Abstract
The synthesis of a variety of iodo complexes of osmium, including trans-[Os(L-L) 2I 2] (L-L = Ph 2PCH 2CH 2PPh 2, o-C 6H 4(PPh 2) 2, Ph 2AsCH 2CH 2AsPh 2 or o-C 6H 4(AsMe 2) 2), the corresponding trans-[Os(L-L) 2I 2]BF 4, trans-[Os{ o-C 6H 4(AsMe 2) 2} 2I 2][(ClO 4] 2, trans-[OsL 2I 4] (L = PPh 3 or AsPh 3), trans- z[OsL ′ 4I 2] (L′ = Me 3P, Me 3As, Ph 3Sb) and trans-[OsL ′ 4I 2BF 4 are described. The complexes have been characterized by analysis, UV-Vis spectroscopy and cyclic voltammetry, and the results compared with analogues containing lighter halogens. The X-ray structure of trans-[Os(Me 3As) 4I 2]I 3 has been determined: orthorhombic, space group I bam, a=10.290(3), b=13.984(2), c=21.101(3) A ̊ , Z=4 and R=0.032 . The cation has Os-I=2.6544(7) and Os-As=2.5013(9)Å. The OsAs 4 unit shows deviations from planarity which are presumably due to steric interactions. Osmium L III -edge EXAFS data are reported for trans-[Os{ o-C 6H 4(AsMe 2) 2} 2I 2] +/2+.
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