Treatment of [(C3H5)3P]3Pt with BCls affords [(C6H6)3P]3Pt•2BCls whereas [(CeHsLPLPt affords [(CeH5)3P]3Pt•2BCl3 and (CSH5)3P-BC13. Reaction of [(C6H5)3P]3Pt-2BCl3 with pyridine (py) yields py-BCl3 while pyrolysis of the adduct affords benzene. Treatment of [(C6H5)3P]2Pt'SiF4 with BC13 yields [(CeHslsPLPt'BCla whereas reaction with [A1(CH3)3L affords a paramagnetic Pt species and mixed fluoromethylsilanes. Reaction of [(C6H3)3Pj3Pt with [A1(CH3)3]2 results in the formation of [(CeHsLPLPt •2 1( 3)3 which readily decomposes in solution to yield two weakly paramagnetic species. One radical is associáted with Pt and the other with Al.3050 vw 1178 m 935 w 614 w 1582 w 1156 m, sh 840 w 539 vw 1570 vw 1092 s 750 s, sh 508 vs ("X" sensitive) 740 s 450 vw 1474 m 1024 w 704 s, sh 420 vw 1430 m 997 w 687 vs, b 1304 vw 970 vw
Treatment of 1,4-dihydridooctaphenyltetrasilane, HzSi4(C6H5)8, with bis(triphenylphosphine)ethyleneplatinum(O), [ (C&)3P]zPtCzH4, affords the first example of a transition metal incorporated into a silicon ring, [ (C,#S)~P]~-Pt[Si(C6Hs)z] $i(C6H5)2. Infrared and ultraviolet spectroscopic examinations are reported and compared with similar data recorded for [ ( C & )~P ]~P~C Z H~, Si4(C6H&, and Sis(C6H5)lo. Attempts at several alternate methods of synthesis are discussed as well as reaction of the cyclo-metallosilane with Brz and Hz.
Methods for the preparation of aluminum trihydride-diethyl etherate, AlH, -0.3 [ (C, H5 )2 01 ,$ have been published,'S2 but the absence of complete experimental details makes duplication difficult. The following procedure is a modification of that reported by Finholt, Bond, and Schlesinger.' Problems inherent in previous methods, such as premature precipitation, decomposition of the alane, and lithium chloride contamination, are avoided.Premature precipitation is controlled by maintaining a low temperature (-5'C.) in the reaction mixture. Purified reactants, as well as minimal exposure to light and higher temperatures, *The Dow Chemical Company, Midland, Mich. 48640. This work was supported by +Ohio State University, Columbus, Ohio 43210. SEbdiometric molecular weight determinations obtained in diethyl ether (concentration range, 0.25-1.0 M ) indicates molecular weights only slightly higher than 30. This is consistent with studies reported by Wiberg and U~o n .~ It must be assumed that in solution, AM, exists essentially as the monomeric form.ARPA and the Air Force under contracts AF 33(616)-6149 and AF 04(611)-7554.
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