Published online by Cambridge University Press: 03 April 2012
Methods of chemical preparation and XRD data are reported for four cyclotriphosphates associated with barium alone and with ammonium and thallium. These phosphates are Ba3(P3O9)2·4H2O, BaNH4P3O9·2H2O, BaTlP3O9·2H2O, and BaTlP3O9·Ba3(P3O9)2·4H2O was prepared by the direct method of chlorures, BaNH4P3O9·2H2O and BaTlP3O9·2H2O by the method of ion-exchange resin, and BaTlP3O9 by total dehydration of BaTlP3O9·2H2O. Ba3(P3O9)2·4H2O is monoclinic, space group P21/n, Z = 4, with a = 7.546(3), b = 12.105(4), c = 11.649(4) Å, β = 100.340(3)°, V = 1046.8(2) Å3, M(20) = 81, and F(20) = 117(0.003 419, 50). BaNH4P3O9·2H2O is monoclinic, space group P21/n, Z = 4, with a = 7.547(1), b = 12.065(1), c = 11.697(1) Å, β = 101.111(1)°, V = 1045.1(3) Å3, M(20) = 9 (AV.EPS = 0.000 116 9), and F(20) = 14(0.0287 06, 53). BaTlP3O9·2H2O is monoclinic, space group P21/n, Z = 4, with a = 7.546(3), b = 12.105(4), c = 11.649(4) Å, β = 100.340(3)°, V = 1046.8(2) Å3, M(20) = 81, and F(20) = 117(0.003 419, 50). BaNH4P3O9·2H2O and BaTlP3O9·2H2O are isostructural. BaTlP3O9 is orthorhombic, space group P212121, Z = 4, with a = 11.086(2), b = 12.283(2), c = 5.786(1) Å, V = 787.9(4) Å3, M(20) = 10 (AV.EPS = 0.000 116 9), and F(20) = 14(0.026 955, 56).