Kent State University, Department of Chemistry, Kent, Ohio 44242, USA.
Inorg Chem. 2009 Mar 16;48(6):2701-6. doi: 10.1021/ic802291u.
The addition of diethylcyanamide to a tetrahydrofuran solution of lithium dialkylamide {LiN(CH(3))(2) or LiN[upper bond 1 start]CH(2)CH(2)C[upper bond 1 end]H(2) CH(2), 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(SiMe(3))(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(SiMe(3))(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, (1)H and (13)C NMR studies.
将二乙氰酰胺加入四氢呋喃溶液中的二锂酰胺（LiN(CH(3))(2)或 LiN[上键 1 开始]CH(2)CH(2)C[上键 1 结束]H(2) CH(2)，Li(PYR)）中，得到相应的锂 1,1,3,3-四烷基胍盐，Li(TAG)。随后，将 2 当量的 Li(TAG)和 2 当量的双三甲基甲硅烷基酰胺锂，LiN(SiMe(3))(2)，与 4 当量的第 11 族卤化物（CuCl、AgBr 和 AuCl）反应，生成具有通式M(2)(mu-TAG){mu-N(SiMe(3))(2)}的四核配合物，其中 M 和 TAG = {Cu、DEDMG、(1)}、{Ag、DEDMG、(2)}、{Au、DEDMG、(3)}、{Cu、DEPYRG、(4)}、{Ag、DEPYRG、(5)}和{Au、DEPYRG、(6)}。化合物 1-6 通过单晶 X 射线衍射进行了表征。所有配合物的块状粉末均通过元素分析、FT-IR 光谱、(1)H 和 (13)C NMR 研究与晶体结构相符。
