412358-25-9Relevant academic research and scientific papers
Synthesis and structural characterization of 2,6-dimesitylphenyl complexes of scandium, ytterbium, and yttrium
Rabe, Gerd W.,Berube, Christian D.,Yap, Glenn P. A.,Lam, Kin-Chung,Concolino, Thomas E.,Rheingold, Arnold L.
, p. 1446 - 1453 (2002)
The molecular structures of a number of 2,6-dimesitylphenyl-based (2,6-dimesitylphenyl = Dmp) complexes of the group 3 elements scandium and yttrium as well as of the lanthanide element ytterbium are reported. Reaction of 1 equiv of DmpLi with 1 equiv of MCl3 (M = Sc, Yb, Y) in tetrahydrofuran at room temperature followed by crystallization from toluene/hexanes at -30°C produces DmpMCl2(THF)2 (M = Sc: 1; M = Yb: 2) and DmpMCl2(THF)3 (M = Y: 3), respectively. The one-pot reaction of DmpLi with 1 equiv of YbCl3 in tetrahydrofuran at room temperature followed by addition of 1 equiv of KOtBu produces the heterobimetallic monoalkoxide complex DmpYb-(THF)(OtBu)(μ-Cl)2Li(THF)2 (4), which was crystallized from toluene/tetrahydrofuran (20:1) at - 30°C. Crystal data for 1: monoclinic, P21/n; T = 203 K; a = 10.178(3) A; b = 15.468(3) A; c = 20.132(5) A; β = 101.85(3)°; V = 3102.0(17) A3; Z′ = 4; Dcalcd = 1.228 g cm-3; R1 = 5.89%. Crystal data for 2: monoclinic, P21/n; T = 173 K; a = 10.2447(7) A; b = 15.5683(12) A; c = 20.0979(14) A; β = 101.749(4)°; V = 3238.3(5) A3; Z′ = 4; Dcalcd = 1.485 g cm-3; R1= 4.32%. Crystal data for 3: monoclinic, P21/n; T = 203 K; a = 15.950(3) A; b = 11.865(2) A; c = 18.254(3) A; β = 92.323(3)°; V = 3451.9(10) A3; Z′ = 4; Dcalcd = 1.327 g cm-3; R1 = 4.43%. Crystal data for 4: triclinic, P1; T = 193 K; a = 10.2252(2) A; b = 11.3497(2) A; c = 18.5814(2) A; α = 98.7353(6)°; β = 102.8964(6)°; γ = 94.8058(5)°; V = 2062.09(5) A3; Z′ = 2; Dcalcd = 1.375 g cm-3; R1 = 4.56%. The molecular structures of 1-3 feature monomeric complexes with distorted trigonal-bipyramidal (1 and 2) or octahedral (3) coordination geometry about the metal atom, with the two chlorine atoms occupying the axial positions. 4 represents the first example of an alkoxide derivative of a terphenyl lanthanide complex. The molecular structure of the ate complex 4 exhibits a heavily distorted trigonal-bipyramidal coordination polyhedron about the ytterbium atom, with one of the μ chlorine atoms and the oxygen atom of the tetrahydrofuran ligand representing the axial positions of the trigonal-bipyramidal arrangement. A terminal alkoxide ligand is another main feature of the molecular structure of complex 4.
