Electrospray Mass Spectrometry Study on Polynuclear Pd (Ⅱ)and Ni (Ⅱ) Complexes of 3,6,9,16,19,22-Hexaazatricyclo [ 22.2.2.211, 14 ] triaconta-11, 13,24,26( 1 ) ,27,29-Hexaene

• 来源期刊: 中国化学（英文版）
• 学科: 化学
• 年，卷（期）: 2001,（8）
• 所属期刊栏目: Articles
• 页码范围: 757-765
• 页数: 9页
• 分类号: O6
• 语种: 英文

摘要

Polynuclear Pd(Ⅱ) and Ni(Ⅱ) com, exes of macrocyclic polyamine 3, 6, 9, 16, 19,22-hexaazatricyclo [ 22. 2.2.211,14]-triaconta 11,13,24,26(1),27,20-hexaene (L) in solution were investigated by electrospray ionization mass spectrometry (ESIMS). For methanol solution of complexes M2LX4(M =Pd(Ⅱ) and Ni(Ⅱ), X= Cr and I-), two main clusters of peaks were observed which can be assigned to [M2LX3]+ and [M2LX2]2+. When Pd2LCl4 was treated with 2 or 4 mol of AgNO3, it gave rise formation of Pd2LCl2(NO3)2· H2O and [Pd2L(H2O) (NO3)n](4-n)+, respectively. ESMS spectra show that the dissociation of the former in the ionization process gave peaks of [Pd2LCl2]2+ and [(Pd2LCl2)NO3]+, while dissociaqtion of the later gave the peaks of[Pd2L(CH3CO2)2]2+ and {[Pd2L(CH3CO2]·(NO3)}+ in the ppresence of acetic acid. Similar species were observed for Pd2LI4 when treated with 4 mol of AgNO3. When [Pd2L.(H2O)4-n(NO3)n](4-n)+ reacted with 2 mol of oxalate anionsat 40℃, [Pd4L2(C2O4)2(NO3)2]2+ and [Pd4L2(C2O4)2·(NO3)]3+ were detected. This implies the formation of square-planar molecular box Pd4L2(C2O4)2(NO3)4 in which C2O2-4 may act as bridging ligands as confirmed by crystal structure analysis. The dissociation for and the stability of complex cations in gaseous state are also discussed.This work provides an excellent example of the usefulness of usefulness of ESIMS in the identification of metal complexes in solution.