Abstract
Raman and NMR spectroscopy were used to establish the structure and stability of several MCl 4· 2Ladducts (M=Zr, Hf; L=neutral Lewis base) in CHCl 3 and CH 2Cl 2. Only trans adducts were found for MCl 4·2(Me 2N) 3PO, cis-trans equilibria were observed for HfCl 4·2Cl 2(Me 2N)PO, MCl 4·2Cl(Me 2N) 2- PO and MCl 4·2(MeO) 3PO and only the cis configuration was present for ZrCl 4·2Cl 2(Me 2N)PO, MCl 4· 2Cl 2(MeO)PO and MCl 4·2L (L=Me 2O, Me 2S, Me 2Se, Cl 3PO). 1H NMR was used to determine the relative stabilities of some of the adducts and the sequence found was: (Me 2N) 3PO⪢Cl(Me 2N) 2PO > (MeO) 3PO⪢Cl(MeO) 2PO>Cl 2(Me 2N)PO). The observed structures and stabilities are explained using steric and electronic arguments. A variable pressure study of the cis-trans equilibrium on ZrCl 4·2(MeO) 3- PO yielded the reaction volume, δ V°=+3.8±0.4 cm 3mol −1
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