Synthesis and Characterization of Some New 22‐Membered Chalcogenoaza Macrocycles and Their Co
<sup>II</sup>
and Ni
<sup>II</sup>
Complexes
作者:Upali Patel、Harkesh B. Singh、Ray J. Butcher
DOI:10.1002/ejic.200600495
日期:2006.12
X-ray diffraction studies. The crystal structure of 14 consists of a distorted octahedral nickel center coordinated by two selenium and four nitrogen atoms. Complex 14: hexagonal, space group P61, a = 17.0747(16), b = 17.0747(16), c = 29.958(4) A, Z = 6. CoII complexes 15 and 16 of selenaaza macrocycles were prepared by the reaction of Co(ClO4)2·6H2O with 11 and 3, respectively. Complex 16: monoclinic
双(邻甲酰基苯基)硫属元素化物 (9, 10) 与反式-1,2-二氨基环己烷的 [2+2] 环缩合反应以非常好的产率提供了新型大环配体 11 和 12。11个晶体是三斜晶系,空间群P,a = 11.4037(11),b = 11.8184(12),c = 14.6835(14) A,Z = 4,12个是三斜晶系,空间群P,a = 11.2692( 9), b = 12.8612(11), c = 15.2439(12) A and Z = 2。用硼氢化钠还原 11 得到大环 13。11 的配位化学已经用“硬”金属离子 NiII 和 CoII 进行了研究. NiCl2·6H2O 与 11 摩尔当量的 11 在回流的甲醇中反应,然后加入 NH4PF6,得到 NiIII 配合物 14。根据其顺磁性(μeff = 2. 50 μB)和紫外/可见光谱,并通过单晶 X 射线衍射研究进一步证实。14 的