Advances in Inorganic Chemistry and Radiochemistry, Vol. 12 by H.J. Emeléus (ed.), A.G. Sharpe (ed.)

By H.J. Emeléus (ed.), A.G. Sharpe (ed.)

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176 (1965). 20. Bagnall, K. , and Jones, P. , J . Chern. p. 2396 (1964). 21. Bagnall, K. , Jones, P. J . , and du Preez, J. G. ,J. Chem. , A p. 737 (1966). 22. Bagnall, K. , Jones, P. , and Robinson, P. , J . Chern. SOC. p. 2531 (1964). 23. Bagnall, K. , t o be published. 24. Bagnall, K. , 2. Nuturforsch,. 24b, 214 (1969). 25. Bagnall, K. , and du Preez, J. G. , J . Chern. p . 2603 (1964). 26. Bagnall, K. , and du Preez, J. G. , J . Chern. p. 5217 (1965). 27. Bagnall, K. , Deane, A. , Robinson, P.

Two crystal modifications, a and /3, of protactinium pentabromide have been identified (Table ID). Single crystal studies have shown that p-PaBr, (53, ,54) is isostructural with uranium pentachloride (127),each protactinium being 6-coordinate. The dimeric Pa,Br,, unit is shown in Fig. 4 which also lists the bond lengths and angles. It is interesting to note that this structure is based on cubic closest packing of the halogen atoms, whereas those of niobium pentachloride and pentabromide are based on hexagonal closest packing.

The 1 : 5 tetrabromide-DMA complexes (Th to I J inclusive) are isostructural ( 2 4 ) . There is a pronounced change in stability proceeding along the actinide series with 1 : 5 complexes being the most stable for thorium and protactinium and the 1 :3 complexes for the remaining actinides. The 1 : 7 complex could not be obtained pure with thorium tetrachloride and under the preparative conditions required, namely, recrystallization from hot dimethyl sulfoxide, protactinium(1V) was oxidized. The solid 1 :5 and 1 : 3 protactinium tetrachloride compounds are, in fact, unstable in dry nitrogen, behavior which contrasts markedly with the stability of the tetrahalide-phosphine oxide and DMA complexes.

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