Unexpected Synthesis and Crystal Structure of Macrocyclic Nickel Complex Involving Rare S-Cl Bond  

作　　者：欧光川 袁先友 李治章 

机构地区：[1]Department of Biology and Chemistry,Hunan University of Science and Engineering

出　　处：《Chinese Journal of Structural Chemistry》2013年第3期420-424,共5页结构化学（英文）

基　　金：supported by the Science and Technology Planning Project of Hunan Province (2012FJ3050,2012NK3067);the Construct Program of the Key Discipline in Hunan Province (2011–76);the Science and Technology Innovative Research Team in Higher Educational Institutions of Hunan Province (2012–318)

摘　　要：A novel complex of [NiL（OOCNH2C2H3SClO3）]·H2O was obtained unexpectedly by the reaction of [Ni（rac-L）]（ClO4）2 with l-cysteine （L=5,5,7,12,12,14-hexamethyl-1,4,8,11-tetra- azacyclotetradecane）, and characterized by EA, IR, ESI-MS and single-crystal X-ray diffraction. It crystallizes in the orthorhombic system, space group P212121 with a=9.211（12）, b=14.942（19）, c=19.002（2）, Mr=563.80, V=2615.3（6）3 , Z=4, Dc=1.432 g/cm3 , F（000）=1204, μ=0.966 mm-1 , the final R=0.0565 and wR=0.1515. The central nickel（Ⅱ） ion displays a distorted six-coordinate octahedral coordination geometry by coordination with four nitrogen atoms of L, and one oxygen and one nitrogen atoms of l-cysteine. The sulfur atom of l-cysteine instead of oxygen atom links directly with the chlorine atom of perchlorate. The title complex is the first example of perchlorate salt involving the sulfur atom.A novel complex of [NiL（OOCNH2C2H3SClO3）]·H2O was obtained unexpectedly by the reaction of [Ni（rac-L）]（ClO4）2 with l-cysteine （L=5,5,7,12,12,14-hexamethyl-1,4,8,11-tetra- azacyclotetradecane）, and characterized by EA, IR, ESI-MS and single-crystal X-ray diffraction. It crystallizes in the orthorhombic system, space group P212121 with a=9.211（12）, b=14.942（19）, c=19.002（2）, Mr=563.80, V=2615.3（6）3 , Z=4, Dc=1.432 g/cm3 , F（000）=1204, μ=0.966 mm-1 , the final R=0.0565 and wR=0.1515. The central nickel（Ⅱ） ion displays a distorted six-coordinate octahedral coordination geometry by coordination with four nitrogen atoms of L, and one oxygen and one nitrogen atoms of l-cysteine. The sulfur atom of l-cysteine instead of oxygen atom links directly with the chlorine atom of perchlorate. The title complex is the first example of perchlorate salt involving the sulfur atom.

关 键 词：macrocyclic nickel（Ⅱ） complexes crystal structure L-CYSTEINE PERCHLORATE 

分 类 号：O627.8[理学—有机化学]