| Summary: | The relevance of multidimensional and porous crystalline materials to nuclear waste remediation and storage applications has motivated exploratory research focused on materials discovery of compounds, such as actinide mixed-oxoanion phases, which exhibit rich structural chemistry. The novel phase K<sub>1.8</sub>Na<sub>1.2</sub>[(UO<sub>2</sub>)BSi<sub>4</sub>O<sub>12</sub>] has been synthesized using hydrothermal methods, representing the first example of a uranyl borosilicate. The three-dimensional structure crystallizes in the orthorhombic space group <i>Cmce</i> with lattice parameters <i>a</i> = 15.5471(19) Å, <i>b</i> = 14.3403(17) Å, <i>c</i> = 11.7315(15) Å, and <i>V</i> = 2615.5(6) Å<sup>3</sup>, and is composed of UO<sub>6</sub> octahedra linked by [BSi<sub>4</sub>O<sub>12</sub>]<sup>5−</sup> chains to form a [(UO<sub>2</sub>)BSi<sub>4</sub>O<sub>12</sub>]<sup>3−</sup> framework. The synthesis method, structure, results of Raman, IR, and X-ray absorption spectroscopy, and thermal stability are discussed.
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