Polynuclear cyclohexasiloxanolates M(6)L(2) and M(n)M'(6-n)L(2) (M, M'
= Ni, Mn, Fe; L = [-SiPh(O)O-](6)) were studied as precursors of supp
orted catalysts. Synchrotron EXAFS data (Novosibirsk VEPP-3 storage ri
ng, 2.5 GeV, 120 mA, Si[111] monochromator) revealed three closest coo
rdination spheres: M-O (2.0-2.2 Angstrom), M ... M (2.72-2.98 Angstrom
) and M ... Si (3.31-3.40 Angstrom). Interatomic distances for M = Ni
or Mn agree with the known X-ray structures of 'tubular' M(6)(mu(2)-O)
(12) cores.