Inorganic Chemistry, Vol.40, No.18, 4780-4784, 2001
Synthesis and X-ray crystal structure determination of first examples of donor-functionalized terphenyl lanthanide complexes
The molecular structures of novel donor-functionalized terphenyl derivatives of trivalent ytterbium, yttrium, and samarium of composition [DaniPyb(mu (2)-Cl)(2)(mu (3)-Cl)Li(THF)](2) (1) and [DanipLn(mu (2)-Cl)(2)(mu (2)-Cl)Li(THF)(2)](2) (Ln = Y, 2; Ln = Sm, 3) are reported [Danip = 2,6-di(o-anisol)phenyl]. The complexes are obtained from the reaction of equimolar amounts of DanipLi and LnCl(3) (Ln = Yb, Y, Sm) in tetrahydrofuran at room temperature in 60% yield. 1.2 toluene crystallizes in the monoclinic space group P1. Crystal data for 1.2 toluene at 203 K: a = 9.7291(9) Angstrom; b = 12.7989(12) Angstrom; c = 13.4870(12) Angstrom; alpha = 91.553(2)degrees; beta = 103.957(2)degrees; gamma = 109.916(2)degrees; V = 1521.2(2) Angstrom (3); Z ' = 1; D-calcd = 1.615 g cm(-3); R1 = 3.43%. 2.toluene crystallizes in the monoclinic space group P1. Crystal data for 2.toluene at 203 K: a = 10.4152(10) Angstrom; b = 12.5783(12) Angstrom; c = 14.4640(14) Angstrom; alpha = 69.963(2)degrees; beta = 80.900(2)degrees; gamma = 66.603(2)degrees; V = 1633.3(3) Angstrom (3); Z = 1; D-calcd = 1.386 g cm(-3); R1 = 4.07%. 3.toluene crystallizes in the monochnic space group P1. Crystal data for 3.toluene at 203 K: a = 10.3457(8) Angstrom; b = 12.5658(10) Angstrom; c = 14.4365(11) Angstrom; alpha = 70.2250(10)degrees; beta = 81.2820(10)degrees; gamma = 66.8330(10)degrees; V = 16233(2) Angstrom (3); Z ' = 1; D-calcd = 1.521 g cm(-3); R1 = 3.40%. Complexes 1-3 represent first examples of donor-functionalized terphenyl complexes of the elements ytterbium, yttrium, and samarium, respectively. The molecular structures of 1-3 feature a "constraint geometry" type arrangement of the Danip ligand at the lanthanide atom. The,complexes reported are dimeric and composed of lithium chloride bridged DanipLnCl(2), moieties (Ln = Yb, Y, Sm), stabilized through additional coordination of two methoxy functions to the lanthanide atom.