Assembly of Mixed-Metal Cages Using Polyimido Antimony(III) Anions. Syntheses and Structures of [Sb3(NCy)4(HNCy)2]K·2(toluene), [Sb2(NCy)4]2M4 (M = Cu, Ag), and [Sb(NCy)3]2Pb3 (Cy = Cyclohexyl, C6H11)

Autor: Dominic S. Wright, Natalie L. Cromhout, Christopher N. Harmer, Moira-Ann Rennie, Michael A. Paver, Michael A. Beswick, and Alexander Steiner, Paul R. Raithby
Rok vydání: 1997
Předmět:
Zdroj: Inorganic Chemistry. 36:1740-1744
ISSN: 1520-510X
0020-1669
DOI: 10.1021/ic961108b
Popis: Transmetalation reactions of the polyimido Sb(III) anions [Sb(3)(NCy)(4)(HNCy)(2)](-), [Sb(2)(NCy)(4)](2)(-), and [Sb(NCy)(3)](3)(-) with metal sources allows the logical assembly of cage compounds containing various mixed-metal stoichiometries. The breadth of this approach is illustrated by the syntheses of [Sb(NCy)(4)(HNCy)(2)]K.2(toluene) (1), containing an early main group metal, [Sb(2)(NCy)(4)](2)M(4) (M = Cu (2), Ag (3)), containing transition metals, and [Sb(NCy)(3)Pb(3)] (4), containing a p-block metal. The low-temperature X-ray structures of complexes 1-4 have been determined. Crystal data: 1, monoclinic, space group C2/c, a = 18.418(3) A, b = 11.457(2) A, c = 24.798(6) A, beta = 90.24(2) degrees, Z = 4; 3, triclinic, space group Po, a = 11.501(2) A, b = 13.752(3) A, c = 22.868(5) A, alpha = 103.50(3) degrees, beta = 95.89(3) degrees, gamma = 96.71(3) degrees, Z = 2; 4, triclinic, space group Po, a = 11.071(2) A, b = 14.892(2) A, c = 17.262(2) A, alpha = 65.36(3) degrees, beta = 74.21(3) degrees, gamma = 70.70(3) degrees, Z = 2. The structure of 2 has been reported in preliminary form. The K(+) ion of 1 is coordinated by four of the N centers of the [Sb(3)(NCy)(4)(HNCy)(2)](-) ligand. In addition, beta-C(-H).K interactions involving four of the Cy groups and MeC(-H).K interactions involving two toluene molecules give the K(+) ion a 10-coordinate geometry. In 2 and 3, the N centers of two [Sb(2)(NCy)(4)](2)(-) dianions symmetrically coordinate a central M(4) square-planar core. The symmetrical complexation of three Pb(II) centers by two [Sb(NCy)(3)](3)(-) trianions produces an 11-membered polyhedral cage structure in 4.
Databáze: OpenAIRE
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