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Four metal phosphites/phosphates crystal materials C₈N₄H₃₄Al₂P₄O₁₈ (1), C₃N₂H₁₇GaP₂O₈ (2), H₅In₂P₃O₁₀ (3), and H₉In₂P₃O₁₃ (4) have been solvothermally synthesized by organic amines in the presence of mixed solvents. Structural analyses indicate that compound 1 and 2 show one-dimensional (1D) chain structures; compound 3 and 4 are three-dimensional (3D) inorganic open-framework indium phosphites. Organic amines show different mechanisms in the four compounds. The 2,2′-bipyridine organic amine acts as a template source and it breaks down small molecules, which enter into the structure of compound 1. For compound 2, 1,2-propanediamine has a role as protonated template and it forms a hydrogen bond with the inorganic skeleton structure. As for compound 3 and 4 without the organic template, the benzylamine and 2,2′-bipyridine mainly serve as structure-directing agent. Especially, compound 3 has an odd seven-ring channel, and compound 4 contains 3D intersecting six-ring, eight-ring, and 10-ring channels. X-ray diffraction (XRD), scanning electron microscopy (SEM), CHN, inductive coupled plasma (ICP), Infrared (IR), and thermal gravimetric (TG) analyze the four compounds.