Complexes of lanthanide dithionates 2. Electrospray mass spectrometry of Ln_2(S_2O_6)_3 and their Ph_3PO complexes; the X-ray crystals structure of Pr_2(S_2O_6)_3(Ph_3PO)_6(H_2O)_6

摘要

The crystal structure of Pr_2(S_2O_6)_3(Ph_3PO)_6(H_2O)_6 (1), has been determined and is compared with the previously reported Nd_2(S_2O_6)_3(Ph_3PO)_4(H_2O)_8 (2), and Nd_2(S_2O_6)_3 centre dot 14H_2O (3). the steric congestion in the primary coordination sphere, evaluated by steric angle sum (SAS) calculations, shows that all the complexes have SAS values within the expected range for the coordination number of the metal. The incorporation of extra Ph_2PO in 1 is accommodated by a very long Pr-OH_2 distance. The behaviour of lanthanide dithionates and their triphenylphosphine oxide complexes under electrospray mass spectrometry conditions has been investigated. For Ln_2(S_2O_6)_3, the expected ions, Ln(S_2O_6)~+ and Ln(S_2O_6)_2~-, and their methanol solvates, are observed as weak signals. The relationship between these and the major ions observed in the gas phase is discussed. The spectra of the triphenylphosphine oxide complexes show no lanthanide containing ions.