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Two new phosphate compounds, KNiPO4·6H2O and NaNiPO4·7H2O, have been synthesized, identified and their crystal structure studied by powder X‐ray diffraction. KNiPO4·6H2O crystallizes in the monoclinic system, with lattice parameters a= 6.8309(3) Å, b= 11.0610(4) Å, c= 6.1165(2) Å, and angle β= 91.045(2)°, volume of the unit cell V= 462.07(3) Å3, space group P21, and Z = 2, while NaNiPO4·7H2O does so in the tetragonal system with a= 6.7390(2) Å, c= 10.9690(4) Å, V= 498.15(4) Å3, space group P42/mmc, and Z = 2. KNiPO4·6H2O has the structure as the struvite analogue KMgPO4·6H2O, whereas NaNiPO4·7H2O is isostructural with the compound NaMgPO4·7H2O. Neither material presents a magnetic order in the range of temperatures measured from 300 K down to 1.8 K.