X-Ray crystallographic determination of the molecular structures of π-cyclopentadienyl-[1-hydroxy-2,3,4,5-tetrakis(trifluoromethyl)phosphole-1-oxide]cobalt and tricarbonyl-η4-[1-pentafluorophenyl-2,3,4,5-tetrakis(trifluoromethyl)thiophen]manganese

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Abstract
The organometallic derivatives [Co(π-C5H5)(C4F6)2PO(OH)](1) and [Mn(CO)3(C4F6)2SC6F5](2) which resulted from the interaction of hexafluorobut-2-yne with metal complexes have been studied by X-ray diffraction and shown to contain non-planar (CF3)4C4X heterocycles with non-bonding metal–heteroatom separations. The absence of an Mn–S bond in (2) leads to the formulation of a zwitterion structure formally involving a sulphonium derivative with a Mn(–1) species. Crystals of (1) are orthorhombic with a= 9·353(7), b= 9·893(7), c= 17·923(10)Å, space group P212121, and Z= 4. Crystals of (2) are triclinic with a= 7·889(6), 6=11·737(8), c= 12·195(9)Å, α= 91·45(10), β= 69·71(10), γ= 81·55(9)°, space group P and Z= 2. Intensity data were collected on a four-circle diffractometer, and the structures solved by Fourier methods; least-squares refinements converged at R 6·3% over 1922 reflections for (1) and 4·5% over 3229 reflections for (2).

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