[(ArO)(2)(THF)Y(mu-OAr>](2) (Ar = C(6)H(3)Me(2)-2,6) reacts with Al(2)Me(6) or AlE(3) in toluene or hexanes to form the mixed-metal products (ArO)(2)(THF)(2)Y(mu-OAr)(2)AlR(2) [R - Me (1), Et(2)]. These complexes can be obtained in quantitative yield from [AlR(2)(OAr)](2) and Y(OAr)(3)(THF)(3) in toluene. Yb and Nd analogs of 1 and 2 can be obtained similarly, and the representative complexes (ArO)(2)(THF)(2)Yb(mu-OAr)(2)AlMe(2), 3, and (ArO)(2)(THF)(2)Nd-(mu-OAr)(2)A1Et(2), 4, were crystallographically characterized. Complexes 1-4 all crystallize from benzene in the same space group C2/c. Unit cell parameters at 298 K follow : 1, a = 24.148(3) Angstrom, b = 12.396(3) Angstrom, c = 18.677(2) Angstrom, beta = 118.68(8)degrees, V = 4704(1) Angstrom(3), Z = 4; 2, a = 21.790 Angstrom, b = 13.039 Angstrom, c = 19.434 Angstrom, beta = 111.68 degrees, V = 5128 Angstrom(3); 3, a = 23.881(9) Angstrom, b = 12.035(7) Angstrom, c = 18.676(6) Angstrom, beta = 118.74(2)degrees, V = 4706(3) Angstrom(3), z = 4; 4, a = 23.185(2) Angstrom, b = 13.128(1) Angstrom, c = 18.905(2) Angstrom, beta = 117.65(1)degrees, V = 5096(1) Angstrom(3), Z = 4 In the case of 3, least-squares refinement of the model based on 2500 reflections (F-0 > 4.0 sigma(F-0)) converged to a final R(F) = 7.6%. For 4 the model based on 2243 reflections (F-0 > 4.0 sigma(F-0)) converged to a final R(F) = 7.2%. Complexes 1, 3, and 4 have distorted octahedral and tetrahedral coordination environments around lanthanide and aluminum, respectively.