Synthesis and structural characterization of two molybdenum carbonyl complexes containing dithiocarbamato ligands derived from pyrrolidine and piperidine
Resource
Journal of Organometallic Chemistry 461 (1-2): 111-116
Journal
Journal of Organometallic Chemistry
Journal Volume
461
Journal Issue
1-2
Pages
111-116
Date Issued
1993
Author(s)
Abstract
Reaction of [MO(pip)2(CO)4] (pip=piperidine) with (S, S)- in acetonitrile gives readily [Moη2-(S, S)(CO)4]-, isolated as [PPN][Mo(η2-(S, S))(CO)4] (PPN+= bis(triphenylphosphine)iminium; (S, S)-= pyrrolidine- (1) or piperidine-1-carbodithioato (2)). The two compounds have been characterized by elemental analysis, IR, nuclear magnetic resonance and X-ray crystallography. 1: monoclinic, P21/n; a = 16.207(5), b= 12.804(3) Å, c = 20.398(4) Å; β = 91.02(2)°; V = 4232(2) Å3, Z = 4; R = 0.034, Rw = 0.037 based on 4989 reflections with I > 3.0σ(I). 2: monoclinic, P21/n; a = 14.148(4) Å, b = 13.646(5) Å, c = 22.535(8) Å; β = 95.92(3)°; V= 4327(3) Å3, Z = 4; R = 0.054, Rw = 0.041 based on 2048 reflections with I > 2.0σ(I). No appreciably modified ligand structure is found in response to the different pKa of the amine used to form the specific (S, S)- in the compounds. This feature is rationalized by the electron-withdrawing effect of the metal carbonyl fragment, leading to the observed similarity in both the CO stretching and the MoCO distances. © 1993.
SDGs
Type
journal article