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The synthesis of a number of pentaborate(1-) salts from cations arising from N -substituted α,α-, α,β-, and α,γ-diaminoalkanes has been attempted in aqueous solution from B(OH) 3 and the appropriate diammine in a 10:1 ratio. Despite relatively mild work-up conditions the pentaborate(1-) salts prepared were not always as anticipated and the following compounds were isolated in good yield: [Me 2 NH(CH 2 ) 2 NHMe 2 ][B 5 O 6 (OH) 4 ] 2 ( 1 ), [Et 2 NH(CH 2 ) 2 NHEt 2 ][B 5 O 6 (OH) 4 ] 2 ( 2 ), [Et 2 NH 2 ][B 5 O 6 (OH) 4 ] ( 3 ), [Me 2 NH 2 ][B 5 O 6 (OH) 4 ] ( 4 ), [Me 2 NH(CH 2 ) 3 NHMe 2 ][B 5 O 6 (OH) 4 ] 2 ( 5 ), [Et 2 NH(CH 2 ) 3 NHEt 2 ][B 5 O 6 (OH) 4 ] 2 ( 6 ), [Me 3 NCH 2 CH=CH 2 ][B 5 O 6 (OH) 4 ] ( 7 ), and [Me 3 N(CH 2 ) 3 NMe 3 ] [B 5 O 6 (OH) 4 ] 2  . 0.5H 2 O ( 8 ). The tetraborate(2-) salt, [Me 3 N(CH 2 ) 2 NMe 3 ][B 4 O 5 (OH) 4 ] . 2B(OH) 3  . 2H 2 O ( 9 ) was obtained in moderate yield (41%) from a 3:1 reaction of B(OH) 3 with [Me 3 N(CH 2 ) 2 NMe 3 ](OH) 2 . All compounds were characterized by spectroscopy ( 1 H, 11 B, 13 C NMR and IR) and thermal gravimetric analysis (TGA). BET analysis on materials derived thermally from selected samples ( 1 , 2 , 6 , 7 ) all had porosities of &lt; 1 m 2 /g, demonstrating that they were non-porous. Single-crystal XRD structures were obtained for 2 , 3 , 7 , 8 and 9 and all contain extensive H-bonded polyborate lattices.

molecules/molecules online/molecules annual

Pentaborate(1-) Salts and a Tetraborate(2-) Salt Derived from C2- or C3-Linked Bis(alkylammonium) Dications: Synthesis, Characterization, and Structural (XRD) Studies