10.1021/acs.inorgchem.5b01101.s002 Luis G. Perla Luis G. Perla Slavi C. Sevov Slavi C. Sevov [Bi<sub>12</sub>Ni<sub>7</sub>(CO)<sub>4</sub>]<sup>4–</sup>: Aggregation of Intermetalloid Clusters by Their Thermal Deligation and Oxidation American Chemical Society 2015 Bi 12Ni clusters Bi 3Ni Bi 3Ni electrospray mass spectrometry Ni atoms Intermetalloid Clusters Bi 12Ni Aggregation Thermal Deligation intermetalloid cluster electron count Bi 6Ni Bi 3 triangles 2015-09-08 00:00:00 Dataset https://acs.figshare.com/articles/dataset/_Bi_sub_12_sub_Ni_sub_7_sub_CO_sub_4_sub_sup_4_sup_Aggregation_of_Intermetalloid_Clusters_by_Their_Thermal_Deligation_and_Oxidation/2133871 Reported are the synthesis and structure of the anionic intermetalloid cluster [Bi<sub>12</sub>Ni<sub>7</sub>(CO)<sub>4</sub>]<sup>4–</sup>. It was synthesized from the known smaller clusters Bi<sub>3</sub>Ni<sub>4</sub>(CO)<sub>6</sub><sup>3–</sup>, Bi<sub>3</sub>Ni<sub>6</sub>(CO)<sub>9</sub><sup>3–</sup>, and Ni@Bi<sub>6</sub>Ni<sub>6</sub>(CO)<sub>8</sub><sup>4–</sup> by their aggregation as a result of thermal deligation and oxidation. The new cluster is structurally characterized by single-crystal X-ray diffraction in the compound (K­[crypt])<sub>4</sub>[Bi<sub>12</sub>Ni<sub>7</sub>(CO)<sub>4</sub>] (<b>1</b>), and its presence in solution is confirmed by electrospray mass spectrometry. It can be viewed as composed of a Ni-centered icosahedral core of Bi<sub>6</sub>Ni<sub>6</sub>(CO)<sub>4</sub> where two diametrically opposed Ni atoms are capped by Bi<sub>3</sub> triangles. However, its electron count is rationalized based on a structure made of fused tetrahedra.