126423-24-3Relevant articles and documents
Synthesis and structural and spectroscopic characterization of the germanazene [GeN(2,6-i-Pr2C6H3)]3 and the tin and lead tetramers [SnN(BMes2)]4, [SnN(2,6-i-Pr2C6H3)]4, and [PbN(2,6-i-Pr2C6H3)]4
Chen, Hong,Bartlett, Ruth A.,Dias, H. V. Rasika,Olmstead, Marilyn M.,Power, Philip P.
, p. 3390 - 3394 (2008/10/08)
The reactions of M[N(SiMe3)2]2 (M = Ge, Sn, Pb) with two bulky primary amines have been investigated. When Ge[N(SiMe3)2]2 was treated with H2N(Dipp) (Dipp = 2,6-i-Pr2C6H3), the trimeric species [GeN(Dipp)]3 (1) was formed in high yield. The reaction of Sn[N(SiMe3)2]2 with H2N(Dipp) or the primary borylamine H2NBMes2 gives the tetrameric species [SnN(Dipp)]4 (2) and [SnN(BMes2)]4 (3). The lead compound [PbN(2,6-i-Pr2C6H3)]4 (4) was prepared in a similar manner. Details of the 1H NMR spectroscopy and X-ray crystal structures of all compounds are reported. The trimer [GeN(Dipp)]3 (1), which was described in a preliminary communication, has a planar Ge3N3 ring structure with stereochemically active Ge lone pairs. The structures of 2-4 are tetrameric, featuring Sn4N4 or Pb4N4 cubane skeletons. The data suggest considerable ionic character in the M-N bonds. Crystal data [Mo Kα (λ = 0.71069 A?)] at 130 K are as follows: 2, a = 12.214 (2) A?, b = 19.129 (4) A?, c = 21.488 (4) A?, α = 84.27 (1)°, β = 76.15 (1)°, γ = 86.78 (1)°, Z = 4, triclinic, space group P1, 9463 unique observed (I > 2σ(I)) data, R(F) = 0.050; 3, a = 28.185 (8) A?, c = 35.161 (11)A?, Z= 12, tetragonal, space group I4c2, 5199 unique observed (I > 3σ(I)) data, R(F) = 0.083; 4, a = 12.330 (3) A?, b = 19.242 (4) A?, c = 21.435 (6) A?, α = 83.06 (2)°, β = 76.61 (2)°, γ = 85.97 (2)°, Z = 4, triclinic, space group P1, 11 095 unique observed (I > 2σ(I)) data, R(F) = 0.074.