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)]

Abstract From the reactions of (CF 3 ) 2 CHOH (hfip.H), (CF 3 )Me 2 COH (tftb.H) and (CF 3 ) 2 MeCOH (hftb.H) with Y{N(SiMe 3 ) 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{OCMe 2 (CF 3 )} 3 ] n ( 1 ), [Y{OCMe 2 (CF 3 )} 3 (thf) 2.5 ] ( 2 ), [Y{OCMe(CF 3 ) 2 } 3 ] n , ( 3 ), [Y{OCMe(CF 3 ) 2 } 3 (NH 3 ) 0.5 ] ( 4 ), [Y{OCMe(CF 3 ) 2 } 3 (NH 3 ) 3 ] ( 5 ), [Y{OCMe(CF 3 ) 2 } 3 (thf) 3 ] ( 6 ), [Y{OCMe(CF 3 ) 2 } 3 (Et 2 O) 0.33 ] ( 7 ), [Y{OCMe(CF 3 ) 2 } 3 (diglyme)] ( 8 ), [Y{OCMe(CF 3 ) 2 } 3 (Bu t OH) 3 ] ( 9 ), [Y{OCH(CF 3 ) 2 } 3 (NH 3 ) 0.5 ] ( 10 ) and [Y{OCH(CF 3 ) 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. 89 Y NMR chemical shifts were obtained for 2 , δ 93.66; 6 , 66.44; 8 , 78.63; and 11 , 82.78.