Structural Studies of Piperidino‐Alanes with Halide, Amide and Hydride as further Ligands at Aluminum

Michael Veith, Tatjana Kirs, Bernd Morgenstern, Volker Huch
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Abstract

Nine different derivatives of piperidino alanes of the general formula (CH2)5N‐AlXY [X=Y= Cl (1), Br (2), I (3); X= (CH2)5N, Y= Cl (4), Br (5), I (6); X=H, Y= Cl (7), Br (8), I (9)] have been synthesized and compared with respect to their structures. All molecules form dimers with an Al2N2 central cycle and aluminum and nitrogen atoms in distorted tetrahedral environments as determined from X‐ray diffraction. The three dihalide derivatives 1, 2 and 3 have C2h (2/m) symmetries in solution of which they maintain the Centro symmetry in the crystal lattice. The bis(piperidino) derivatives 4, 5 and 6 have either C1 (1) symmetry with the bridging piperidino cycles oriented in the same direction (4, 5) or Ci (ī) point symmetry as found for 6 (in solution at least one other isomer is present). Whereas the chlorine derivative 7 has crystallographic Ci (ī) symmetry, the bromine 8 has almost C2 and the iodine 9 crystallographic C2 (2) point symmetry. In solution all derivatives 7, 8, 9 show equilibria between cis (C2) and trans (Ci) isomeric forms (27Al NMR). The longest Al‐N bond lengths within the rings are found for 5 (1.969(4) Å) and the shortest for 8 (1.940(4) Å).
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以卤化物、酰胺和氢化物作为铝的进一步配体的哌啶烷结构研究
我们合成了通式为 (CH2)5N-AlXY [X=Y= Cl (1)、Br (2)、I (3);X= (CH2)5N,Y= Cl (4)、Br (5)、I (6);X=H,Y= Cl (7)、Br (8)、I (9)]的九种不同的哌啶烷衍生物,并对它们的结构进行了比较。根据 X 射线衍射测定,所有分子都形成二聚体,具有 Al2N2 中心循环,铝原子和氮原子处于扭曲的四面体环境中。三种二卤化物衍生物 1、2 和 3 在溶液中具有 C2h (2/m) 对称性,它们在晶格中保持了 Centro 对称性。双(哌啶基)衍生物 4、5 和 6 要么具有 C1 (1) 对称性,桥接的哌啶基循环方向相同(4、5),要么像 6 一样具有 Ci (ī) 点对称性(在溶液中至少存在另一种异构体)。氯衍生物 7 具有晶体学上的 Ci (ī) 点对称性,溴衍生物 8 几乎具有 C2 点对称性,碘衍生物 9 具有晶体学上的 C2 (2) 点对称性。在溶液中,所有衍生物 7、8 和 9 都显示出顺式(C2)和反式(Ci)异构体之间的平衡(27Al NMR)。环内 Al-N 键长度最长的是 5(1.969(4) Å),最短的是 8(1.940(4) Å)。
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