³⁵CI and ^121.123Sb nuclear quadrupole resonance (n.q.r.) spectra of tetrachloro(acetylacetonato)antimony(v), (1), and ten related compounds have been observed and measured in the range 77-300 K. The crystal structures of (1 ) and of tetrachloro( benzoylbenzophenato)antimony (5) are also reported. The n.q.r. spectrum of the latter compound indicates the occurrence of a second-order phase-change in the neighbourhood of 135 K; this is confirmed by thermal analysis. Comparison of the crystal structure and n.q.r. spectrum of (1) indicates that a similar phase-change takes place here below 77 K. The distinction between the ³⁵CI resonance frequencies of the axial and equatorial chlorine atoms of these compounds, already suggested in Part 1, is confirmed.