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[R2P(E)NP(E)R2] has of late received much attention.1 Whereas extensive work has focused on symmetrical systems (E = O, S or Se), there has been considerably less documentation regarding asymmetrical ligands [R2P(O)NP(S)R2]. Our working group has undertaken a study of the interaction of bromopentacarbonylmanganese with symmetrical [R2P(E)NP(E)R2] systems.2,3 In an effort to extend our studies to asymmetrical systems, we tested the reactivity of the imidothiophospinate ligand, [R2P(S)NP(O)R2], towards [BrMn(CO)5]. Here, we report on the X-ray structure of the manganese(II) complex, Mn[Ph2P(S)NP(O)Ph2O,S]2 1. Data were collected on a Siemens SHELXTL PLUS (PC Version) diffractometer. Crystallographic data, the details of Xray data collection and a structure refinement are summarized in Table 1. The intensities were collected using nickel-filtered Cu Kα radiation (λ = 1.54178 Å) at room temperature, and were corrected for Lorentz and polarization effects.3 The structure was solved by direct methods4 and refined by full-matrix leastsquares with anisotropic temperature factors for the nonhydrogen atoms. The structure solution and refinement included the observed reflections with F > 4.0σ (F) only. The hydrogen atoms were placed at their idealized positions and included in the structure factor calculation with fixed isotropic thermal parameters (U = 0.08 Å2). A diagram of the structure of complex 1 is shown in Fig. 1. The asymmetric unit and the atomic numbering are shown in Fig. 2. The geometry around the metal center is a distorted tetrahedron. The distortion is especially plain to see in the angles of the systems, E–Mn–E′, where E ≠ E′, even though both chalcogens belong to the same ligand. The six-membered rings 611 ANALYTICAL SCIENCES MAY 2002, VOL. 18 2002 © The Japan Society for Analytical Chemistry

Crystal Structure of Mn[Ph2P(S)NP(O)Ph2-O,S]2: A Manganese(II) Complex with a Mixed Chalcogen Imidothiodiphosphinate Ligand