Methods of chemical preparation and XRD data are reported for a new triphosphate CuNa3P3O10 and two cyclotriphosphates SrRbP3O9·3H2O and SrRbP3O9. SrRbP3O9·3H2O was prepared by the method of ion-exchange resin, while CuNa3P3O10 and SrRbP3O9 were obtained by total dehydration of CuNa3P3O10·12H2O and SrRbP3O9·3H2O, respectively. CuNa3P3O10 crystallizes in the hexagonal system, with space group P-31c, Z=2, and the following unit-cell dimensions: a=b=7.022(1) Å, c=9.217(1) Å, M(20)=81, F(20)=117(0.003 419, 50), and V=393.24(2) Å3. SrRbP3O9·3H2O is orthorhombic, with Z=4, space group Pnma, and the following unit-cell dimensions: a=9.120(1) Å, b=8.141(1) Å, c=15.234(1) Å, M(20)=5.1, F(20)=5.8(0.0173,199), and V=1131.1(3) Å3. SrRbP3O9 is monoclinic, with space group P21/m or P21, Z=4, and the following unit-cell dimensions: a=14.958(3) Å, b=8.503(2) Å, c=7.898(2) Å, β=122.19(2)°, M(20)=9.9, F(20)=16.5(0.0189, 64), and V=850.2(8) Å3.
