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Inorganic Chemistry, Vol.48, No.6, 2701-2706, 2009
Synthesis and Characterization of Group 11 1,1,3,3-Tetraalkylguanidinate (TAG) Clusters: [M-2(mu-TAG){mu-N(SiMe3)(2)}](2) (M = Cu, Ag, and Au)
The addition of diethylcyanamide to a tetrahydrofuran solution of lithium dialkylamide {LiN(CH3)(2) or LiNCH2CH2CH2CH2, Li(PYR)} results in the corresponding lithium 1,1,3,3-tetraalkylguanidinate, Li(TAG). Two equivalents of Li(TAG) and 2 equiv of lithium bistrimethylsilylamide, LiN(SiMe3)(2), were subsequently reacted with 4 equiv of Group 11 halide (CuCl, AgBr, and AuCl) to generate tetranuclear complexes with the general formula [M-2(mu-TAG){mu-N(SiMe3)(2)}](2) where M and TAG = {Cu, DEDMG, (1)}, {Ag, DEDMG, (2)}, {Au, DEDMG, (3)}, {Cu, DEPYRG, (4)}, {Ag, DEPYRG, (5)}, and {Au, DEPYRG, (6)}. Compounds 1-6 were characterized by single-crystal X-ray diffraction. The bulk powders for all complexes were found to be in agreement with the crystal structures based on elemental analyses, FT-IR spectroscopy, H-1 and C-13 NMR studies.