Mrak Maja, Kolitsch Uwe, Lengauer Christian, Kaucic Venceslav, Tillmanns Ekkehart
Institut für Mineralogie und Kristallographie, Universität Wien, Geozentrum, Althanstrasse 14, A-1090 Vienna, Austria.
Inorg Chem. 2003 Jan 27;42(2):598-604. doi: 10.1021/ic025663r.
Two new layered gallophosphate-oxalate materials have been prepared hydrothermally using ethylenediamine and oxalic acid as structure-directing agents. The compounds (C2N2H10)2[Ga2(C2O4)2(HPO4)3].H2O 1 and (C2N2H10)3- [Ga4(C2O4)4(HPO4)4(H2PO4)2] 2 are closely related, consisting of anionic double chains built of alternating paris of GaO6 and HPO4 polyhedra. These double chains are linked via bridging HPO4 or H2PO4 tetrahedra to form corrugated layers containing eight-membered rings. The oxalate group acts as a bidentate ligand to each of the GaO6 octahedron. The corrugated layers are held together by strong to weak hydrogen-bonding interactions between oxalate groups, water and diprotonated ethylenediamine molecules, and the framework components. The compounds were characterized by single-crystal X-ray diffraction, thermogravimetric analysis, and infrared and Raman spectroscopy. Crystal data for 1: monoclinic, space group P21/C (No. 14), a = 6.355(1) A, b = 39.362(8) A, c = 9.249(2) A, beta = 106.7(1) degrees, Z = 2. Crystal data for 2: triclinic, space group P1 (No. 2), a = 8.730(1) A, b = 11.575(1) A, c = 11.696(1) A, alpha = 115.12(1) degree, beta = 90.07(1) degree, gamma = 111.23(1) degree, Z = 2.
使用乙二胺和草酸作为结构导向剂，通过水热法制备了两种新型层状镓磷酸盐 - 草酸盐材料。化合物（C₂N₂H₁₀）₂[Ga₂（C₂O₄）₂（HPO₄）₃]·H₂O 1和（C₂N₂H₁₀）₃[Ga₄（C₂O₄）₄（HPO₄）₄（H₂PO₄）₂] 2密切相关，由GaO₆和HPO₄多面体交替对构成的阴离子双链组成。这些双链通过桥连的HPO₄或H₂PO₄四面体连接形成包含八元环的波纹层。草酸根基团作为二齿配体与每个GaO₆八面体配位。波纹层通过草酸根基团、水和双质子化乙二胺分子与骨架成分之间强到弱的氢键相互作用结合在一起。通过单晶X射线衍射、热重分析以及红外和拉曼光谱对这些化合物进行了表征。1的晶体数据：单斜晶系，空间群P21/C（编号14），a = 6.355(1) Å，b = 39.362(8) Å，c = 9.249(2) Å，β = 106.7(1)°，Z = 2。2的晶体数据：三斜晶系，空间群P1（编号2），a = 8.730(1) Å，b = 11.575(1) Å，c = 11.696(1) Å，α = 115.12(1)°，β = 90.07(1)°，γ = 111.23(1)°，Z = 2。
