A series of open-framework aluminoborates (ABOs), [CH3NH3][(CH3CH2)2NH2][Al(B5O10)] (1), [CH3CH2NH3][(CH3CH2)2NH2][Al(B5O10)] (2), [CH3CH2NH3][(CH3)2NH2](H2O)0.5[Al(B5O10)] (3) and [CH3NH3][CH3CH2NH3](H2O)2[Al(B5O10)] (4) have been made co-templated by two types of primary amines under solvothermal conditions and characterized by elemental analysis, IR, TGA, UV-Vis, powder XRD, single crystal XRD and NLO determination, respectively. These four ABOs display two structural types: 1, 2 and 3 are isostructural and exhibit CrB4 topology, showing three different layers along three different directions; while 4 contains 8-, 14-ring layers, which are packed along the [001] direction to form a noncentrosymmetric 3D framework with 8-, 14-ring channels, showing second harmonic generation (SHG) response that is about 0.5 times that of KDP (KH2PO4). The electronic structure calculations for 1 and 4 also have been performed.
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