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              <p>The 2D composition-space diagram of the Al(OH)&lt;sub&gt;3&lt;/sub&gt;−&lt;i&gt;Am&lt;/i&gt;&lt;sub&gt;&lt;i&gt;2&lt;/i&gt;&lt;/sub&gt;&lt;i&gt;TAZ&lt;/i&gt;−HF&lt;sub&gt;aq&lt;/sub&gt;−ethanol system is established under microwave heating at 190 °C for [Al&lt;sup&gt;3+&lt;/sup&gt;] = 1 mol·L&lt;sup&gt;−1&lt;/sup&gt;. Four new fluoroaluminates are evidenced when the [HF]/[&lt;i&gt;Am&lt;/i&gt;&lt;sub&gt;&lt;i&gt;2&lt;/i&gt;&lt;/sub&gt;&lt;i&gt;TAZ&lt;/i&gt;] ratio is increased in the starting solution, and the dimensionality of the inorganic frameworks is increased from 0D in [H&lt;i&gt;Am&lt;/i&gt;&lt;sub&gt;&lt;i&gt;2&lt;/i&gt;&lt;/sub&gt;&lt;i&gt;TAZ&lt;/i&gt;]&lt;sub&gt;2&lt;/sub&gt;·(AlF&lt;sub&gt;5&lt;/sub&gt;(H&lt;sub&gt;2&lt;/sub&gt;O))·2H&lt;sub&gt;2&lt;/sub&gt;O (&lt;i&gt;Pc&lt;/i&gt;, &lt;i&gt;Z&lt;/i&gt; = 2), to 1D in [H&lt;i&gt;Am&lt;/i&gt;&lt;sub&gt;&lt;i&gt;2&lt;/i&gt;&lt;/sub&gt;&lt;i&gt;TAZ&lt;/i&gt;]&lt;sub&gt;2&lt;/sub&gt;·(AlF&lt;sub&gt;5&lt;/sub&gt;) and [H&lt;i&gt;Am&lt;/i&gt;&lt;sub&gt;&lt;i&gt;2&lt;/i&gt;&lt;/sub&gt;&lt;i&gt;TAZ&lt;/i&gt;]&lt;sub&gt;2&lt;/sub&gt;·(Al&lt;sub&gt;2&lt;/sub&gt;F&lt;sub&gt;8&lt;/sub&gt;) (&lt;i&gt;Fdd&lt;/i&gt;2, &lt;i&gt;Z&lt;/i&gt; = 8), and to 2D in [H&lt;i&gt;Am&lt;/i&gt;&lt;sub&gt;&lt;i&gt;2&lt;/i&gt;&lt;/sub&gt;&lt;i&gt;TAZ&lt;/i&gt;]&lt;sub&gt;2&lt;/sub&gt;·(Al&lt;sub&gt;5&lt;/sub&gt;F&lt;sub&gt;17&lt;/sub&gt;) (&lt;i&gt;Imm&lt;/i&gt;2, &lt;i&gt;Z&lt;/i&gt; = 2). This evolution is partially paralleled by the thermal decomposition of [H&lt;i&gt;Am&lt;/i&gt;&lt;sub&gt;&lt;i&gt;2&lt;/i&gt;&lt;/sub&gt;&lt;i&gt;TAZ&lt;/i&gt;]&lt;sub&gt;2&lt;/sub&gt;·(AlF&lt;sub&gt;5&lt;/sub&gt;(H&lt;sub&gt;2&lt;/sub&gt;O))·2H&lt;sub&gt;2&lt;/sub&gt;O; on heating, this hydrate gives [H&lt;i&gt;Am&lt;/i&gt;&lt;sub&gt;&lt;i&gt;2&lt;/i&gt;&lt;/sub&gt;&lt;i&gt;TAZ&lt;/i&gt;]&lt;sub&gt;2&lt;/sub&gt;·(AlF&lt;sub&gt;5&lt;/sub&gt;) at 100−150 °C and [H&lt;i&gt;Am&lt;/i&gt;&lt;sub&gt;&lt;i&gt;2&lt;/i&gt;&lt;/sub&gt;&lt;i&gt;TAZ&lt;/i&gt;]&lt;sub&gt;2&lt;/sub&gt;·(Al&lt;sub&gt;2&lt;/sub&gt;F&lt;sub&gt;8&lt;/sub&gt;) at 180 °C; the loss and simultaneous decomposition of [H&lt;i&gt;Am&lt;/i&gt;&lt;sub&gt;&lt;i&gt;2&lt;/i&gt;&lt;/sub&gt;&lt;i&gt;TAZ&lt;/i&gt;]F leave a solid residue of polymeric paracyanogen (CN)&lt;sub&gt;2&lt;i&gt;n&lt;/i&gt;&lt;/sub&gt; that is further decomposed and hydrolyzed into HCN and HNCO by atmospheric water traces. NMR &lt;sup&gt;19&lt;/sup&gt;F spectroscopy of [H&lt;i&gt;Am&lt;/i&gt;&lt;sub&gt;&lt;i&gt;2&lt;/i&gt;&lt;/sub&gt;&lt;i&gt;TAZ&lt;/i&gt;]&lt;sub&gt;2&lt;/sub&gt;·(AlF&lt;sub&gt;5&lt;/sub&gt;) is in agreement with the crystallographic determination, and the &lt;sup&gt;27&lt;/sup&gt;Al spectrum demonstrates that a significant F&lt;sup&gt;−&lt;/sup&gt;/OH&lt;sup&gt;−&lt;/sup&gt; substitution is excluded.</p>
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