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Unsaturated silicon clusters with only partial substitution, and thus, "naked" Si atoms are well studied species as they are proposed intermediates in gas-phase deposition processes. Although a remarkable number of stable molecular clusters has been reported, they are typically still obtained by multi-step syntheses. Herein we introduce a newly developed synthetic approach which led to the formation of the anionic species {Si(TMS) 3 } 3 Si 9  - ( 1a ) and {Si(TMS) 3 } 2 Si 9  2- ( 1b ), and an extension of this synthetic protocol resulted in the first covalent attachment of ligands through metal atoms to these clusters, (SnCy 3 ) 3 Si 9  - ( 2a ) and (SnCy 3 ) 2 Si 9  2- ( 2b ). The influence of the substituents on the electron localization in the central Si 9 unit is analyzed by means of intrinsic bond orbital (IBO) analysis and partial atomic charge distribution. The IBO analyses reveal a new type of delocalization including 5-center-6-electron besides 3-center-2-electron bonds. The Raman spectra of 1b and 2b allow an assignment of the Si-Si intra-cluster vibrations by comparison to calculated (DFT-PBE0) spectra. The anions are formed in a one-step synthesis from binary K 12 Si 17 which can easily be obtained by fusing the elements K and Si. The anions are characterized by ESI mass spectrometry and comprehensive NMR studies ( 1 H, 13 C, 29 Si, 119 Sn). Attempts to crystallize 1a and 2a as their (K-222crypt) + salts yielded after the loss of one of the substituents single crystals containing 1b and 2b . The single crystal X-ray structure analyses reveal the presence of anionic siliconoids with surfaces of seven unsubstituted silicon atoms.

Silicon clusters with six and seven unsubstituted vertices via a two-step reaction from elemental silicon