Abstract
AbstractBis(tetraphenylphosphonium) hexachloridodiberyllate, (Ph4P)2[Be2Cl6], reacts with excess trimethylsilyl‐iso‐thiocyanate to give a mixture of colourless single crystals of (Ph4P)2[Be(NCS)4] (1) and (Ph4P)4[{Be2(NCS)4(μ‐NCS)2}{Be2(NCS)6(μ‐H2N2C2S2)}] (2), which can be separated by selection. Both complexes were characterized by X‐ray diffraction. Compound 1 can be prepared without by‐products by treatment of (Ph4P)2[BeCl4] with excess Me3SiNCS in dichloromethane solution. 1: Space group I41/a, Z = 4, lattice dimensions at 100(2) K: a = b = 1091.2(1), c = 3937.1(3) pm, R1 = 0.0474. The [Be(NCS)4]2– ion of 1 forms tetragonally distorted tetrahedral anions with Be–N distances of 168.4(2) pm and weak intermolecular S···S contacts along [100] and [010]. 2·4CH2Cl2: Space group P$\bar{1}$, Z = 1, lattice dimensions at 100(2) K: a = 919.5(1), b = 1248.3(1), c = 2707.0(2) pm, α = 101.61(1) °, β = 95.08(1) °, γ = 94.52(1) °, R1 = 0.103. Compound 2 contains two different anionic complexes in the ratio 1:1. In {Be2(NCS)4(μ‐NCS)2}2–, the beryllium atoms are connected by (NCS)– bridging groups forming centrosymmetric eight‐membered Be2(NCS)2 rings with distances Be–N of 168(1) pm and Be–S of 235.2(9) pm. The second anion {Be2(NCS)6(μ‐H2N2C2S2)}2– consists of two {Be(NCS)3}– units, which are linked by the nitrogen atoms of the unique dimeric cyclo‐addition product of HNCS with Be–N distances of 179(1) pm.
Talk to us
Join us for a 30 min session where you can share your feedback and ask us any queries you have