Reactions of Heteroboranes. Synthesis of *CH2Cl2, its Crystal and Molecular Structure and that of SeB11H11

Article abstract of DOI:10.1039/DT9870000699

The reaction (refluxing ethanol) of with closo-SeB11H11 affords two products.One, characterised spectroscopically, is .The second product, isolated after recrystallisation from dichloromethane-ethanol solution is <2,2-(PPh3)2-1,2-SePtB10H10>*CH2Cl2 (1).An X-ray diffraction study shows crystals of (1) to be triclinic, space group P1, with two formula units in a cell of dimensions a = 12.837(3), b = 14.534(2), c = 11.898(3) Angstroem, α = 96.59(2), β = 107.31(2), γ = 81.89(1) deg.Using 5046 reflections, the structure was refined to R = 0.028.The dodecahedral SePtB10 cage has Se and Pt atoms occupying adjacent sites.The principal dimensions include the bond lengths Pt-Se 2.676(1), Se-B 2.098(9)-2.210(6), Pt-P 2.326(1) and 2.350(2), and Pt-B 2.231(8)-2.311(6) Angstroem and an interplanar angle of 80.0 deg between the plane containing the PtP2 unit and that containing the Se and Pt atoms and passing through the mid-point of the B(2)-B(3) bond opposite the Se atom.The crystal and molecular structure of SeB11H11 was studied by X-ray diffraction methods in an attempt to provide more information on Se-B bonding.Crystals of SeB11H11 are cubic, space group Pa3, with four molecules in a cell, a = 9.847(3) Angstroem.The structure was refined to R = 0.075 for 164 reflections.The molecule lies on a site with 3 crystallographic symmetry; the electron density and refinement are consistent with scrambling of the Se atom and eleven B-H groups over the twelve dodecahedral positions.This precluded any precise determination of Se-B bond distances.

Full text of DOI:10.1039/DT9870000699

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