Abstract: | Synthesis, Vibrational Spectra, and Crystal Structure of the Disiloxanato‐chloroberyllate (Ph4P)2Be4Cl6(OSiMe2OSiMe2O)2] (Ph4P)2Be4Cl6(OSiMe2OSiMe2O)2] ( 1 ) was prepared by the reaction of (Ph4P)2Be2Cl6] with cyclo‐hexamethyl‐trisiloxane in dichloromethane solution, forming colourless, moisture sensitive crystals, which are characterized by their vibrational spectra (IR, Raman) and by an X‐ray crystal structure determination. 1 crystallizes in the triclinic space group with Z = 1 and with the lattice dimensions at 193 K: a = 1050.0(1), b = 1248.2(1), c = 1312.5(1) pm, α = 84.37(1)°; β = 76.53(1)°; γ = 70.79(1)°; R1 = 0.0349. 1 consists of (Ph4P)+ions and centrosymmetric anions Be4Cl6(OSiMe2OSiMe2O)2]2‐, in which the four beryllium atoms are connected by the terminal oxygen atoms of the (OSiMe2OSiMe2O)2‐ ligands via two‐forked bonds to give Be2O2 four‐membered rings. The Be atoms of these units are additionally bridged by two μ‐Cl atoms. 1 is also obtained by reaction of (Ph4P)2Be2Cl6] with Baysilon grease. |