SYNTHESIS AND MOLECULAR-STRUCTURE OF THE TRINUCLEAR MIXED-METAL COMPLEX [((ME2NCH2CH2CH2)2CR(MU-CL)2)2MG] AND OF THE TETRANUCLEAR GRIGNARD-REAGENT [(ME2NCH2CH2CH2)MG2CL3(THF)2]2
U. Casellato et F. Ossola, SYNTHESIS AND MOLECULAR-STRUCTURE OF THE TRINUCLEAR MIXED-METAL COMPLEX [((ME2NCH2CH2CH2)2CR(MU-CL)2)2MG] AND OF THE TETRANUCLEAR GRIGNARD-REAGENT [(ME2NCH2CH2CH2)MG2CL3(THF)2]2, Organometallics, 13(10), 1994, pp. 4105-4108
CrCl3.3THF reacts with [(Me2NCH2CH2-CH2)Mg2Cl3(THF)2]2 (1) in THF at r
oom temperature to form the complex [{(Me2NCH2CH2CH2)2Cr(mu-Cl)2}2Mg[
(2). The solid-state structures of 1 and 2 have been determined by X-r
ay crystal analysis. 1 is triclinic, space group P1BAR (No. 2), with a
= 10.035(8) angstrom, b = 10.393(8) angstrom, c = 10.707(8) angstrom,
alpha = 75.59(6)-degrees, beta = 68.61(6)-degrees, gamma = 75.28(7)-d
egrees, and Z = 1 (the asymmetric unit is half of the molecule); the s
tructure was refined to a conventional R factor of 0.079. In this tetr
anuclear Grignard reagent 1 Mg and Cl atoms form a system of five four
-membered bridging units, where the Mg atoms exhibit five and six coor
dination and are connected by doubly (mu) or triply (mu3) bridging chl
oro ligands. 2 is triclinic, space group P1BAR (No. 2), with a = 8.514
(8) angstrom, b = 12.471(9) angstrom, c = 14.976(9) angstrom, alpha =
81.54(5)-degrees, beta = 92.52(6)-degrees, gamma = 95.32(6)-degrees, a
nd Z = 2; the structure was refined to R = 0.064. 2 is a trinuclear co
mplex with two (Me2NCH2CH2CH2)2Cr(mu-Cl)2 fragments attached either si
de of a central Mg atom through four Cr-Cl-Mg bridges.