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Inorganics 2015, 3(4), 429-447;

New Lanthanide Alkynylamidinates and Diiminophosphinates

Organometallic and Organometalloid Chemistry Department, National Research Centre, 12622 Cairo, Egypt
Chemisches Institut der Otto-von-Guericke-Universität Magdeburg, 39106 Magdeburg, Germany
Author to whom correspondence should be addressed.
Academic Editors: Stephen Mansell and Steve Liddle
Received: 7 October 2015 / Revised: 23 October 2015 / Accepted: 27 October 2015 / Published: 5 November 2015
(This article belongs to the Special Issue Rare Earth and Actinide Complexes)
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This contribution reports the synthesis and structural characterization of several new lithium and lanthanide alkynylamidinate complexes. Treatment of PhC≡CLi with N,N′-diorganocarbodiimides, R–N=C=N–R (R = iPr, Cy (cyclohexyl)), in THF or diethyl ether solution afforded the lithium-propiolamidinates Li[Ph–C≡C–C(NCy)2] S (1: R = iPr, S = THF; 2: R = Cy, S = THF; 3: R = Cy, S = Et2O). Single-crystal X-ray diffraction studies of 1 and 2 showed the presence of typical ladder-type dimeric structures in the solid state. Reactions of anhydrous LnCl3 (Ln = Ce, Nd, Sm or Ho) with 2 in a 1:3 molar ratio in THF afforded a series of new homoleptic lanthanide tris(propiolamidinate) complexes, [Ph–C≡C–C(NCy)2]3Ln (4: Ln = Ce; 5: Ln = Nd; 6: Ln = Sm; 7: Ln = Ho). The products were isolated in moderate to high yields (61%–89%) as brightly colored, crystalline solids. The chloro-functional neodymium(III) bis(cyclopropylethynylamidinate) complex [{c-C3H5–C≡C–C(NiPr)2}2Ln(µ-Cl)(THF)]2 (8) was prepared from NdCl3 and two equiv. of Li[c-C3H5–C≡C–C(NiPr)2] in THF and structurally characterized. A new monomeric Ce(III)-diiminophosphinate complex, [Ph2P(NSiMe3)2]2Ce(µ-Cl)2Li(THF)2 (9), has also been synthesized in a similar manner from CeCl3 and two equiv. of Li[Ph2P(NSiMe3)2]. Structurally, this complex resembles the well-known “ate” complexes (C5Me5)2Ln(µ-Cl)2Li(THF)2. Attempts to oxidize compound 9 using trityl chloride or phenyliodine(III) dichloride did not lead to an isolable cerium(IV) species. View Full-Text
Keywords: amidinate; alkynylamidinate; diiminophosphinate; lithium; lanthanide complexes; crystal structure amidinate; alkynylamidinate; diiminophosphinate; lithium; lanthanide complexes; crystal structure

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Sroor, F.M.; Hrib, C.G.; Edelmann, F.T. New Lanthanide Alkynylamidinates and Diiminophosphinates. Inorganics 2015, 3, 429-447.

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