Polymorphism and Structural Variety in Sn(II) Carboxylate Coordination Polymers Revealed from Structure Solution of Microcrystals.

Autor: Ramana AK; Department of Chemistry, University of Warwick, Coventry, CV4 7AL, UK., Tidey JP; Department of Physics, University of Warwick, Coventry, CV4 7AL, UK., de Lima GM; Departamento de Química, Universidade Federal de Minas Gerais, Avenida Antônio Carlos 6627, Belo Horizonte, MG, CEP 31270-901, Brazil., Walton RI; Department of Chemistry, University of Warwick, Coventry, CV4 7AL, UK.
Jazyk: angličtina
Zdroj: Small methods [Small Methods] 2024 Mar 10, pp. e2301703. Date of Electronic Publication: 2024 Mar 10.
DOI: 10.1002/smtd.202301703
Abstrakt: The crystal structures of four coordination polymers constructed from Sn(II) and polydentate carboxylate ligands are reported. All are prepared under hydrothermal conditions in KOH or LiOH solutions (either water or methanol-water) at 130-180 °C and crystallize as small crystals, microns or less in size. Single-crystal structure solution and refinement are performed using synchrotron X-ray diffraction for two materials and using 3D electron diffraction (3DED) for the others. Sn 2 (1,3,5-BTC)(OH), where 1,3,5-BTC is benzene-1,3,5-tricarboxylate, is a new polymorph of this composition and has a three-dimensionally connected structure with potential for porosity. Sn(H-1,3,5-BTC) retains a partially protonated ligand and has a 1D chain structure bound by hydrogen bonding via ─COOH groups. Sn(H-1,2,4-BTC) contains an isomeric ligand, benzene-1,2,4-tricarboxylate, and contains inorganic chains in a layered structure held by hydrogen bonding. Sn 2 (DOBDC), where DOBDC is 2,5-dioxido-benzene-1,4-dicarboxylate, is a new polymorph for this composition and has a three-dimensionally connected structure where both carboxylate and oxido groups bind to the tin centers to create a dense network with dimers of tin. In all materials, the Sn centers are found in highly asymmetric coordination, as expected for Sn(II). For all materials phase purity of the bulk is confirmed using powder X-ray diffraction, thermogravimetric analysis, and infrared spectroscopy.
(© 2024 The Authors. Small Methods published by Wiley-VCH GmbH.)
Databáze: MEDLINE