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Stoichiometry mechanosynthesis and interconversion of metal salts containing [CuCl3(H2O)] and [Cu2Cl8]4−

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Abstract

Solid-state grinding plays a very important role in the study of the dynamics changes of a reaction, especially as a means of selectively preparing specific stoichiometric crystalline supramolecular complexes or cocrystals. Herein, using the tetradentate ligand (1R,2R)-N,N′-bis(pyridin-4-ylmethyl)cyclohexane-1,2-diamine (L), two copper(II) chloride salts, namely [H4L]4+·[CuCl3(H2O)]·3Cl (1) and [H4L]4+·[Cu2Cl8]4−·H2O (2), were produced via 1 : 1 and 1 : 2 stoichiometric controlled synthesis in a two-step process by grinding the reactants together using a mortar and pestle. By adding appropriate amounts of the corresponding components, the reversible transformation of the two salts occurred. The progress of the reversible reaction between the salt 1 and 2 was dynamically monitored by fluorescence spectroscopy, powder X-ray diffraction and Raman spectroscopy. Quantum-mechanical (QM) calculations specific for crystalline solid phases provided some insights into the relative stabilities of the two salts, indicating plausible driving forces for the reversible transformation.

Graphical abstract: Stoichiometry mechanosynthesis and interconversion of metal salts containing [CuCl3(H2O)]− and [Cu2Cl8]4−

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Publication details

The article was received on 13 Jun 2019, accepted on 14 Oct 2019 and first published on 15 Oct 2019


Article type: Paper
DOI: 10.1039/C9CE00911F
CrystEngComm, 2019, Advance Article

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    Stoichiometry mechanosynthesis and interconversion of metal salts containing [CuCl3(H2O)] and [Cu2Cl8]4−

    H. Li, A. Famulari, L. Xin, H. Zhou, P. Zhang and F. Guo, CrystEngComm, 2019, Advance Article , DOI: 10.1039/C9CE00911F

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