A SIMPLE SYNTHETIC ROUTE TO N,N'-DIALKYL-2,11-DIAZA[3.3](2,6)-PYRIDINOPHANES - CRYSTAL-STRUCTURES OF N'-DI-TERT-BUTYL-2,11-DIAZA[3.3](2,6)PYRIDINOPHANE AND ITS COPPER(II) COMPLEX
Cm. Che et al., A SIMPLE SYNTHETIC ROUTE TO N,N'-DIALKYL-2,11-DIAZA[3.3](2,6)-PYRIDINOPHANES - CRYSTAL-STRUCTURES OF N'-DI-TERT-BUTYL-2,11-DIAZA[3.3](2,6)PYRIDINOPHANE AND ITS COPPER(II) COMPLEX, Polyhedron, 13(5), 1994, pp. 771-776
Reaction of 2,6-bis(bromomethyl)pyridine with primary amines gave the
12-membered N,N'-dialkyl-2,11-diaza[3.3](2,6)pyridinophanes. The struc
tures of N'-di-tert-butyl-2,11-diaza[3.3](2,6)pyridinophane (4) and it
s copper(II) derivative [Cu(4)Cl2] (7) have been characterized by X-ra
y crystal analysis. The average axial Cu-N (tertiary amine) distance o
f 2.490 angstrom in 7 is appreciably longer than the related value of
2.347 angstrom in Cu(6)Cl2 . H2O.4 In 4, the two planar pyridyl rings
are not in the same plane, but roughly parallel and the 12 atoms of th
e macrocyclic ring constitute a syn chair-chair conformation. In compl
ex 7, the copper(II) ion adopts a distorted octahedral geometry, in wh
ich the tertiary amine nitrogen atoms span axial positions approximate
ly normal to the square plane formed by the two pyridine nitrogens and
the chloro ligands. The average Cu-N (tertiary amine), Cu-N(pyridine)
and Cu-Cl distances are 2.49(2), 2.03(2) and 2.287(7) angstrom, respe
ctively.