addition,　the　response　of　the　stretching　vibrations　of　B-OH,　B-O　and　V-O-V　was　detected　in　the　2D　IR　correlation　spectra　with　thermal　perturbation.　©　2015,　Science　Press.　All　right　reserved.