The chemistry of cyclopentadienyl and related nitrosyl complexes of molybdenum. Part V. Dihalogenonitrosyl[tris(pyrazolyl)borato]molybdenum complexes, their alcoholysis, and the crystal structure of chloronitrosylisopropoxo[tris(4-chloro-3,5-dimethylpyrazolyl)borato]molybdenum
- 1 January 1976
- journal article
- research article
- Published by Royal Society of Chemistry (RSC) in J. Chem. Soc., Dalton Trans.
- No. 10,p. 898-908
- https://doi.org/10.1039/dt9760000898
Abstract
Halogenation of [Mo{HB(3,5-R2C3HN2)3}(NO)(CO)2] gives [{Mo[HB(3,5-R2-4-XC3N2)3](NO)Y2}n](R = X = H, Y = Cl, Br, or I, n= 2; R = Me, X = H, Y = Cl, Br, or I; n= 1; R = Me, X = Cl or Br, Y = Cl or Br, n= 1). These halides react with alcohols affording [Mo{HB(3,5-R2-4-XC3N2)3}(NO)Y(OR′)](R′= Me, Et, Pri, Bu8, or CH2CH:CH2), the 1H and 13C n.m.r. spectra of which are discussed. The crystal structure of [Mo{HB(3,5-Me2-4-ClC3N2)3}(NO)Cl(OPri)] has been determined by X-ray diffraction methods using counter data and refined by block-diagonal least-squares procedures, to R 0.047 for 2 450 reflections. The monoclinic unit-cell, space-group P21/n, has dimensions a= 12.268(4), b= 16.041(4), c= 15.033(5)Å, β= 91.44(4)° for Z= 4. The molybdenum atom has octahedral co-ordiantion and both the Mo–Cl and, particularly, the Mo–O distances are short. The Mo–O bond length (1.86 Å) indicates significant MoOR bonding and pπ→dπ donation from the alkoxy-group to the metal is discussed in terms of the apparent co-ordinative unsaturation of the alkoxide complexes.Keywords
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