A new phase of the compound PbBiBO(4) has been successfully synthesized via the standard solid-state reaction, and the crystal structure has been determined from X-ray monocrystal diffraction data. It crystallizes in orthorhombic space group Cmca (No. 64) with lattice constants a = 10.782(3) angstrom, b = 10.502(3) angstrom, c = 7.477(2) angstrom, Z = 8. The crystal structure is characterized by a three-dimensional structure consisting of BiO(6) octahedra, PbO(4) tetrahedra and BO(3) triangles. The BiO(6) octahedra compose the layers through the O(2) atoms and O(3) atoms along the 101 direction, which connects the BO(3) trigonal groups by sharing the O(3) and two O(1) atoms and links the PbO(4) tetrahedra through the O(2) atoms. The UV-Vis-NIR Diffuse-Reflectance spectrum shows that the ultraviolet cutoff edge for the PbBiBO(4) crystal is about 310 nm. Functional groups in the sample were identified by Infrared spectrum.