The framework gallium diphosphonates Ga2[O3PC2H4PO3](H2O)2F2·2H2O (1) (triclinic, P1̄, a = 5.0432(2) Å, b = 7.2468(3) Å, c = 8.3499(4) Å, α = 107.489(2)°, β = 92.444(2)°, γ = 109.338(2)°, Z = 1) and Ga2[O3PCH2(C6H4)CH2PO3](H2O)2F2 (2) (triclinic, P1̄, a = 4. 9673(1) Å, b = 7. 0898(2) Å, c = 10. 1220(3) Å, α = 92. 698(2)°, β = 93.153(2)°, γ = 109. 122(2)°, Z = 1) and the solid-solution series Ga2{[O3PCH2(C6H4)CH2PO3]1 - x (HPO3)2 x }(H2O)2F2 (0 ≤ x ≤ 0.146) x = 0.541 (3) and x = 0.144 Ga2{[O3PCH2(C6H4)CH2PO3]0.853(6)(HPO3)0.29(1)}(H2O)2F2 (4) (triclinic, P1̄, a = 4.959(2) Å, b = 7.078(2) Å, c = 10.024(3) Å, α = 92.404(5)°, β = 92.955(5)°, γ = 109.187(5)°, Z = 1) have been synthesized by solvothermal methods and their structures determined using X-ray diffraction data. All the materials contain linear chains of corner-sharing GaO4F2 octahedra that are linked by the diphosphonate groups to form framework structures. The channels of 1 are found to contain two water molecules per unit cell while those in 2 are too narrow to contain extraframework species. The apertures created in the phosphite-substituted derivatives of 2 (3 and 4) are shown, by crystallographic methods, to be considerably larger than those in 2 and, by thermogravimetric methods, to create more open structures. The synthetic conditions or form of the diphosphonate group are found to play a defining role in the adoption of this particular configuration of the inorganic component in the reported compounds and provide an additional strategy for the rational design of framework hybrid organic−inorganic solids.
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