Abstract
The crystal and molecular structure of pentakis-2,8,9-trioxa-1-phosphaadamantane-nickel(II) perchlorate, Ni(P(OC2H3)3)5(ClO4)2, has been determined from three-dimensional X-ray data collected by counter techniques. Due to disorder in one of the perchlorate groups and the large number of parameters involved, only isotropic refinement was carried out, to a final R factor of 0.15. The material crystallized in space group P1̄ with lattice parameters a = 11.53(5), b = 18.92(7), c = 12.61(5) Å, α =96.4(5), β = 103.4(6) and γ = 96.9(5)°. There are two molecules per unit cell and the calculated density is 1.67 g/cc. The inner coordiantion about the nickel atom is approximately trigonal bipyramidal. The average axial bond distance is somewhat shorter than the equitorial distance 2.14(1) vs. 2.19(1) Å.
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