Oxacalix[3]arene Complexes with the ReI(CO)3 Fragment†
dataset
posted on 2006-08-21, 00:00 authored by Matthias Hinrichs, Florian R. Hofbauer, Peter Klüfers, Mihael SuhanjiOxacalix[3]arenes p-methyloxacalix[3]arene (L1), p-isopropyloxacalix[3]arene (L2), and p-ethoxycarbonyloxacalix[3]arene (L3) are able to bind the ReI(CO)3 moiety with two of their three phenol-O atoms and one of their ether-O
atoms. The monoanionic complexes were isolated in the salts (DBUH)[Re(CO)3(L1H-2)]·L1 (1) and (NEt4)[Re(CO)3(L2H-2)]·L2·0.5 MeCN (2) (DBU = 1,8-diazabicyclo[5.4.0]undec-7-ene). Over the course of its reaction with
(NEt4)2[Re(CO)3Br3] and DBU, p-ethoxycarbonyloxacalix[3]arene decomposes to form [{Re(CO)3(L4H-2)}2] (3) {L4
= 1-(5-ethoxycarbonyl-2-hydroxy-3-hydroxymethyl-benzyl)-2,3,4,6,7,8,9,10-octahydro-pyrimido[1,2-a]azepin-1-ium.
The expected monoanion [Re(CO)3(L3H-2)]- (4) was identified by 13C NMR and mass spectra.
