Applications of molybdenum-95 N.M.R. spectroscopy. VI. ⁹⁵Mo and ¹³C N.M.R. of certain cis-dioxomolybdenum(VI) compounds and related species. The crystal and molecular structure of Bis(N,N-diethylhydroxylamido(l -)-O,N)- disulfidomolybdenum(VI) hemibenzene

Abstract

The ⁹⁵MO n.m.r. spectra of a series of compounds containing the fac-[Mo^VIO₃] and cis-[ Mo^VIO₂] units are reported, together with those for the series [MoX₂(R₂NO)₂] (X = O or S; R = Et, PhCH₂). Trends in the data are discussed. The stereochemistry in solution of certain of the cis-dioxo species is assigned by means of ¹³C n.m.r. spectroscopy. The crystal and molecular structure of [MoS₂(Et₂NO)₂],0.5C₆H₆ has been determined by X-ray crystallography. The steric and electronic requirements of the terminal sulfide ligands significantly affect the detailed coordination geometry relative to that observed for the dioxo analogue [MoO₂(Et₂NO)₂]. Crystal data: a 10.162(2), b 11.836(2), c 14.437(2) Å, β 106.12(2)º P2₁/a; Z 4.