Trichloroberyllate complexes of dimethyl cyanamide, morpholine, and 4,4′-bipyridine

The trichloroberyllate complexes (Ph4P)[BeCl3(NCNMe2)] (1), (Ph4P)[BeCl3{HN(CH2)(4)O}] (2), and (Ph4P)(2)[(BeCl3)(2)(4,4'-bipy)] (3) were prepared by reactions of (Ph4P)(2)[Be2Cl(6)] with dimethyl cyanamide, trimethylsilylmorpholinate, and 4,4'-bipyridine, respectively, in dichloromethane solutions. 1-3 were characterized by X-ray crystallography and by IR-spectroscopy. 1 center dot CH2Cl2: Space group P1, Z = 1, lattice dimensions at 173 K: a 714.2(1), b = 919.5(2), c = 1233.4(2) pm, alpha = 94.97(1)degrees, beta = 90.86(1)degrees, gamma = 111.90(1)degrees, R-1 = 0.0310. In the complex anion [BeCl3(NCNMe2)](-) the dimethyl cyanamide ligand is coordinated via a linear Be-N C-NMe2 arrangement, the CH2O2 molecules forming linear chains by hydrogen bridges center dot center dot center dot HCH center dot center dot center dot Cl center dot center dot center dot with the chlorine atoms of the {BeCl3-} groups. 2: Space group P (1) over bar, Z = 2, lattice dimensions at 173 K: a 1050.9(1), b = 1099.7(1), c 1308.3(2) pm, alpha = 87.57(1)degrees, beta = 70.97(1)degrees, gamma = 74.58(1)degrees, R-1 = 0.0397. The complex anions are dimerized by centrosymmetric puckered eight-membered [Be-N-H center dot center dot center dot Cl](2) rings. 3 center dot 2CH(2)Cl(2): Space group P (1) over bar, Z = 2, lattice dimensions at 173 K: a = 1095.4(1), b = 1559.6(2), c = 1869.8(3) pm, alpha = 79.12(1)degrees, beta = 73.83(1)degrees, gamma = 78.76(1)degrees, R-1 = 0.0548. The complex contains dianions [Cl3Be(mu-bipy)BeCl3](2-) with Be-N distances of 177.0(6) and 178.5(6) pm. Both {BeCl3}(-) groups form C-H center dot center dot center dot Cl hydrogen bridges with the dichloromethane molecules.