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The crystal structures of flux-grown Li 2 (MoO 4 ), LiY(MoO 4 ) 2  and LiNd(MoO 4 ) 2  were solved and refined from single-crystal intensity data collected with a four-circle diffractometer (Mo K  α X-radiation, CCD area detector, room temperature). Li 2 (MoO 4 ) is isostructural with phenacite, Be 2 (SiO 4 ) and has space group  R 3̅,  a  = 14.330(2),  c  = 9.584(2) Å,  Z  = 18 (R1 = 1.6%). The structure consists of a three-dimensional network of corner-linked, slightly distorted LiO 4  and fairly regular MoO 4  tetrahedra. Average Li–O and Mo–O distances are 1.965 Å (Li1) and 1.967 Å (Li2), and 1.764 Å (Mo). The atomic arrangement is characterised by a narrow open channel along the three-fold axis. Comparisons are drawn with other phenacite-type compounds. Low-temperature single-crystal X-ray studies of Li 2 (MoO 4 ) in the range from 103 to 293 K gave no evidence of a phase transition, thus contradicting recent literature reports. Both LiY(MoO 4 ) 2  and LiNd(MoO 4 ) 2  crystallise in the scheelite-type structure, with space group  I 4 1 /a and  Z  = 2 ( R 1 = 1.7 and 2.7 %, re-spectively). The first has  a  = 5.148(1),  c  = 11.173(2) Å,  V  = 296.11(10) Å3, the latter  a  = 5.243(1),  c  = 11.440(2) Å,  V  = 314.47(10) Å 3 . Both Li and Y/Nd are completely disordered on a jointly occupied site. Mean (Y,Li)– and (Nd,Li)–O distances are 2.40 and 2.47 Å, respectively. In both compounds the unique MoO 4  tetrahedron has four identical Mo–O bonds with lengths of 1.779 Å. The stoichiometry of Li RE (MoO 4 ) 2  ( RE  = rare-earth element) compounds is discussed and the relation to structure types of other  MRE (XO 4 ) 2  ( M  = alkali metal,  X  = Mo, W) compounds is briefly addressed.

The crystal structures of phenacite-type Li 2 (MoO 4 ), and scheelite-type LiY(MoO 4 ) 2 and LiNd(MoO 4 ) 2