Copper(I)Acetylenide pi-Complexes.Synthesis and Structure of Cluster Compound HAmp[Cu_9Cl_8(C=CCH_2OH)_2](HAmp is 4-Aminopyridinium Cation)

摘要

Crystals of the HAmp[Cu_9Cl_8(C=CCH_2OH)_2]cluster compound(HAmp is the 4-aminopyridinium cation(NH_2-C5H_4NH)~+)were obtained through ac electrochemical synthesis and their structure was determined using X-ray diffraction analysis(DARCh autodiffractometer,6/20 scan mode,3435 independent reflections with F>=4sigma(F),R=0.047).The crystals are triclinic: space group P1 ,a=12.547(5) A,b=12.502(4)A,c=8.201(2) A,a=75.93(2)deg,p=82.21(3)deg,y=76.05(3)deg,V=1207(2) A~3,Z=2.Two crystallographically independent moieties ~-(C=CCH_2OH)were detected in the complex structure.Each moiety acts as a double bridging pi,sigma-ligand and binds four or five Cu(I)atoms,thus forming the[Cu_4(C=CCH_2OH)]and[Cu_8(C=CCH_2OH)_2]clusters.The shortest Cu-Cu distance is equal to 2.337(4)A.