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  • Title: Synthetic and theoretical study of the incorporation of metal halides in [{Ti(eta5-C5Me5)(mu-NH)}3(mu3-N)].
    Author: García-Castro M, Gracia J, Martín A, Mena M, Poblet JM, Sarasa JP, Yélamos C.
    Journal: Chemistry; 2005 Jan 21; 11(3):1030-41. PubMed ID: 15614870.
    Abstract:
    The capacity of the imido-nitrido organometallic ligand [{Ti(eta5-C5Me5)(mu-NH)}3(mu3-N)] (1) to entrap main group metal halides MXn has been investigated. Treatment of 1 with metal halides in toluene or dichloromethane afforded several soluble adducts [MXn(L)] (L=1) in good yields. The reaction of 1 with one equivalent of Group 1 and 13 monohalides MX afforded single cube-type complexes [XM{(mu3-NH)3Ti3(eta5-C5Me5)3(mu3-N)}] (M=Li, X=Br (2), I (3); M=Na, X=I (4); M=In, X=I (5); M=Tl, X=I (6)). Analogous treatment of 1 with Group 2 and 14 dihalides MX(2) gave the corresponding adducts [I2M{(mu3-NH)3Ti3(eta5-C5Me5)3(mu3-N)}] (M=Mg (7), Ca (8), Sr (9)) and [Cl(2)M{(mu3-NH)3Ti3(eta5-C5Me5)3(mu3-N)}] (M=Sn (10), Pb (11)). The treatment of 1 with SnI2 or the reaction of 10 with MeI at 60 degrees C afforded two azametallocubane units linked by two bridging iodine atoms [{ISn(mu3-NH)3Ti3(eta5-C5Me5)3(mu3-N)}2(mu-I)2] (12). Indium triiodide reacted with 1 in toluene to form the adduct [I3In(mu3-NH)3Ti3(eta5-C5Me5)3(mu3-N)] (13). Density functional theory calculations have been carried out to study these processes and evaluate the influence of the solvent. X-ray crystal structure determinations have been performed for complexes 10, 12, and 13.
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