Synthesis and Characterization of Air-Sensitive Silane Compounds

All reactions involving air-sensitive
compounds were carried out under an atmosphere of dry nitrogen or
argon using either Schlenk techniques or a glove box. All solvents
were dried using a column-based solvent purification system.^{44 (link)} 2,2,5,5-Tetrakis(trimethylsilyl)decamethylhexasilane,^{45 (link)} 1,4-dipotassio-1,1,4,4-tetrakis(trimethylsilyl)tetramethyltetrasilane
(1),^{36 (link)} 1,3-bis[potassiobis(trimethylsilyl)silyl]-1,1,3,3-tetramethyldisiloxane
(3),^{41 (link)} Cp₂YCl,^{46 (link)} 1,1′-bis[tris(trimethylsilyl)silyl]ferrocene,^{42 (link)} and 5(42 (link)) were prepared following published procedures. All other chemicals
were obtained from different suppliers and used without further purification.
¹H (300 MHz), ¹³C (75.4 MHz), and ²⁹Si (59.3 MHz) NMR spectra were recorded on a Varian INOVA 300 spectrometer.
If not noted otherwise all samples were measured in C₆D₆. To compensate for the low isotopic abundance of ²⁹Si, the INEPT pulse sequence was used for the amplification of the
signal.^{47 (link)−49 (link)} Spectra are calibrated to the deuterium resonance
of the solvent (C₆D₆)^{50 (link)} and referenced to tetramethysilane (TMS).^{51 (link)}Elementary analyses were carried out using a Heraeus VARIO
ELEMENTAR.