The Heavy Transition Elements by S. A. Cotton; F. A. Hart

By S. A. Cotton; F. A. Hart

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Spectra of niobium(V) in aqueous HF indicate that NbOF 5 2 - predominates up to 30 per cent HF and NbF 6 - in stronger solution; solubility as well as concentration determines which species crystallises out. Nb0Cl 5 2- THE HEAVY TRANSITION ELEMENTS 24 and TaC1 6 - appear to be the predominant species in strong aqueous HCl. The MF 6 salts are octahedrally co-ordinated; MOF 5 z- salts are nearly so. Na 3 TaF 8 shows the more usual square antiprismatic eight-co-ordination. Cs 2 [MC1 6 ] contains octahedral anions.

WC1 4(PMe 2 Ph)2 ] reacts with borohydrides to form [WH 6 (PMe 2 Phh]; this hydride also results from reaction with sodium amalgam under hydrogen. Under the appropriate atmospheres,fac- [W(COh {PMe 2 Phh] and [W(N 2 h {PMe 2 Ph) 4 ] are formed. The structures have recently been reported of phosphine complexes of the type mer-ML3 Cl 3 (M = Re, Os, Ir) and trans-M~Cl 4 (M = W, Re, Os, lr, Pt). Here, the ML2 Cl 4 complexes, for example, cover the range of electronic configurations d 2 to d6 • It was found that unit increase of electronic configuration has little effect on M-Cl bond lengths but rather more on M-P bond lengths (a contraction of 5 pm).

2 Oxidation State V Apart from the pentahalide ad ducts MoCl 5 L (L = POCh, NMe 3 ), the compounds have mainly halide, nitrogen-bonded thiocyanate, cyanide or oxide ligands. The most investigated complexes are undoubtedly [Mo(CN) 8 p- and [W(CN) 8 p- and their reduction products, [MoiV(CN)s] 4 -arid [WIV(CN)s] 4 -. The Mo compounds have been especially closely examined, but theW compounds appear to be very similar in properties The compounds are prepared as indicated in the equation above; the [Mo(CN) 8 ] 3 ion may be reduced to [Mo(CN) 8 ] 4 - by ferrocyanide ion.

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