A　novel　three-dimensional　compound　of　Na4Sb12Mo5O35　has　been　synthesized　by　hydrothermal　methods　and　structurally　characterized　by　X-ray　crystallography.　It　crystallizes　in　the　triclinic　system　T　ace　group　PI　with　a　=　11.574(2)　angstrom,　b　=　12.594(3)　angstrom,　c　=　13.277(3)　angstrom,　alpha　=　94.59(3)degrees,　beta　=　112.68(3)degrees,　gamma　=　92.97(3)degrees,　V　=　1772.7(6)　angstrom(3),　Z　=　2,　R-1　=　0.0275,　wR(2)　=　0.0984　for　7364　unique　reflections　with　I　＞　2　sigma(I).　The　molecular　structure　is　built　up　of　Mo6O21,　MoO4　units,　and　cage-like　units　that　contain　12　Sb　atoms.　IR,　UV-Vis　DRIS　(Ultraviolet-Visible　Diffuse　Reflection　Integral　Spectrum),　fluorescent　spectra,　and　the　thermogravimetric　analysis　of　this　compound　were　investigated.　(c)　2005　Elsevier　Inc.　All　rights　reserved.