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Crystal and molecular structures of Mo(CO)5P(p-tol)3 and Mo2(CO)8P(p-tol)3 and spectral properties of related σ- and π-bonded phosphine complexes
Alyea, Elmer C.,Ferguson, George,Somogyvari, Arpad
, p. 668 - 674 (2008/10/08)
Molybdenum complexes of the type Mo(CO)5L (L = P(o-tol)3, P(m-tol)3, and P(p-tol)3), Mo(CO)3L (L = P(p-tol)3 and P(mes)3; tol = tolyl) and Mo2(CO)8P(p-tol)3 have been prepared and their IR and 1H, 31P and 95Mo NMR spectra determined. The structure of Mo2(CO)8P(o-tol)3 (I) was determined by X-ray crystallography; one Mo atom is coordinated to phosphorus and the other is π bonded to a p-tol group. Crystals of I are monoclinic of space group P21/n with four molecules in the unit cell of dimensions a = 11.297 (2) A?, b = 20.415 (2) A?, c = 13.016 (2) A?, and β= 100.32 (1)°. Crystals of the related Mo(CO)5P(p-tol)3 (II) are triclinic of space group P1 with two independent molecules in the asymmetric unit. Unit-cell dimensions for II are a = 10.908(5) A?, b = 15.281 (8) A?, c = 16.055 (4) A?, a = 106.04 (3)°, β = 95.25 (2), and γ = 91.33 (4)°. Both structures were solved by the heavy-atom method. Refinement was by full-matrix least-squares calculations with anisotropic thermal parameters for I and by blocked-diagonal matrix least-squares calculations with anisotropic thermal parameters for Mo, P, and CO groups for II. R converged to 0.0239 for 5115 observed reflections for I and 0.0388 for 4078 observed reflections for II measured by diffractometer. The crystal structures contain discrete monomeric molecules separated by normal van der Waals distances. Principal dimensions are as follows: for I, Mo(1)-C(carbonyl) = 1.961-1.974 (3) A?, Mo(1)-C(arene) = 2.314-2.370 (2) A?, Mo(2)-P = 2.557 (1) A?, Mo(2)-C(carbonyl) = 1.997 (3) A? (trans to P), 2.038-2.053 (3) A? for others; for II, Mo-P = 2.562 (2) and 2.555 (1), Mo-C(carbonyl) = 1.986 (7) and 1.988 (7) A? (trans to P), 2.001 (6)-2.041 (8) A? for others.
