School of Chemistry, Bangor University, Bangor, Gwynedd, LL57 2UW, UK.
Dalton Trans. 2012 Apr 21;41(15):4396-403. doi: 10.1039/c2dt12310j. Epub 2012 Feb 17.
The synthesis and characterization of a series of cyclo-alkylammonium pentaborate salts {[cyclo-C(n)H(2n-1)NR(3)][B(5)O(6)(OH)(4)] (R = H, n = 3, 5-7 (1-4); R = Me, n = 6 (5))} are reported. Compounds 1, 2 and 5 have been further characterized by single-crystal XRD studies. Attempted recrystallization of 3 and 4 yielded small crops of the unexpected heptaborate salts, cyclo-C(6)H(11)NH(3)[B(7)O(9)(OH)(5)]·3H(2)O·B(OH)(3) (6) and cyclo-C(7)H(13)NH(3)[B(7)O(9)(OH)(5)]·2H(2)O·2B(OH)(3) (7) which were also characterized crystallographically. All compounds show extensive supramolecular H-bonded anionic lattices templated by the cations. H-bond interactions are described in detail. TGA-DSC analysis of the pentaborates 1-5 showed that they thermally decomposed in air at 800 °C to 2.5B(2)O(3), in a 2 step process involving dehydration (<250 °C) and oxidative decomposition (250-600 °C). BET analysis of materials derived from the pentaborates had internal porosities of <1 m(2) g(-1).
报道了一系列环烷基铵五硼酸盐盐的合成和表征，包括 {[cyclo-C(n)H(2n-1)NR(3)][B(5)O(6)(OH)(4)] (R = H, n = 3, 5-7 (1-4); R = Me, n = 6 (5))}。化合物 1、2 和 5 进一步通过单晶 XRD 研究进行了表征。尝试对 3 和 4 进行重结晶得到了少量意想不到的七硼酸盐盐，cyclo-C(6)H(11)NH(3)[B(7)O(9)(OH)(5)]·3H(2)O·B(OH)(3) (6)和cyclo-C(7)H(13)NH(3)[B(7)O(9)(OH)(5)]·2H(2)O·2B(OH)(3) (7)，它们也通过晶体学进行了表征。所有化合物都显示出由阳离子模板的广泛超分子氢键阴离子晶格。详细描述了氢键相互作用。五硼酸盐 1-5 的 TGA-DSC 分析表明，它们在空气中于 800°C 热分解为 2.5B(2)O(3)，分两步进行，涉及脱水(<250°C)和氧化分解(250-600°C)。来自五硼酸盐的材料的 BET 分析具有<1 m(2) g(-1)的内部孔隙度。
