Abstract
(DME)2] 1 (R = C6H4-4-CH3; DME = dimethoxyethane) was prepared by reaction of calcium with NR=CPh-CPh=NR in DME solution. The compound forms orange, moisture sensitive crystals, which were characterized by an X-ray structure determination [space group orthorhombic, P212121, Z = 4, 4634 observed unique reflections, R = 0.046; lattice dimensions at –70 °C: a = 1340.2(3), b = 1528.1(3), c = 1609.1(3) pm]. The calcium atom is coordinated by the four oxygen atoms of two chelating DME molecules and two nitrogen atoms of the diazadiene ligand, bonded in its enediamide form. [Ba2(DME)3(NPh–CPh=CPh–NPh)2 · DME] 3 was obtained from barium metal and NPh=CPh-CPh=NPh in DME solution as red crystals [space group monoclinic, P2l/c, Z = 4, 4000 observed unique reflections, R = 0.166; lattice dimensions at -70 °C: a = 1704.5(3), b = 1786.1(4), c = 2177.4(4) pm, β = 105.98(3)°]. The two barium atoms are bridged by two differently bonded diazadiene ligands (μ2-Ν,Ν′;μ-Ν, σ-Ν′). Additionally, one of the barium atoms is coordinated to two DME molecules and the other one to only one of the ether molecules. A further DME molecule is a constituent of the crystal lattice.
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