(Requ le 5 juillet 1976, acceptd le 24 septembre I976)The structure of NazSb407 has been determined by single-crystal X-ray techniques. The crystals are monoclinic, space group C2/c or Cc, with a = 11.03, b = 16.92, c = 9.64/~,, fl = 149.4 o, Z = 4. An R value of 0-067 has been obtained atter refinement by the least-squares method for 2162 independent reflexions. The structure consists of chains of (Sb207~ "-parallel to [I01 ]; these chains are linked to form tunnels into which the Sb m lone pairs project. A comparative study of bond lengths and angles in the antimony coordination polyhedra is made between this stucture, KSbaO~ and NaSb~O 8.
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