Zhang Min, Zhou Dan, Li Jiyang, Yu Jihong, Xu Jun, Deng Feng, Li Guanghua, Xu Ruren
State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, College of Chemistry, Jilin University, Changchun 130012, People's Republic of China.
Inorg Chem. 2007 Jan 8;46(1):136-40. doi: 10.1021/ic061362w.
A new two-dimensional-layered fluoroaluminophosphate (C4H11NOH)3.5[Al4(PO4)5F] x 0.5H3O (denoted as AlPO-CJ20) with an Al/P ratio of 4:5 has been synthesized solvothermally by using 2-amino-2-methyl-1-propanol as the structure-directing agent. Its structure was determined by single-crystal X-ray diffraction analysis and further characterized by solid-state NMR techniques, including 27Al, 19F --> 27Al cross-polarization, and 31P magic angle spinning NMR. The alternation of Al-centered tetrahedra (AlO4 and AlO3F) and PO3(=O) tetrahedra gives rise to a new type of 4.6.16-net sheet. The inorganic sheets are stacked in an ABAB sequence along the [010] direction and further held together through strong H bonds between protonated template molecules and P=O groups in the inorganic layers. Except for Mu-4, AlPO-CJ20 is the second layered aluminophosphate with an Al/P ratio of 4:5, and it contains the largest pore opening of 16-rings in the known layered aluminophosphates. Furthermore, the coordination of Al and P of fluoroaluminophosphates is summarized. Crystal data: (C4H11NOH)3.5[Al4(PO4)5F] x 0.5H3O, monoclinic, C2/c (No. 15), a = 32.678(7) A, b = 12.956(3) A, c = 21.045(4) A, beta = 115.17(3) degrees, V = 8064(3) A3, Z = 8, R1 = 0.0837 [I > 2sigma(I)], and wR2 = 0.2428 (all data).
一种新型的二维层状氟铝磷酸盐（C4H11NOH）3.5[Al4(PO4)5F]·0.5H3O（记为AlPO-CJ20），其铝磷比为4:5，已通过以2-氨基-2-甲基-1-丙醇为结构导向剂的溶剂热法合成。通过单晶X射线衍射分析确定了其结构，并通过固态核磁共振技术进一步表征，包括27Al、19F→27Al交叉极化和31P魔角旋转核磁共振。以铝为中心的四面体（AlO4和AlO3F）和PO3(=O)四面体的交替产生了一种新型的4.6.16-网层。无机层沿着[010]方向以ABAB序列堆叠，并通过质子化模板分子与无机层中P=O基团之间的强氢键进一步结合在一起。除了Mu-4之外，AlPO-CJ20是第二种铝磷比为4:5的层状铝磷酸盐，并且它在已知的层状铝磷酸盐中具有最大的16元环孔口。此外总结了氟铝磷酸盐中铝和磷的配位情况。晶体数据：（C4H11NOH）3.5[Al4(PO4)5F]·0.5H3O，单斜晶系，C2/c（编号15），a = 32.678(7) Å，b = 12.956(3) Å，c = 21.045(4) Å，β = 115.17(3)°，V = 8064(3) Å3，Z = 8，R(1) = 0.0837 [I > 2σ(I)]，wR(2) = 0.2428（所有数据）。
