New phosphates Ca9–xPbxEu(PO4)7 were obtained by solid state reaction techniques at 1213–1253 K in air atmosphere and were found to be isotypic with whitlockite-type β-Ca3(PO4)2. The unit cell parameters were determinate using Le Bail decomposition. Rietveld method structural refining showed that Eu3+ ions are located statistically with calcium in M1, M2, and M3 sites, whereas Pb2+-ions are preferentially located in the M3. Examination of optical second harmonic generation evidences nonlinear optical activity and confirms polar space group R3c.
