THE SYNTHESIS AND CHARACTERIZATION OF VOLATILE COMPLEXES OF FLUORINATED ALKOXIDES OF YTTRIUM - X-RAY STRUCTURES OF [Y(OCME(CF3)2)3(THF)3] AND [Y(OCME(CF3)2)3(DIGLYME)]

From the reactions of (CF3)2CHOH (hfip.H), (CF3)Me2COH (tftb.H) and (CF3)2MeCOH (hftb.H) with Y{N(SiMe3)2}3 in benzene, thf or diethyl ether as solvents the following compounds have been isolated and characterized by elemental analysis, IR, NMR and mass spectroscopy: [Y{OCMe2(CF3)}3]n (1), [Y{OCMe2(CF3)}3(thf)2.5] (2), [Y{OCMe(CF3)2}3]n (3), [Y{OCMe(CF3)2}3(NH3)0.5] (4), [Y{OCMe(CF3)2}3(NH3)3] (5), [Y{OCMe(CF3)2}3(thf)3] (6), [Y{OCMe(CF3)2}3(Et2O)0.33] (7), [Y{OCMe(CF3)2}3 (diglyme)] (8), [Y{OCMe(CF3)2}3(ButOH)3] (9), [Y{OCH(CF3)2}3(NH3)0.5] (10) and [Y{OCH(CF3)2}3(thf)3] (11). Sublimation in vacuo is usually accompanied by loss of some of the neutral ligand, but 8 sublimes intact. Single-crystal X-ray structures of 6 and 8 showed that these mononuclear octahedral complexes have the facial configuration. Y-89 NMR chemical shifts were obtained for 2, delta 93.66; 6, 66.44; 8, 78.63; and 11, 82.78.