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Co-existence of Distinct Supramolecular Assemblies in Solution and in the Solid State

机译：溶液中不同超分子组件的共存和固态

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摘要

The formation of distinct supramolecular assemblies, including a metastable species, is revealed for a lipophilic guanosine (G) derivative in solution and in the solid state. Structurally different G-quartet-based assemblies are formed in chloroform depending on the nature of the cation, anion and the salt concentration, as characterized by circular dichroism and time course diffusion-ordered NMR spectroscopy data. Intriguingly, even the presence of potassium ions that stabilize G-quartets in chloroform was insufficient to exclusively retain such assemblies in the solid state, leading to the formation of mixed quartet and ribbon-like assemblies as revealed by fast magic-angle spinning (MAS) NMR spectroscopy. Distinct N-H···N and N-H···O intermolecular hydrogen bonding interactions drive quartet and ribbon-like self-assembly resulting in markedly different 2D ~1H solid-state NMR spectra, thus facilitating a direct identification of mixed assemblies. A dissolution NMR experiment confirmed that the quartet and ribbon interconversion is reversible- further demonstrating the changes that occur in the self-assembly process of a lipophilic nucleoside upon a solid-state to solution-state transition and vice versa. A systematic study for complexation with different cations (K~+, Sr~(2+)) and anions (picrate, ethanoate and iodide) emphasizes that the existence of a stable solution or solid-state structure may not reflect the stability of the same supramolecular entity in another phase.
机译：形成不同的超分子组件，包括稳定物种，用于溶液中的亲脂性鸟苷（g）衍生物和固态。根据阳离子，阴离子和盐浓度的性质，在氯仿中形成了结构不同的基于G-Quartet基组件，其特征在于圆形二色性和时间过程扩散有序的NMR光谱数据。有趣的是，即使存在稳定氯仿中的G-四分之二的钾离子的存在不足以排除在固态中的这种组件，导致形成混合四重奏和带状的组件，如通过快速魔法角旋转（MAS）所揭示的NMR光谱学。不同的n-h···n和n-h···o分子间氢键相互作用驱动四重子型和带状自组装，得到显着不同的2d〜1H固态NMR光谱，从而便于混合组件的直接识别。溶解NMR实验证实了四重奏和色带互联是可逆的 - 进一步证明在固态到溶液状态转变的脂肪核苷酸的自组装过程中发生的变化，反之亦然。用不同阳离子络合的系统研究（K〜+，Sr〜（2+）和阴离子（怯懦，乙酸盐和碘化物）强调，存在稳定的溶液或固态结构可能不会反映相同的稳定性另一阶段的超分子实体。

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