Probing Hydrogen Bond Networks in Half-Sandwich Ru(II) Building Blocks by a Combined 1H DQ CRAMPS Solid-State NMR, XRPD, and DFT Approach

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• 作者：Michele R. Chierotti ; Roberto Gobetto ; Carlo Nervi ; Alessia Bacchi ; Paolo Pelagatti ; Valentina Colombo ; Angelo Sironi
• 刊名：Inorganic Chemistry
• 出版年：2014
• 出版时间：January 6, 2014
• 年：2014
• 卷：53
• 期：1
• 页码：139-146
• 全文大小：477K
• ISSN：1520-510X

文摘

The hydrogen bond network of three polymorphs (1伪, 1尾, and 1纬) and one solvate form (1路H₂O) arising from the hydration鈥揹ehydration process of the Ru(II) complex [(p-cymene)Ru(魏N-INA)Cl₂] (where INA is isonicotinic acid), has been ascertained by means of one-dimensional (1D) and two-dimensional (2D) double quantum ¹H CRAMPS (Combined Rotation and Multiple Pulses Sequences) and ¹³C CPMAS solid-state NMR experiments. The resolution improvement provided by homonuclear decoupling pulse sequences, with respect to fast MAS experiments, has been highlighted. The solid-state structure of 1纬 has been fully characterized by combining X-ray powder diffraction (XRPD), solid-state NMR, and periodic plane-wave first-principles calculations. None of the forms show the expected supramolecular cyclic dimerization of the carboxylic functions of INA, because of the presence of Cl atoms as strong hydrogen bond (HB) acceptors. The hydration鈥揹ehydration process of the complex has been discussed in terms of structure and HB rearrangements.