Complexes of ligands providing endogenous bridges. Part 7. The concurrent formation of 1 + 1 and 2 + 2 oxa-azamacrocycles; the X-ray crystal structure of an exocyclic dinuclear copper(II) complex
- 1 January 1989
- journal article
- research article
- Published by Royal Society of Chemistry (RSC) in J. Chem. Soc., Dalton Trans.
- No. 9,p. 1727-1738
- https://doi.org/10.1039/dt9890001727
Abstract
A series of oxa-azamacrocycles derived from the non-template condensation of 1,3-diamino-2-propanol and acyclic dialdehydes followed by in situ reduction with tetrahydroborate has been prepared. Fast atom bombardment mass spectrometry (f.a.b.m.s.) showed the presence of 1 + 1 and 2 + 2 condensates and these were separated using medium pressure liquid chromatography. Metal complexes of the 1 + 1 macrocycles (HL) were prepared and characterised. Mononuclear complexes, M (HL)X2, were recovered for M = CoII, NII, ZnII, CdII, or HgII and X = Cl or Br and homo-dinuclear complexes, Cu2LCl2(OH)·nH2O, for CuCl2. The salts M(ClO4)2 and M(NO3)2(M = CoII, NiII, CuII, ZnII, or CdII) gave complexes [M(L)X] and f.a.b.m.s. provided evidence for oligomer formation. Mononuclear complexes were recovered from the reaction of one 2 + 2 macrocycle with M(ClO4)2(M = CoII, NiII, or ZnII) and CdCl2, whereas a homodinuclear complex was obtained for Cu(ClO4)2. The crystal structure of [Cu2(µ-C19H23N2O3)(µ-O2CPh)(OH2)Cl2]·2PhCH2OH reveals a dimeric structure in which the dinuclear units are linked by chloride bridges. The compound crystallises in monoclinic space group P21/c(C2h 5 no. 14) with unit-cell dimensions a= 13.460(15), b= 14.608(16), c= 17.096(8)Å, β= 96.227(9)°, and Z= 2; 3 678 independent reflections with I/σ(I) > 3.0 gave R= 0.0532.Keywords
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