Anorg. Allg. Chem. 608, 100-114.
CommentThe synthesis of the title compound, (I), was undertaken as part of our current research (Carrillo, Gouzerh & Jeannin, 1985;Bustos et al. 1991; Carrillo, Robert © 1995 , 1992; Debenjak, Bustos, Carrillo, Robert & Gouzerh, 1992a,b;Li-Kao, Bustos, Carrillo, Robert & Gouzerh, 1993). The purpose was to obtain a new precursor for the preparation of molybdenum complexes containing organo-dinitrogen ligands, for use as models of the postulated intermediates in the convertion of coordinated dinitrogen into ammonia (Henderson, Leigh & Picket, 1983;Leigh, 1992).The complex is dianionic in nature ( Fig. 1) and shows monomeric units composed of two mercaptobenzoate ligands coordinated to a cis-Mo02 core through atoms S1, $2, 03 and 05. The coordination sphere around the Mo vt ion is best described as a slightly distorted octahedron, where the basal plane is defined by Mo---O1 The apical sites are occupied by atoms S1 and $2 of the organic anion, 5 ° away from the vertical due to the strain imposed by the close chelate structure. The anion presents a non-crystallographic twofold axis which bisects the Ol~Mo---O2 and O3~Mo---05 angles. These structural characteristics are similar• cc,'~ c20 Fig. 1. View of the title molecule showing the atom-labelling scheme. Displacement ellipsoids are shown at the 40% probability level. H atoms are omitted for clarity, except for those involved in strong hydrogen bonds.to those found in closely related compounds, mainly in (NHn)2[MoO2{O2CC(S)Ph2}2].2H20 (Palanca et al., 1990). The structure is completed by two Et3NH ÷ cations, the geometry of which posed some problems in the early stages of refinement. A soft similarity restraint applied to the C---C and CmN bond lengths was enough to stabilize the convergence. The resulting geometry was fairly regular, showing a strong coupling to the anion through two rather short hydrogen-bonded contacts ( Fig. 1) (04...H1AmN1, estimated length/angle 1.86/~d175°; O6.--H2A~N2, estimated length/angle 1.80/~/171°), leading to somewhat independent neutral units connected to one another only through coulombian interactions (Fig. 2).
ExperimentalThe title compound was prepared by reaction of 10 mmol 1.478 (9) CI0---CI 1 i.376 (9) N I---C!51.479(9) CI 1---C12 1.371 (10) N2--C211.477 (7) C12----C13 1.394 (9) N2---C231.481 (7) CI 3------CIA 1.403 (8) N2---C251.485 (8) C15---C16 1.505 (10) O3---CI 1.250 (7) C17---C18 1.514 (10) O4----CI 1.254 (7) Ci9---C20 1.502 (10) O5---C81.270 (7) C21----C22 1.506 (10) O6---C81.251 (7) C23----C24 1.505 (10) C 1----C21.499 (8) C25---C26 1.507 (10) The structure was solved through a combination of direct methods and difference Fourier synthesis using the