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Ruser, Niklas
Kiel University
in Cooperation with on an Cooperation-Score of 37%
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article
Synthesis, crystal structure, and topology of a polycatenated bismuth coordination polymer
Abstract
<jats:title>Abstract</jats:title><jats:p>Solvothermal reaction of Bi(NO<jats:sub>3</jats:sub>)<jats:sub>3</jats:sub>·5H<jats:sub>2</jats:sub>O with the flexible ligand 1,3,5-tris[4-(carboxyphenyl)oxamethyl]-2,4,6-trimethylbenzene (H<jats:sub>3</jats:sub>TBTC) in methanol at 120 °C for 1 h led to the formation of a novel coordination polymer (CP) with the composition of Bi(TBTC). The structure of the microcrystalline material was determined through three-dimensional electron diffraction (3DED) measurements and phase purity was confirmed by a Pawley refinement, elemental analysis, and thermal analysis. The compound crystallizes in the triclinic space group <jats:inline-formula id="j_znb-2022-0002_ineq_001"><jats:alternatives><m:math xmlns:m="http://www.w3.org/1998/Math/MathML" overflow="scroll"><m:mrow><m:mi>P</m:mi><m:mover accent="true"><m:mn>1</m:mn><m:mo stretchy="true">‾</m:mo></m:mover></m:mrow></m:math><jats:tex-math> $P{1}$ </jats:tex-math><jats:inline-graphic xmlns:xlink="http://www.w3.org/1999/xlink" xlink:href="graphic/j_znb-2022-0002_ineq_001.png" /></jats:alternatives></jats:inline-formula> with one Bi<jats:sup>3+</jats:sup> cation and one TBTC<jats:sup>3−</jats:sup> trianion in the asymmetric unit. Edge-sharing of BiO<jats:sub>7</jats:sub> polyhedra leads to the formation of dinuclear Bi<jats:sub>2</jats:sub>O<jats:sub>12</jats:sub> units, which through coordination to six TBTC<jats:sup>3−</jats:sup> ions form a layered two-periodic structure. Upon heating the material in air, the unit cell volume contracts by 9%, which is attributed to a shift in the inter-layer arrangement and to the flexibility of the building units of the structure. The compound starts to decompose at ∼300 °C. Topological analysis revealed layers consisting of 3-c and 6-c nodes, consistent with the two-periodic <jats:bold>kgd</jats:bold> net – the dual of the Kagome net (<jats:bold>kgm</jats:bold>). However, due to the non-planar nature of the Bi(TBTC) layers, adjacent layers are interlaced by polycatenation.</jats:p>