ASSEMBLY OF MIXED-METAL CAGES USING POLYIMIDO ANTIMONY(III) ANIONS - SYNTHESES AND STRUCTURES OF [SB-3(NCY)(4)(HNCY)(2)]K-CENTER-DOT-2(TOLUENE), [SB-2(NCY)(4)](2)M-4 (M=CU, AG), AND [SB(NCY)(3)](2)PB-3 (CY EQUALS CYCLOHEXYL, C6H11)
Ma. Beswick et al., ASSEMBLY OF MIXED-METAL CAGES USING POLYIMIDO ANTIMONY(III) ANIONS - SYNTHESES AND STRUCTURES OF [SB-3(NCY)(4)(HNCY)(2)]K-CENTER-DOT-2(TOLUENE), [SB-2(NCY)(4)](2)M-4 (M=CU, AG), AND [SB(NCY)(3)](2)PB-3 (CY EQUALS CYCLOHEXYL, C6H11), Inorganic chemistry, 36(9), 1997, pp. 1740-1744
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 so
urces allows the logical assembly of cage compounds containing various
mixed-metal stoichiometries. The breadth of this approach is illustra
ted by the syntheses of [Sb(NCy)(4)(HNCy)(2)]K . 2 (toluene) (1), cont
aining 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), contain
ing 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 = 18.318(3) Angstrom, b = 11.457(2) Angstrom, c = 24.798(6) Angs
trom, beta = 90.24(2)degrees, Z = 4; 3, triclinic, space group P (1) o
ver bar, a = 11.501(2) Angstrom, b = 13.752(3) Angstrom, c = 22.868(5)
Angstrom, alpha = 103.50(3)degrees, beta = 95.89(3)degrees, gamma = 9
6.71(3)degrees, Z = 2; 4, triclinic, space group P (1) over bar, a = 1
1.071(2) Angstrom, b = 14.892(2) Angstrom, c = 17.262(2) Angstrom, alp
ha = 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 invo
lving four of the Cy groups and MeC(-H)... K interactions involving tw
o 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 coo
rdinate 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.