Issue 19, 2020

High-temperature, high-pressure hydrothermal synthesis, crystal structure, and infrared and NMR spectroscopy of a barium lead borate with a 2D layer structure: [Ba3Pb(H2O)][B11O19(OH)3]

Abstract

With a high-temperature, high-pressure hydrothermal technique, a new barium lead borate, [Ba3Pb(H2O)][B11O19(OH)3] (1), has been synthesized and characterized by single-crystal X-ray diffraction, and infrared and solid-state NMR spectroscopy. The structure of 1 contains planar thick layers of borates with the Ba2+ cations at sites in the inter- and intralayer space. Each layer consists of three single sheets. The central sheet is very corrugated and is built up from the fundamental building block (FBB) 2Δ3□:〈Δ2□〉–〈Δ2□〉. On both sides of the central sheet there are borate single chains formed of the very rare FBB 2Δ4□:〈Δ2□〉–〈3□〉Δ via corner-sharing. This FBB was first observed in a high-pressure polymorph of CaB2O4. These chains are linked into a sheet by PbO5(H2O) polyhedra, which are further linked to the central sheet by sharing vertices between triangles and tetrahedra to form a thick layer. The IR spectrum shows the presence of hydroxyl groups of HBO4, water molecules, BO3 triangles, and BO4 tetrahedra. The presence of BO3 and BO4 polyhedra was also confirmed by 11B MAS NMR spectroscopy.

Graphical abstract: High-temperature, high-pressure hydrothermal synthesis, crystal structure, and infrared and NMR spectroscopy of a barium lead borate with a 2D layer structure: [Ba3Pb(H2O)][B11O19(OH)3]

Supplementary files

Article information

Article type
Paper
Submitted
28 Mar 2020
Accepted
13 Apr 2020
First published
14 Apr 2020

Dalton Trans., 2020,49, 6220-6226

High-temperature, high-pressure hydrothermal synthesis, crystal structure, and infrared and NMR spectroscopy of a barium lead borate with a 2D layer structure: [Ba3Pb(H2O)][B11O19(OH)3]

Y. Kuo, H. Liu, S. Wang and K. Lii, Dalton Trans., 2020, 49, 6220 DOI: 10.1039/D0DT01172J

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