Crystal structure of a dinuclear dinitrogen complex: tetrachloro-{chlorotetrakis[dimethyl(phenyl)phosphine]rhenium(I)}-µ-dinitrogen-methoxymolybdenum(V)–methanol–hydrochloric acid

Abstract

The crystal structure of the title complex has been determined from three-dimensional X-ray data. The N–N bond length is 1·18, with MO–N 1·90, and Re–N 1·82 Å. These distances are consistent with a linear Re–N–N–Mo delocalised bonding scheme.

The rhenium atom is octahedrally co-ordinated to four phosphorus atoms (Re–P 2·48 Å), and a chlorine atom, trans to nitrogen (Re–Cl 2·42 Å). The molybdenum atom is octahedrally co-ordinated to four chlorine atoms (mean Mo–Cl 2·39 Å) and a methoxy-group trans to N (MO–O 2·15 Å). The planes of phosphorus and chlorine atoms are parallel, and the atoms are in eclipsed positions.

Crystals are monoclinic, space group P2₁/c, with a= 14·918(1), b= 11·176(2), c= 28·162(3)Å, β= 9·6(1)°, Z= 4. The structure was solved by the heavy-atom method by use of 3589 independent reflections, measured on a diffractometer, and refined by block-diagonal least-squares to R 0·059.