Crystal structure of the complex cis-oxobis[piperidine N-oxido(1–)-NO]thiomolybdenum(VI), containing a cis-MoOS2+ group

Abstract

The first example of a MoOS²⁺ complex, cis-[MoOS(C₅H₁₀NO)₂][C₅H₁₀NO = piperidine N-oxido(1–)], prepared by reaction of the corresponding cis-MoO₂²⁺ complex with B₂S₃, has been crystallographically characterised. The title compound crystallises in the monoclinic space group P2₁/n, with a= 9.671(1), b= 22.401(2), c= 13.116(2)Å, β= 95.51(1)°, and eight molecules, comprising two crystallographically distinct species, per unit cell. The structure has been determined from 4 033 unique observed diffractometer data and refined to R= 0.047. The two independent molecules are virtually identical, and possess Mo–O and Mo–S bonds of length 1.723(12) and 2.106(5)Å respectively and an O–Mo–S interbond angle of 116.9(7)°. The dimensions and a selection of spectroscopic properties of the title complex are compared with those of the corresponding cis-[MoY₂(C₅H₁₀NO)₂](Y = O or S) complexes; cis-[MoS₂(C₅H₁₀NO)₂] may be prepared by treating the MoOS²⁺ complex with B₂S₃.