Sm. Harben et al., RHENIUM AND MOLYBDENUM OXO-COMPLEXES CONTAINING LIGANDS RELATED TO N-HYDROXYIMINODIPROPIONIC ACID, Journal of the Chemical Society. Dalton transactions, (16), 1997, pp. 2777-2784
The reaction of N-hydroxy-2,2'-iminodipropionic acid with [PPh4][ReOBr
4], [ReOCl3(PPh3)(3)], [ReOCl2(OEt)(PPh3)(2)] or [PPh4][MoOCl4(H2O)] h
as produced four novel complexes: [ReOBr3(C6H8NO5)](-), [ReOBr3(C3H3NO
2)](-), [ReOCl2(R,S-idpa)](-)(H(3)idpa = 2,2'-iminodipropionic acid) a
nd [MoO2Cl2(C3H4NO3)](-). All have been successfully crystallised as t
heir [PPh4](+) salts which have been characterised by single-crystal X
-ray diffraction. The anions [ReOBr3(C6H8NO5)](-)and [ReOBr3(C3H3NO2)]
(-) involve tetragonally distorted octahedral (ReOBr3)-O-V (N,O) centr
es with the bromides cis to the oxo-group; [ReOCl2(R,S-idpa)](-) invol
ves a tetragonally distorted octahedral (ReOCl2)-O-V (O,N,O) centre wi
th the 2Cl cis and O trans to the ore-group; [MoO2Cl2(C3H4NO3)](-) inv
olves a skew-trapezoidal (MoO2Cl2)-O-VI (N,O) centre with essentially
mutual cis ore-groups and trans chloro-groups. The dimensions of each
of these co-ordination spheres are generally typical of related comple
xes; however, [ReOBr3(C3H3NO2)](-) involves an unusually short Re-O-ox
o bond of 1.45(4) Angstrom. The organic moieties are considered to ari
se from rearrangement and/or fragmentation of N-hydroxy-2,2'-iminodipr
opionic acid, presumably under the influence of the metal centre.