The hydrogen bond network of three polymorphs (1α, 1β, and 1γ) and one solvate form (1·H2O) arising from the hydration−dehydration process of the Ru(II) complex [(p-cymene)Ru(κN-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 1γ 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−dehydration process of the complex has been discussed in terms of structure and HB rearrangements.

Probing Hydrogen Bond Networks in Half-Sandwich Ru(II) Building Blocks by a Combined1H DQ CRAMPS Solid-State NMR, XRPD, and DFT Approach / Michele R., Chierotti; Roberto, Gobetto; Carlo, Nervi; Bacchi, Alessia; Pelagatti, Paolo; Valentina, Colombo; Angelo, Sironi. - In: INORGANIC CHEMISTRY. - ISSN 0020-1669. - 53:1(2014), pp. 139-146. [10.1021/ic401762z]

Probing Hydrogen Bond Networks in Half-Sandwich Ru(II) Building Blocks by a Combined1H DQ CRAMPS Solid-State NMR, XRPD, and DFT Approach

BACCHI, Alessia;PELAGATTI, Paolo;
2014

Abstract

The hydrogen bond network of three polymorphs (1α, 1β, and 1γ) and one solvate form (1·H2O) arising from the hydration−dehydration process of the Ru(II) complex [(p-cymene)Ru(κN-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 1γ 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−dehydration process of the complex has been discussed in terms of structure and HB rearrangements.
Probing Hydrogen Bond Networks in Half-Sandwich Ru(II) Building Blocks by a Combined1H DQ CRAMPS Solid-State NMR, XRPD, and DFT Approach / Michele R., Chierotti; Roberto, Gobetto; Carlo, Nervi; Bacchi, Alessia; Pelagatti, Paolo; Valentina, Colombo; Angelo, Sironi. - In: INORGANIC CHEMISTRY. - ISSN 0020-1669. - 53:1(2014), pp. 139-146. [10.1021/ic401762z]
File in questo prodotto:
Non ci sono file associati a questo prodotto.

I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.

Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/11381/2670065
Citazioni
  • ???jsp.display-item.citation.pmc??? ND
  • Scopus 15
  • ???jsp.display-item.citation.isi??? 15
social impact