Institut für Anorganische Chemie, Georg-August-Universität Göttingen, Tammannstrasse 4, D-37077 Göttingen, Germany.
J Org Chem. 2011 Nov 4;76(21):9081-5. doi: 10.1021/jo2019152. Epub 2011 Oct 13.
A propeller-shaped boron-nitrogen compound (NB(3)) with three binding sites for fluoride anions was synthesized and investigated by optical absorption, luminescence, and ((1)H, (11)B, (13)C, (19)F) NMR spectroscopy. Binding of fluoride in dichloromethane solution occurs in three clearly identifiable steps and leads to stepwise blocking of the three initially present nitrogen-to-boron charge transfer pathways. As a consequence, the initially bright blue charge transfer emission is red-shifted and decreases in intensity, until it is quenched completely in presence of large fluoride excess. Fluoride binding constants were determined from global fits to optical absorption and luminescence titration data and were found to be K(a1) = 4 × 10(7) M(-1), K(a2) = 2.5 × 10(6) M(-1), and K(a3) = 3.2 × 10(4) M(-1) in room temperature dichloromethane solution. Complexation of fluoride to a given dimesitylboryl site increases the electron density at the central nitrogen atom of NB(3), and this leads to red shifts of the remaining nitrogen-to-boron charge transfer transitions involving yet unfluorinated dimesitylboryl groups.
一种具有三个氟阴离子结合位点的桨形硼氮化合物(NB(3)),通过光吸收、发光和(1H、11B、13C、19F)NMR 光谱进行了研究。在二氯甲烷溶液中,氟的结合分三个明显可辨的步骤进行,并导致最初存在的三个氮到硼的电荷转移途径逐步受阻。结果,最初明亮的蓝色电荷转移发射发生红移并强度降低,直到在大量氟化物过剩存在下完全猝灭。通过对光吸收和荧光滴定数据的全局拟合确定了氟结合常数,在室温二氯甲烷溶液中,它们分别为 K(a1) = 4 × 10(7) M(-1)、K(a2) = 2.5 × 10(6) M(-1)和 K(a3) = 3.2 × 10(4) M(-1)。氟与特定二苯甲硼基位点的络合增加了 NB(3)中中心氮原子上的电子密度,这导致了剩余的氮到硼的电荷转移跃迁发生红移,涉及尚未氟化的二苯甲硼基基团。