Syntheses and Crystal Structures of the Cyclotriphosphate Hydrates Nd(P3O9)·3H2O, Nd(P3O9)·4.5H2O, RE(P3O9)·5H2O (RE = Pr, Nd), and Na3RE(P3O9)2·6H2O (RE = Pr, Nd)

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Abstract

Several rare-earth cyclotriphosphate hydrates were obtained from mixtures of sodium cyclotriphosphates and the respective rare-earth chlorides. Nd(P3O9)·3H2O [Pequation image, Z = 3, a = 677.90(9), c = 608.67(9) pm, R1 = 0.016, wR2 = 0.038, 312 data, 36 parameters] was obtained by a solid state reaction and is isotypic with respective rare-earth phosphate hydrates, while all the others adopt new structure types. Nd(P3O9)·4.5H2O [C2/c, Z = 8, a = 1644.6(3), b = 756.11(15), c = 1856.1(4) pm, β = 97.25(3)°, R1 = 0.032, wR2 = 0.081, 1763 data, 194 parameters], Nd(P3O9)·5H2O [P21/c, Z = 4, a = 773.75(15), b = 1149.1(2), c = 1394.9(3) pm, β = 106.07(3)°, R1 = 0.042, wR2 = 0.082, 1338 data, 194 parameters], Pr(P3O9)·5H2O [Pequation image, Z = 2, a = 745.64(15), b = 889.07(18), c = 934.55(19) pm, α = 79.00(3), β = 80.25(3), γ = 66.48(3), R1 = 0.059, wR2 = 0.089, 1468 data, 193 parameters], Na3Nd(P3O9)2·6H2O [P21/n, Z = 4, a = 1059.78(18), b = 1207.25(15), c = 1645.7(4) pm, β = 99.742(17), R1 = 0.047, wR2 = 0.119, 1109 data, 351 parameters] and Na3Pr(P3O9)2·6H2O [P21/n, Z = 4, a = 1061.42(16), b = 1209.0(2), c = 1635.5(3) pm, β = 99.841(13), R1 = 0.035, wR2 = 0.062, 1323 data, 350 parameters] were obtained by careful crystallization at room temperature. A thorough structure discussion is given. The infrared spectrum of Nd(P3O9)·4.5H2O is also reported.

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